The application is that application number is 200610014896.4, the applying date is on July 24th, 2006, denomination of invention is divided an application for the application of " multifunction safety efficient nano-antiseptic fiber ".
Summary of the invention
The invention provides a kind of master batch and fiber and manufacture method thereof, with solve as above functional fibre functional single, the fiber fungistatic effect low, the fiber function lacks the problems such as lasting.
The invention provides a kind of far infrared rays casting charge, this far infrared rays casting charge comprises nano level solid oxide zirconium and titanium dioxide, and zirconic weight percent is 45%, and the weight percent of titanium dioxide is 55%.
The invention provides a kind of anion emission agent, this anion emission agent comprises nano-scale tourmaline powder and titanium dioxide, and the weight percent of tourmaline powder is 75%, and the weight percent of titanium dioxide is 25%.
The invention provides a kind of fungistat, this fungistat comprises Ag
+And titanium dioxide, and Ag
+Weight percent be 6.5%, the weight percent of titanium dioxide is 93.5%.
The invention provides a kind of manufacture method of master batch, the method comprises:
Add the silylation coupling agent in fungistat, the silylation coupling agent of adding accounts for 3% of fungistat weight, 140~160 ℃ lower to water treatment 4~6 hours, mixed at 140~160 ℃ and 4000rpm, form the fungistat mixture;
In the far infrared rays casting charge, add the silylation coupling agent, the silylation coupling agent that adds accounts for 3% of far infrared rays casting charge weight, 140~160 ℃ lower to water treatment 4~6 hours, mixed under 140~160 ℃ and 4000rpm, form far infrared rays casting charge mixture;
Add the silylation coupling agent in the anion emission agent, the silylation coupling agent of adding accounts for 3% of anion emission agent weight, 130~140 ℃ lower to water treatment 3~4 hours, mixed under 130~140 ℃ and 4000rpm, form the anion emission agent composition;
Fungistat mixture, far infrared rays casting charge mixture and anion emission agent composition by 1: 1: 0.75 high-speed stirring admixture activation, were stirred 20 minutes under 135 ℃~145 ℃ and 4000rpm;
B215 stirred 5 minutes under 4000rpm among the adding oxytolerant agent PKB;
Add the polymer support section under low speed 500rpm, additional proportion is superpolymer: mixture=72.5: 27.5, temperature are more than the carrier softening temperature and be lower than 40~50 ℃ of fusing points, stir 20 minutes under high speed 4000rpm; The polymer support section is PP, PET or PA;
Add the organic dispersing agent high-molecular polythene, add-on is 5% of section amount, and high-speed stirring 5~7 minutes changes low speed 200rpm over to again and stirs;
At room temperature be cooled to 28 ℃, reduce the time that contacts with air as far as possible;
Push slivering at twin-screw extruder, temperature is about 250 ℃;
Water-bath cooling in 30 ℃ water;
Dry up with the air knife type hair dryer;
Pelletizing also filters out the antibacterial master batch of multifunctional efficient.
The invention provides a kind of manufacture method of fiber, the method comprises:
The polymer dry section adds master batch, and spinning the PA-6 silk needs with entering the spinning extrusion machine under the nitrogen protection, and temperature is than low 8~10 ℃ of conventional fibre spinning temperature;
Through fondant filter, to spinning manifold, spin manifold temperature is lower than 5~8 ℃ that conventional fibre is used;
Adjust spinning at filament spinning component, assembly place melt pressure should be low than the conventional fibre spinning;
Spinning cooling, wind speed, blast are low than conventional fibre, and wind-warm syndrome is slightly high;
The protofilament first adds water, and profit spins a little more than routine;
Add water through network protofilament second, profit spins a little more than routine;
Spin multi-functional preorientated fiber, multi-functional orientation fibers or multi-functional fully-drawn fibers;
Take interior drafting false twisting to add the bullet method and the POY precursor is processed into DTY adds elater, add again water 3~3.5%;
Drawing product DTY is the antibacterial spandex of multifunctional nano.
Adopt this programme can embody following superiority: 1. the functional of fiber is by the inorganic salt with function are added to obtain.In order to solve the functional single problem of functional fibre, this programme has added three kinds of function inorganic salt, make fiber have several functions, these three kinds of inorganic salt are respectively the efficient fungistat c of a anion emission agent b far infrared rays casting charges, because these three kinds of inorganic salt add among the fiber simultaneously, make fiber have simultaneously the bactericidal effect and to the effect of human body beneficial's far infrared rays and anion emission function; 2. general bacteriostatic fiber only has restraining effect to negative bacterium such as intestinal bacteria, positive bacteria such as gold-coloured staphylococci, and fungi such as Candida albicans are lacked bacteriostatic action.This programme uses the Ag+ fungistat content of high-content 6.5%, and the fiber that so just makes this programme can reach more than 99% to the restraining effect of Candida albicans; 3. carry out spinning among above-mentioned three kinds of inorganic salt being dissolved in spinning melt, make the inorganic salt in the fiber can not lose its function, thereby make the fiber function sustained; 4. this programme demonstrates fully the nourishing function of fabric, has multi-functional, safe, efficient antagonistic property.Its bacteriostasis rate is up to more than 95%, and the emittance of far infrared rays is more than 85%, and the anion emission rate is at 7000/cm
3Above (seeing examining report).Three kinds of function inorganic salt combinations all form with nanometer grade powder, and solve the dispersiveness of each component in superpolymer by technique, have avoided the melten gel particle in the spinning melt to produce.The activation characteristic that has so not only fully shown small size, bigger serface can make again the effect performance of each function more abundant, can carry out smoothly through melt-spinning.
Embodiment
Below by drawings and Examples, technical scheme of the present invention is described in further detail.
● three kinds of function inorganic salt formula combination that the fiber of this programme adds:
1. far infrared rays casting charge: the nano level zirconium white account for far infrared rays casting charge weight 45%, titanium dioxide accounts for 55% of far infrared rays casting charge weight, silylation coupling agent (account for above substance weight 3%);
2. anion emission agent: nano-scale tourmaline powder account for anion emission agent weight 75%, titanium dioxide accounts for 25% of anion emission agent weight, silylation coupling agent (account for above substance weight 3%);
3. efficient fungistat: Ag+ account for efficient fungistat weight 6.5%, account for the titanium dioxide 93.5% of efficient fungistat weight, silylation coupling agent (account for above substance weight 3%);
4. oxytolerant agent: B215 among the PKB (Switzerland's trade names), wherein, PKB is composite antioxidant series, B215 is the compound of oxidation inhibitor pentaerythritol tetrathioglycollate (ky-7910) and oxidation inhibitor tris phosphite (pky-168);
5. organic dispersing agent: high-molecular polythene.
● this programme improvement and innovative point are:
1. have multi-functional in order to reach fiber, this programme is through studying efficient far infrared rays casting charge, efficient anion emission agent and efficient fungistat, be respectively 2%, 2%, 1.5% in its ratio in fiber, add in the spinning melt and carry out spinning, purpose is that the inorganic salt that content is many can be compatible with spinning melt fully; Select suitable silylation coupling agent as the particle surface treatment agent of inorganic salt, impelled inorganic salt and polymer to carry out surface reaction; The function inorganic salt can not separated out in washing use procedure, thereby to keep the multifunctionality of fiber, make the fiber function more lasting.
2. contain a small amount of Ag+ in the fiber and will be difficult to Antifungi, and the Ag+ of vast scale is difficult to join in the superpolymer and goes.This programme adopts non-crystal cotton-shaped titanium dioxide to add as the implantation bed of Ag+, has solved the adding problem of vast scale Ag+, has reached the inhibition effect of fiber to fungi.
3. the use of nano material:
This programme uses the inorganic salt nano material, and the small size of nano material, bigger serface reflect the activity that it is larger, have brought into play fully the functional of multifunctional inorganic salt.The adding of less ratio just can obtain large effect.But use nanometer particle to add in the spinning melt and just have the difficulties in dispersion problem.This programme is taked various particle individual curing, namely processes with surface treatment agent, does dispersion agent with a pulvis again, and agent is tentatively to disperse as primary titanium dioxide as dispersion take tourmalinite such as anion emission.And then add again high-molecular polythene as the melt dispersion agent before sneaking into melt, and then make spinning melt.Through as above individual curing nanometer grade powder and twice dispersion, then can there be gel particles and dispersed fabulous melt, be conducive to normally carrying out of spinning.
4. the master batch method is produced multifunctional fibre:
Multifunctional inorganic salt to be dispersed at first (PP, PET or PA) makes master batch in a small amount of carrier as the master batch method, and then by going to carry out spinning in the melt of deciding ratio and mix spinning.So not but increase a melt dispersion and can carry out less volume and more variety according to market demand and arrange production.
● determining of multifunction safety efficient nano-antiseptic master batch manufacture craft parameter:
1. efficient antibacterial formula combination (J) and high-strength negative ion and far infrared rays casting charge (F) the high temperature activation that dewaters:
Temperature: 140 ℃-160 ℃;
Time: 3~6h;
J∶F=1∶2。
Temperature is high, and overlong time has the component caking; Temperature is low, and the too short pulvis dehydration deficiency that then can make of time does not reach the activation purpose.
2. can recipe ingredient surface treatment (height stirs processing):
Temperature: 140 ℃ ± 5 ℃;
Treatment agent: silylation surface treatment agent;
Height stirs revolution: 4000rpm;
Time: 20 minutes.
The same temperature 1. of temperature; The treatment agent add-on is crossed conference and is caused the pulvis bonding, and height stirs the revolution deficiency, and too short meeting of time causes the pulvis caking, disperses irregular.
3. the adding of polymer support (low speed adding high-speed stirring):
Temperature: on the superpolymer softening temperature, be lower than 40 ℃-50 ℃ of superpolymer fusing points;
Low speed: 200rpm;
At a high speed: 4000rpm;
Time: 20 minutes.
Temperature is crossed the low activation that can reduce pulvis, and excess Temperature can make superpolymer near fusing point, affects pulvis and disperses.In the stirring of low speed short period of time pulvis is disperseed uneven.
4. high-speed stirring adds organic dispersing agent and heatproof oxytolerant auxiliary agent dispersion agent:
Choose high-molecular polythene,
Temperature: be higher than 10 ℃ of dispersion agent flux fusing points;
Time: 5~7 minutes:
Promoter addition: superpolymer weight * (3~5%).
Its fusing point of macromolecule dispersing agent polyethylene is about 114 ℃, and melting temperature adopts dispersion agent fusing point+10 ℃.
Excess Temperature, overlong time dispersion agent viscosity is excessively low, and then parcel is uneven; Otherwise viscosity is too high, and the superpolymer section can't be wrapped up.Promoter addition is very few, and the polymkeric substance viscosity loss is excessive; Otherwise polymkeric substance is easy to change.
5. twin screw temperature:
The twin screw temperature is generally got superpolymer fusing point+(10-15 ℃);
Excessively low slivering (granulating), pulvis and the auxiliary agent dispersion inequality of being unfavorable for of temperature.
● determining of multifunction safety efficient nano-antiseptic fiber manufacture craft parameter:
1. spinning temperature:
Spinning temperature is than low 8-15 ℃ of conventional spinning temperature:
The general superpolymer fusing point that adds pulvis and auxiliary agent is lower than 8-10 ℃ of conventional spinning high polymer temperature;
Cross and exceed low spinning temperature and all can affect the spinning melt flowability, cause difficulty in spinning.
2. spinning cooling conditions:
Wind speed, blast are a little less than conventional spinning;
Rheumatism, wind-warm syndrome are higher than conventional spinning;
Because it is lower a little less than conventional superpolymer enthalpy to contain pulvis superpolymer fusing point, accelerating cooling can affect spinning drawing.
3. spinning one, two road finishes:
Spinning one, two road finishes should be a little more than about 5% of conventional spinning;
Contain the pulvis polymer water absorbent stronger, the low moulding that can affect spinning drawing and POY of profit.
● the principle of work of this programme is three kinds of function inorganic salt are given simultaneously that it to be possessed among a kind of fiber multi-functional more comprehensively to promote the body-care effect.
1. efficient antibacterial its principle is free mainly with the extremely strong Ag+ of activity, when it arrived electronegative microorganism cells, both firmly adsorbed owing to coulombic force, and Ag+ enters cell through cell walls and reacts with " SH ", destroy the activity of cell synthetic enzyme, cell is lost the division growth ability and death.(seeing examining report).
2. nano level anion inorganic salt has (7000/cm of the functions of the high-strength negative ion of emission
3Above).After human body is accepted, reach activation blood, relieving fatigue, the neuro vegetative effect of balance.The suction of negative ion causes the human-body biological effect, regulates nervus centralis and vegetative nervous system.Regulate corticocerebral function the recycle system is had good improvement effect.Because the existence of negative ion, then adsorbable stink improves envrionment conditions.
3. the formula combination of far infrared and inorganic salt can be launched the far infrared rays of the absorbent 2~14um of human body.
Above three kinds of nano grade inorganic salt functional formula combination are dispersed in the high polymers carrier by concrete technology, make master batch.Master batch quantitatively is dispersed in again makes the high poly-melt of function in the superpolymer.By special spinning technique, it is that multi-functional entirely raising oneself slightly to fiber, POY is that multi-functional preorientated fiber, HOY are that multi-functional orientation fibers, DTY are the multifunction safety efficient nano-antiseptic spandex that high-speed spinning becomes functional fibre FDY again.For the new function fabric of spinning fabric enterprise development provides good textile raw material.
It should be noted that at last: above embodiment only in order to technical scheme of the present invention to be described, is not intended to limit; Although with reference to previous embodiment the present invention is had been described in detail, those of ordinary skill in the art is to be understood that: it still can be made amendment to the technical scheme that aforementioned each embodiment puts down in writing, and perhaps part technical characterictic wherein is equal to replacement; And these modifications or replacement do not make the essence of appropriate technical solution break away from the spirit and scope of various embodiments of the present invention technical scheme.