CN101724265B - Denier/superfine denier nylon master granule, preoriented yarn (POY) and draw textured yarn (DTY) stretch yarn and preparation method thereof - Google Patents
Denier/superfine denier nylon master granule, preoriented yarn (POY) and draw textured yarn (DTY) stretch yarn and preparation method thereof Download PDFInfo
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- CN101724265B CN101724265B CN2009103113960A CN200910311396A CN101724265B CN 101724265 B CN101724265 B CN 101724265B CN 2009103113960 A CN2009103113960 A CN 2009103113960A CN 200910311396 A CN200910311396 A CN 200910311396A CN 101724265 B CN101724265 B CN 101724265B
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Abstract
The invention belongs to the field of spinning materials. Firstly, the invention provides a fine denier/superfine denier nylon master granule prepared by proportionally adding a modifying agent, an antioxidant and a dispersant to nylon 6 sliced sheets according to the proportion, melting, mixing and extruding, and the modifying agent is a metallic salt which can take effect on nylon base; The fine denier/superfine denier nylon master granule and the nylon 6 sliced sheets are proportionally mixed, melted and spun, and the fine denier/superfine denier nylon POY is prepared by cooling, oiling, bundling and coiling; and the POY is textured to obtain the DTY. The invention provides the fine denier/superfine denier nylon POY of which the filament size is 0.3-0.8dtex, the filament size of the DTY is 0.25-0.70dtex, which fills the vacancy that the fine denier/superfine denier nylon POY and the DTY are produced by the conventional yarn-spinning process at home and abroad.
Description
Technical field
The invention belongs to the spinning material field, be specifically related to special-purpose master batch of a kind of denier/superfine denier nylon and preparation method thereof and denier/superfine denier nylon POY long filament prepared therefrom, DTY stretch yarns.
Background technology
Take synthon at present terylene (polyethylene terephthalate), polyamide fibre (polyamide-based), polypropylene fibre (polypropylene), spandex (urethane), acrylic fibers (polyacrylonitrile) etc. are generally arranged.These fibers have different qualities, thereby different purposes is also arranged.But at present general wearing fabric, because its fiber is thicker, feel is coarse, flexibility is poor, ventilation property is poor, water-absorbent is poor, be easy to pilling.Along with the raising of people's living standard, also more and more higher for the dress requirement of textiles.Address these problems, satisfy people's different requirements, exploitation different sorts, just like a raging fire the carrying out of research novel, functional fiber.
At present, fiber finer dawnization is an important research direction of new fiber development, existing many relevant reports and product.Thin dawn or super fine denier technology such as polyester, polypropylene-base have obtained extensive popularization." dawn " is a kind of technical term, refers to the 9000m long filament and weighs 1 gram, promptly is called for 1 dawn.Generic term is represented the thickness degree of fiber for " dtex " at present: the 10000m macrofiber weighs 1 gram, is 1dtex.Fiber is thin more, and the dawn number is more little.The thin dawn refers to the fiber of filament number at 3-0.6dtex; Super fine denier refers to the fiber of filament number at 0.1-0.55dtex.
Ultra-fine fibre its specific structure performance just more and more causes people's interest, and the research of the type fiber is also developed rapidly.The present method of making ultra-fine fibre has several, comprises conventional spinning improved method, sea-island-type composite spun method, methods such as exfoliated conjugate spinning.Polyamide fibre has superior physicals, is widely used in fields such as knitted underwear, hosiery, sweat shirt, ski-wear, tights; And compare with polyolefine, trevira, the molecular structure property of polyamide fibre (containing amide group, the analogous protein structure) has good hydrophilic skin-friendly, water absorbability, excellent properties such as ventilation property; The thin dawnization of polyamide fibre can further improve quality of fibre and value, produces the top grade that meets fashion trend and voguish style and takes product; Polyamide fibre fine-denier elastic silk feel is level and smooth, comfortable softness, and good springiness, good permeability, band is few, therefore uses also more and more widely in knitting field.But because the characteristic of nylon itself contains a large amount of hydrogen bonds in the molecular structure, crystallization velocity is fast, and the degree of crystallinity height is difficult for tensile deformation, the situation that therefore causes conventional spinning improved method thin dawn of direct production of present utilization and super fine denier polyamide fibre to realize.Conventional after-processing technology method also is not suitable for the thin dawn and the post-treatment of ultra-fine nylon POY long filament, thereby has also limited the application of thin dawn and ultra-fine nylon greatly.
The patent No. provides a kind of modified poly ester and preparation method thereof for the ZL03112242.6 Chinese invention patent, be that to adopt terephthalic acid (or dimethyl terephthalate (DMT)), ethylene glycol be raw material, esterification (or transesterify) or polycondensation phase add contain the m-phthalic acid composition of metal organic sulfonate base and polyalkylene glycol that molecular-weight average is 500-10000 with batch form carry out block copolymerization and make.On composite spinning machine, make sea island fiber with this raw material, after alkali lye is handled, obtain ultra-fine fibre.Though this invention can make ultra-fine fibre, following essential distinction is arranged: at first, it is to be used in the polyester superfine fibre manufacture view, is not to be used in thin dawn of polyamide fibre or superfine Denier fibre aspect; Secondly, the salt of its adding is the m-phthalic acid of metal organic sulfonate base, is not the metallic salt on the ordinary meaning; Its three, the making of this kind ultra-fine fibre is a sea island fiber, needs just to obtain after alkali lye is handled, compare with direct spinning, complex process, with high costs.
The patent No. provides the preparation method of a kind of nylon 6/ polyelectrolyte anti-static composite material and antistatic master granule for the Chinese invention patent of ZL200510036637.7, by adding basic metal or alkylbenzene sulfonate, hydrophilic polymer in the reactor successively, add dehydrated alcohol or acetonitrile, stirring reaction; Vacuum drying Powdered or particulate state polyelectrolyte; Gained polyelectrolyte, nylon 6, antioxidant, dispersion agent melt blending, the nylon 6/ polyelectrolyte matrix material for preparing has excellent mechanical performances, excellent antistatic property and weather resistance.Also can make antistatic master granule, can become antistatic nylon with nylon 6 melt-spinnings.But, there is essential distinction in this invention with the invention that we set forth: at first, it is by with an alkali metal salt or alkylbenzene sulfonate and hydrophilic polymer carries out stirring reaction and dry back obtains polyelectrolyte, metallic salt only comprises basic metal or alkylbenzene sulfonate, and is that mode and nylon 6 with polyelectrolyte is mixed and made into matrix material; Secondly, this kind method only is to be used in the antistatic fibre field, does not belong to the denier/superfine denier fiber art; Its three, this kind method operational path comparatively speaking is longer, more complicated.
Summary of the invention
The present invention is directed to the shortcoming and defect of prior art, from preparing the purpose that denier/superfine denier high added value chinlon POY filaments and DTY add elater, by using the denier/superfine denier nylon master granule of development voluntarily, make denier/superfine denier nylon POY long filament, denier/superfine denier nylon POY long filament is added bullet and produces denier/superfine denier nylon DTY add elater.Described technology simple possible is saved cost, and spinning process is stable; Simultaneously, the denier/superfine denier nylon POY long filament and the DTY that make add elater, and the range of application of denier/superfine denier nylon is expanded in stable performance greatly.
The contriver is from preparation chinlon master batch angle, by in chinlon master batch, adding properties-correcting agent metallic salt material, change nylon 6 melt structures, when improving the nylon melt structure, the tensile strength of Reinforced Nylon melt, reduce the crystallization rate of nylon melt, on common high-speed spinning equipment, can produce denier/superfine denier nylon POY long filament and DTY adds elater thereby provide a kind of.Denier/superfine denier nylon POY long filament of the present invention, its filament number is 0.3-0.8dtex; Denier/superfine denier nylon DTY of the present invention adds elater, and its filament number is 0.25-0.70dtex.
The objective of the invention is to be implemented by the following technical programs:
The contriver at first provides a kind of denier/superfine denier nylon master granule, it is to be extruded by properties-correcting agent, antioxidant, dispersion agent and nylon 6 slice melt blending to make, wherein, by nylon 6 slice weight, the properties-correcting agent add-on is 0.5-10%, antioxidant 0.1-1%, dispersion agent 0.1-1%, the metallic salt material of described properties-correcting agent for having an effect with nylon matrix is selected from one or more combinations in the compound of the 1st, 2 main group elements.
Antioxidant of the present invention can guarantee nylon 6 slice not oxidative degradation in the high-temperature fusion process, nondiscoloration; Tangible chelating coordination can take place with the nylon molecule in the metallic salt material, changes the nylon melt structure, increases nylon melt tensile strength, and thin dawn spinning is played an important role.The adding of dispersion agent can obviously improve the mixed performance between nylon and the metal-salt, makes the effective constituent can homodisperse, to make the special-purpose master batch of the good and stable denier/superfine denier nylon of performance.Properties-correcting agent metallic salt material, antioxidant, dispersion agent and nylon 6 slice are made master batch under suitable proportioning, suitable conditions such as temperature, and then can on conventional spinning equipment, spin out denier/superfine denier nylon POY long filament and DTY stretch yarns.
As preferred version, according to denier/superfine denier nylon master granule of the present invention, wherein, described metallic salt material is selected from the compound of the 1st, the 2nd main group metal element, comprise one or more combinations in muriate, Sulfates, the metal carboxylate material, its content is the 0.5%-10% of nylon matrix weight.Muriate such as LiCl, CaCl
2, Sulfates material such as MgSO
4, silicates material such as Na
2SiO
3Or the like, these salts are cheap and easy to get, can either take place obviously to interact with nylon, improve its spinning properties; Significantly improve simultaneously the added value of fiber, createed considerable benefit.
As preferred version, according to denier/superfine denier nylon master granule of the present invention, wherein, described antioxidant is selected from one or more in Hinered phenols, triazole species, amine, phosphorous acid esters or the thioesters class antioxidant.Wherein, described hindered phenol anti-oxidants is selected from antioxidant 1010 etc.; The triazole species antioxidant is selected from antioxidant BHT etc.; Amine antioxidants is selected from oxidation inhibitor 5057 etc.; The phosphorous acid esters antioxidant is selected from oxidation inhibitor 168 etc.; The sulfuric acid ester antioxidant is selected from anti-oxidant DLTP etc.
As preferred scheme, the antioxidant among the present invention is from Hinered phenols antioxidant 1010 and phosphite ester kind antioxidant 168.Antioxidant 1010 is a kind of well behaved antioxidant, and stable performance and most polymers have good consistency, and the good discoloration that light and heat causes that prevents can be arranged; Oxidation inhibitor 168 is antioxidants that a kind of resistance to hydrolysis can be good, and stable performance is widely used.The two collaborative use, antioxidant effect can be better.
As preferably, according to denier/superfine denier nylon master granule of the present invention, wherein, and described dispersion agent, it mainly is selected from paraffin, the low-molecular weight polymer at least a.Described lower molecular weight is meant the polymkeric substance of molecular weight at 200-10000, described polymkeric substance comprises polyoxyethylene glycol (PEG), polyvinyl alcohol (PVA), poly(lactic acid) (PLA), PCL (polycaprolactone) etc., is that 600 and 10000 polyoxyethylene glycol (PEG), molecular weight are that 5000 PLA (poly(lactic acid)), molecular weight are PVA (polyvinyl alcohol) of 10000 etc. as molecular weight.These dispersion agents can take place to interact on the one hand and reach miscible with nylon matrix; Also there is significantly effect on the other hand, thereby makes component thorough mixing such as metal-salt, nylon matrix and dispersion agent, fully effect with metal-salt.
The present invention also provides the preparation method of above-mentioned denier/superfine denier nylon master granule, described preparation method comprises: with properties-correcting agent metallic salt material, antioxidant, dispersion agent and nylon 6 slice mixed melting, through the twin-screw extruder granulation, wherein, nylon 6 melt temperatures are that 190-270 ℃, screw speed are that 10-30r/min, die temperature are 190-250 ℃.
As preferred version, according to the preparation method of denier/superfine denier nylon master granule of the present invention, wherein, described nylon 6 slice water ratio is below 600ppm; Before the metallic salt material uses in vacuum drying oven in 150-250 ℃ of dry 6-12h.Thin dawn spinning has significant effects to water ratio to nylon: the water ratio height, easily cause the oxidative degradation of nylon melt, and molecular weight reduces, melt viscosity reduces, and causes tensile strength to reduce, and the spinning lousiness increases, end breakage rate increases, and has a strong impact on spinning production of thin dawn of nylon and fibrous quality thereof.Described nylon 6 slice and properties-correcting agent metallic salt material can be dry as follows: the vacuum drum drying, and drying temperature 85-95 ℃, time of drying, the section water ratio promptly can be controlled in the 600ppm at 18-24 hour; The metallic salt material got final product at 150-250 ℃ of dry 6-12h in the vacuum drying oven before adding.
The denier/superfine denier nylon master granule that the present invention obtains, its melt flow index is 1-10g/10min, melting range is 100-200 ℃.
The present invention also provides a kind of denier/superfine denier nylon POY long filament, it is to add above-mentioned denier/superfine denier nylon master granule by nylon 6 slice to make through direct high speed spinning method, the filament number of gained chinlon POY filaments is 0.3-0.8dtex, wherein, the content of additive master batch accounts for the 1-10% of nylon 6 slice weight.Described master batch addition causes in the fine denier nylon spinning process after a little while, and fiber easily breaks end, produces lousiness, causes cost to raise.When described master batch addition is too high, can cause that fibre strength descends, be unfavorable for that follow-up dyeing and finishing processing weaves.
Above-mentioned high speed spinning method is meant at spinning speed and surpasses under the situation of 3500m/min, carries out the spinning production of denier/superfine denier nylon.When spinning speed was lower than 4000m/min, the gained undrawn yarn had certain orientation degree, and elongation is called pre-oriented yarn (POY) between 55-100%.
As preferred version, according to denier/superfine denier nylon POY long filament of the present invention, wherein, the content of additive master batch accounts for the 1-10% of nylon 6 slice weight.Master batch described in the preferred version adds scope when realizing that the object of the invention promptly provides denier/superfine denier nylon POY long filament, also can make the production cost optimization.
As preferred version, according to denier/superfine denier nylon POY long filament of the present invention, wherein, the breaking tenacity of described denier/superfine denier nylon is 3.3-3.8cN/dtex, and elongation at break is 60-120%.
The present invention also provides the preparation method of above-mentioned denier/superfine denier nylon POY long filament, and described preparation method comprises the steps: successively
(1) mixed melting spinning: nylon 6 slice adds above-mentioned master batch and carries out the mixed melting spinning, and wherein, the screw pressure during fusion is 90-120kg/cm
2, screw speed is 18-35r/min, spinning temperature is 230-290 ℃; Its diameter of orifice that adopts is that 0.15-0.35mm, length-to-diameter ratio are 2.5-4.0,
(2) cross air blow cooling: the blowing of spinning nozzle ring, wind-warm syndrome 28-40 ℃, humidity 40-60%, wind speed 0.3-0.5m/s,
(3) oil, boundling: through the oil thrower boundling that oils, used finish is the polyamide fibre finish second distillation water miscible liquid of 8-12wt% through the cross air blow cooled fibers; The rate of oiling is 0.8-1.8%.
(4) reel: the tow that oils enters winding head through bottom tumbler, top tumbler, rabbit silk head, begins the spinning of reeling, and spinning speed is 3500-4500m/min, promptly gets denier/superfine denier nylon POY long filament.
Polyamide fibre finish second distillation water miscible liquid of the present invention is about to the polyamide fibre finish adds in proportion in the redistilled water to stir and makes emulsion and get final product, and consumption accounts for polyamide fibre finish and redistilled water total weight by it.The polyamide fibre finish selects for use the general reagent in this area to get final product, and as the chinlon filament HOY that uses among the embodiment, the trade mark is DELIONHO-7.
As preferred version, according to the preparation method of denier/superfine denier nylon POY long filament of the present invention, wherein, described nylon 6 slice water ratio is below 600ppm; The master batch water ratio is at (more preferably below the 900ppm) below the 1200ppm.The water ratio height easily causes the oxidative degradation of nylon melt, and molecular weight reduces, and melt viscosity reduces, and causes tensile strength to reduce, and the spinning lousiness increases, and end breakage rate increases.Have a strong impact on spinning production of thin dawn of nylon and fibrous quality thereof.Described nylon 6 slice and master batch can be dry as follows: the vacuum drum drying, and drying temperature 85-95 ℃, time of drying, the section water ratio promptly can be controlled in the 600ppm at 18-24 hour; Master batch can be controlled at water ratio below the 1200ppm at 100-110 in the vacuum drying oven ℃ of dry 12-24h.
The present invention also provides a kind of denier/superfine denier nylon DTY stretch yarns, wherein, described DTY stretch yarns is after adding the above-mentioned direct high speed spinning of denier/superfine denier nylon master granule by nylon 6 slice, make through texturing craft again, the filament number of gained DTY stretch yarns is 0.25-0.70dtex, wherein, the described master batch addition 1-10% that is nylon 6 slice weight.Described master batch addition causes in the fine denier nylon spinning process after a little while, and fiber easily breaks end, lousiness, causes cost to raise.When described master batch addition is too high, can cause that fibre strength descends, be unfavorable for that follow-up dyeing and finishing processing weaves.
As preferred version, according to denier/superfine denier nylon DTY stretch yarns of the present invention, wherein, the content of additive master batch accounts for the 3-6% of nylon 6 slice weight.Master batch described in the preferred version adds scope when realizing that the object of the invention promptly provides denier/superfine denier nylon DTY stretch yarns, also can make the production cost optimization.
The present invention also provides the preparation method of above-mentioned denier/superfine denier nylon DTY stretch yarns, and described preparation method comprises the steps: successively
(1) mixed melting spinning: nylon 6 slice adds above-mentioned master batch and carries out the mixed melting spinning, and wherein, the screw pressure during fusion is 90-120kg/cm
2, screw speed is 18-35r/min, spinning temperature is 230-290 ℃; Its diameter of orifice that adopts is that 0.15-0.35mm, length-to-diameter ratio are 2.5-4.0,
(2) cross air blow cooling: the blowing of spinning nozzle ring, wind-warm syndrome 28-40 ℃, humidity 40-60%, wind speed 0.3-0.5m/s,
(3) oil, boundling: through the oil thrower boundling that oils, used finish is the polyamide fibre finish second distillation water miscible liquid of 8-12wt% through the cross air blow cooled fibers; The rate of oiling is 0.8-1.8%.
(4) reel: the tow that oils enters winding head through bottom tumbler, top tumbler, rabbit silk head, begins the spinning of reeling, and spinning speed is 3500-4500m/min, promptly gets denier/superfine denier nylon POY long filament,
(5) add the bullet operation:
1. seal wire heating: through filar guide, the hot case heating of first roller to the first, Heating temperature is 140-175 ℃ (for the process for processing of denier/superfine denier nylon DTY stretch yarns, Heating temperature must strictly be controlled, can not be too high) with denier/superfine denier nylon POY long filament;
2. cool off false twisting: the heating of POY long filament is after the cooling plate cooling enters scroll tube and twists, and the friction disc material is a pottery, and the assembling form is 1-5-3, and D/Y ratio is (for the production of ultra-fine nylon, D/Y ratio needs strict control) between 1.50-1.75;
3. drawing-off: through step 2. after, the gained fiber enters second roller, carry out drawing-off, enter oil nozzle then and oil, then doing reels again handles, and promptly gets denier/superfine denier nylon DTY stretch yarns, wherein, drafting multiple (carries out suitable drawing-off, when increasing fibre strength, also can reduce elongation of fiber rate and fiber number) between 1.05-1.25; Winding speed is 200-400m/min.
As preferred version, according to the preparation method of denier/superfine denier nylon DTY stretch yarns of the present invention, wherein, described nylon 6 slice water ratio is below 600ppm; The master batch water ratio is at (more preferably below the 900ppm) below the 1200ppm.The water ratio height easily causes the oxidative degradation of nylon melt, and molecular weight reduces, and melt viscosity reduces, and causes tensile strength to reduce, and the spinning lousiness increases, and end breakage rate increases.Have a strong impact on spinning production of thin dawn of nylon and fibrous quality thereof.Described nylon 6 slice and master batch can be dry as follows: the vacuum drum drying, and drying temperature 85-95 ℃, time of drying, the section water ratio promptly can be controlled in the 600ppm at 18-24 hour; Master batch can be controlled at water ratio below the 1200ppm at 100-110 in the vacuum drying oven ℃ of dry 12-24h.
Denier/superfine denier nylon master granule of the present invention is a kind of special-purpose master batch of producing denier/superfine denier nylon POY long filament and DTY stretch yarns that is exclusively used in, it utilizes improving agent metallic salt material and nylon 6 slice and other auxiliary agents (comprising antioxidant, dispersion agent) melt blending extruding pelletization, and modifier content is the 0.5-10% of nylon 6 slice weight.Use described master batch and nylon 6 slice direct fabrics behind mixed melting in the screw rod then, the master batch addition is the 1-10% (preferred 3-6%) of nylon 6 slice weight, master batch and nylon molecule interact, can change the molecular structure of nylon melt, thereby may ultimately reach the purpose of producing denier/superfine denier nylon POY long filament on conventional spinning-drawing machine, the denier/superfine denier nylon POY long filament of gained can obtain denier/superfine denier nylon DTY through texturing craft again and add elater.The filament number of gained denier/superfine denier nylon POY long filament is 0.3-0.8dtex, and fibre breakage intensity is 3.3-3.8cN/dtex, and elongation at break is 60-120%; The filament number that gained denier/superfine denier nylon DTY adds elater is 0.25-0.70dtex, and fibre breakage intensity is 3.9-4.4cN/dtex, and elongation at break is 20-40%, and boiling water shrinkage is 6.0-9.0%, and the crimp shrinkage rate is 40-55%.Denier/superfine denier nylon POY long filament provided by the invention and DTY add elater constant product quality, excellent property, and Color is better.
Denier/superfine denier nylon master granule of the present invention is preparation as follows generally:
(1) get the raw materials ready: in nylon 6 slice weight, take by weighing the properties-correcting agent metallic salt material of its weight 0.5-10%, the antioxidant of 0.1-1%, the dispersion agent of 0.1-1%,
(2) preparation method: the nylon 6 slice that vacuum-drying is good mixes in agitator with properties-correcting agent metallic salt material, antioxidant, dispersion agent, mixes.Then mixture is poured in the hopper of twin screw extruder (containing static state, dynamic mixer), the mixture melt blending is extruded check rod, wherein nylon 6 melt temperatures are that 190-270 ℃, screw speed are that 10-30r/min, extrusion mould-outlet temperature are 190-250 ℃, extrude product pelletizing behind metal track cooling check rod, master batch throughput is 10-20kg/h.The melt flow index of gained master batch is 1-10g/10min, and melting range is 100-200 ℃.
Denier/superfine denier nylon POY long filament of the present invention is preparation as follows generally:
Nylon 6 slice after the vacuum-drying and denier/superfine denier nylon master granule are transported in the twin screw high-speed spinning machine, the nylon chips pump is 50-100g/min for amount, the master batch pump is 0.5-10g/min for flow, is that 230-290 ℃, screw speed are that 18-35r/min and screw pressure are 90-120kg/cm at spinning temperature
2Down fused mixture melt is pushed through screw rod (containing static state, dynamic mixer), pump into spinning pack, after extra large sand filters, extrude through orifice (orifice is characterized as: diameter 0.15-0.35mm, length-to-diameter ratio 2.5-4.0) again through metering.In spinning nozzle ring blowing device, be that 28-40 ℃, humidity are that 40-60% and wind speed are cross air blow cooling under the 0.3-0.5m/s then in the wind-warm syndrome that blows out.Then oil through the oil thrower boundling through the cross air blow cooled fibers, the rate of oiling is 0.8-1.8wt%, and used finish is that concentration is the polyamide fibre finish second distillation water miscible liquid of 8-12wt%.The tow that then oils enters winding head through bottom tumbler, top tumbler, rabbit silk head, begins the spinning of reeling, and spinning speed is 3500-4500m/min.The filament number of gained denier/superfine denier nylon POY long filament is 0.3-0.8dtex, and breaking tenacity is 3.3-3.8cN/dtex, and elongation at break is 60-120%.
Denier/superfine denier nylon DTY stretch yarns of the present invention is preparation as follows generally:
Nylon 6 slice after the vacuum-drying and denier/superfine denier nylon master granule are transported in the twin screw high-speed spinning machine, the nylon chips pump is 50-100g/min for amount, the master batch pump is 0.5-10g/min for flow, is that 230-290 ℃, screw speed are that 18-35r/min and screw pressure are 90-120kg/cm at spinning temperature
2Down fused mixture melt is pushed through screw rod (containing static state, dynamic mixer), pump into spinning pack, after extra large sand filters, extrude through orifice (orifice is characterized as: diameter 0.15-0.35mm, length-to-diameter ratio 2.5-4.0) again through metering.In spinning nozzle ring blowing device, be that 28-40 ℃, humidity are that 40-60% and wind speed are cross air blow cooling under the 0.3-0.5m/s then in the wind-warm syndrome that blows out.Then oil through the oil thrower boundling through the cross air blow cooled fibers, the rate of oiling is 0.8-1.8wt%, and used finish is that concentration is the polyamide fibre finish second distillation water miscible liquid of 8-12wt%.The tow that then oils enters winding head through bottom tumbler, top tumbler, rabbit silk head, begins the spinning of reeling, and spinning speed is 3500-4500m/min.Gained denier/superfine denier nylon POY long filament is through filar guide, the hot case heating of first roller to the first (heating and temperature control is at 140-175 ℃); The heating of POY long filament enters scroll tube and twists processing (generally between 1.50-1.75, the friction disc material is a pottery to the selection of D/Y ratio, and the assembling form is 1-5-3) after cooling plate cools off; Enter second roller after the overcooling false twisting, (drafting multiple when increasing fibre strength, also can reduce elongation of fiber rate and fiber number between 1.05-1.25 to carry out suitable drawing-off; Enter oil nozzle then and oil, then be wound into barrier packaging (winding speed is 200-400m/min) again, promptly get denier/superfine denier nylon DTY stretch yarns, its filament number is 0.25-0.70dtex; Breaking tenacity is 3.9-4.4cN/dtex; Elongation at break is 20-40%; Boiling water shrinkage is 6.0-9.0%; The crimp shrinkage rate is 40-55%.
What the present invention used is conventional twin screw high-speed spinning machine, adopts the master batch volume pump accurately to control the master batch adding proportion, utilizes specific spinning pack: orifice footpath 0.15-0.35mm, length-to-diameter ratio 2.5-4.0; Assembly inland sea sand filtering material is the 40-80 order.Screw rod respectively distinguishes temperature and spin manifold temperature is controlled automatically, and screw rod, volume pump rotating speed and melt pressure frequency conversion are controlled automatically.
The denier/superfine denier nylon POY long filament finished silk performance of gained of the present invention is as follows:
1. filament number: 0.3-0.8dtex;
2. breaking tenacity: 3.3-3.8cN/dtex;
3. elongation at break is 60-120%;
4. oil length is 0.8-1.8%.
It is as follows that the denier/superfine denier nylon DTY of gained of the present invention adds elater finished silk performance:
1. filament number: 0.25-0.70dtex;
2. breaking tenacity: 3.90-4.40cN/dtex;
3. elongation at break is 20-40%;
4. boiling water shrinkage is 6.0-9.0%;
5. the crimp shrinkage rate is 40-55%.
Compared with prior art, the present patent application has the following advantages:
1. the present invention adopts and adds properties-correcting agent metallic salt substance change nylon melt structure, the tensile strength of while Reinforced Nylon melt, reduce the crystallization rate of nylon melt, on common high-speed spinning equipment, can produce denier/superfine denier nylon POY long filament and DTY stretch yarns thereby provide a kind of; The resulting ultra-fine fibre of the present invention can be contained plurality of specifications, has stable excellent properties, weaves the different demands of arrangement processing after can satisfying, the ultra-fine fibre kind of the present invention's exploitation, also can produce non-woven, medical, filtering material etc. enlarges its range of application;
2. the present invention adopts the method for the special-purpose master batch of denier/superfine denier nylon that interpolation develops voluntarily, on conventional high-speed spinning machine, produce denier/superfine denier nylon POY long filament and DTY stretch yarns, with the island method, peel off composite spinning methods such as method and compare, technology is simple, is a kind of eco-friendly high-performance fiber production technology;
3. the present invention adopts conventional high speed spinning method, and production cost declines to a great extent, and the gained fibre property is stable, easy dyeing;
4. production method of the present invention is easy, has filled up the blank that domestic and international denier/superfine denier nylon POY long filament and DTY stretch yarns adopt conventional high speed spinning method to produce, and has promoted the scientific and technological content and the added value of polyamide fibre product.
Description of drawings
Fig. 1 is the technological process of production synoptic diagram of denier/superfine denier nylon master granule of the present invention.
Fig. 2 is the technological process of production synoptic diagram of denier/superfine denier nylon POY long filament of the present invention.
Fig. 3 is the technological process of production synoptic diagram of denier/superfine denier nylon DTY stretch yarns of the present invention.
Embodiment
Below in conjunction with embodiment, be described more specifically content of the present invention.Should be appreciated that enforcement of the present invention is not limited to the following examples, all will fall into protection domain of the present invention any pro forma accommodation and/or the change that the present invention made.
In the present invention, if not refer in particular to, all part, per-cents are weight unit, and all equipment and raw material etc. all can be buied from market or the industry is commonly used.
Main raw material, instrument and equipment:
Nylon 6 slice: relative viscosity 2.47 ± 0.02, density 1.14g/cm
3, fusing point is 215-222 ℃, water ratio is less than 600ppm.
Finish: be polyamide fibre finish second distillation water miscible liquid, wherein said polyamide fibre finish is the chinlon filament HOY that Suzhou this grease of bamboo company limited produces, and the trade mark is DELION HQ-7.
Agitator: high-speed mixing stirrer (good machinery is created in the Zhangjiagang)
Twin screw extruder: twin screw extruder (power chemical industry SHJ-35 is gathered in Nanjing)
Master batch volume pump: Masterbatch volume pump (the new more chemical fiber machinery DKTJ-1 of factory of Wuxi City)
Twin screw high speed spinning trier: (Dalian Synthetic Fibres Inst.)
Volume pump: specification: 0.6ml/rep (0.6 milliliter of revolution), its rotating speed is according to calculating such as finished silk fiber number, proportioning raw materials, spinning speeds.
Elasticizer: Britain Scragg DCS-1200A type polyamide fibre elasticizer
Friction disc: the low snowflake pottery of Britain Scragg Positorg II type plasma spraying 4cm friction disc.
Embodiment 1:
Get the raw materials ready:, take by weighing the antioxidant (mass ratio is 1: 1 antioxidant 1010 and an oxidation inhibitor 168) of its weight 0.2%, 0.3% dispersion agent (mass ratio is 1: 1 whiteruss and PEG600), 0.8% metal-salt MgSO in nylon 6 slice weight
4
The preparation method: the nylon 6 slice that vacuum-drying is good (water ratio 600ppm), metal-salt, antioxidant, dispersion agent mix in agitator, mix.Then mixture is poured in the hopper of twin screw extruder, melt blending is extruded, and nylon 6 melt temperatures are that 245 ℃, screw speed 70r/min, extrusion mould-outlet temperature are 240 ℃, pelletizing behind the metal track cooling check rod, and throughput is 11kg/h.The melt flow index of gained master batch is 6.0g/10min, and melting range is 185-200 ℃.The gained master batch is used for embodiment 2.
Embodiment 2
Nylon 6 slice after the vacuum-drying, master batch (water ratio 700ppm) are transported in the conventional spinning-drawing machine of twin screw, the nylon chips pump is 64g/min for amount, the master batch pump is 6.4g/min for flow, is that 285 ℃, screw speed are that 22r/min and screw pressure are 90-100kg/cm at spinning temperature
2Down fused mixture melt is pushed through screw rod (containing static state, dynamic mixer), pump into spinning pack, after 60-80 order sea sand filters, extrude through orifice (orifice is characterized as: diameter 0.18mm, length-to-diameter ratio 3.8) again through metering.Then in spinning nozzle ring blowing device in the wind-warm syndrome that blows out be 32 ℃, humidity be 50% and wind speed be to cool off under the 0.3m/s.Then oil through cooled fibers through the oil thrower boundling, the rate 1.6% that oils, the used finish amount of attaching most importance to mark is 12% polyamide fibre finish second distillation water miscible liquid, the tow that oils enters winding head through bottom tumbler, top tumbler, rabbit silk head, begin the spinning of reeling, spinning speed is 4000m/min.The filament number of gained chinlon POY filaments is 0.5dtex, and breaking tenacity is 3.7cN/dtex, and elongation is 68%, oil length: 1.5%.The gained chinlon POY filaments is used for embodiment 3.
Embodiment 3
Denier/superfine denier nylon POY long filament through filar guide, the hot case of first roller to the first in 163 ℃ of heating of temperature; The heating of POY long filament enters scroll tube then and twists processing (D/Y ratio is 1.65, and the friction disc material is a pottery, and the assembling form is 1-5-3) after cooling plate cools off; After the overcooling false twisting, enter second roller, carry out suitable drawing-off (drafting multiple is 1.25), when increasing fibre strength, also can reduce elongation of fiber rate and fiber number; Enter oil nozzle then and oil, then be wound into barrier packaging (winding speed is 300m/min) again, promptly get denier/superfine denier nylon DTY stretch yarns, its filament number is 0.4dtex, and breaking tenacity is 4.2cN/dtex, and elongation is 28%, boiling water shrinkage is 7.2%, and the crimp shrinkage rate is 43%.
Embodiment 4
Get the raw materials ready:, take by weighing the antioxidant (mass ratio is 1: 1 antioxidant 1010 and an oxidation inhibitor 168) of its weight 0.5%, 0.5% dispersion agent (mass ratio is 1: 1 whiteruss and PEG600), 2.5% the anhydrous CaCl of metal-salt in nylon 6 slice weight
2
The preparation method: the nylon 6 slice that vacuum-drying is good (water ratio 600ppm) mixes in agitator with metal-salt, antioxidant, dispersion agent, mixes.Then mixture is poured in the hopper of twin screw extruder, melt blending is extruded, and nylon 6 melt temperatures are that 247 ℃, screw speed 60r/min, extrusion mould-outlet temperature are 243 ℃, pelletizing behind the metal track cooling check rod, and throughput is 10kg/h.The melt flow index of gained master batch is 3.9g/10min, and melting range is 180-200 ℃.The gained master batch is used for embodiment 5.
Embodiment 5
Nylon 6 slice after the vacuum-drying, master batch (water ratio 850ppm) are transported in the twin screw spinning-drawing machine, the nylon chips pump is 76g/min for amount, the master batch pump is 7.6g/min for flow, is that 282 ℃, screw speed are that 25r/min and screw pressure are 90-100kg/cm at spinning temperature
2Down fused mixture melt is pushed through screw rod (containing static state, dynamic mixer), pump into spinning pack, after 60-80 order sea sand filters, extrude through orifice (orifice is characterized as: diameter 0.25mm, length-to-diameter ratio 3) again through metering.Then in spinning nozzle ring blowing device in the wind-warm syndrome that blows out be 33 ℃, humidity be 45% and wind speed be to cool off under the 0.3m/s.Then oil through cooled fibers through the oil thrower boundling, the rate of oiling is 1.5%, and the used finish amount of attaching most importance to mark is 12% polyamide fibre finish second distillation water miscible liquid, and the tow that oils enters winding head through bottom tumbler, top tumbler, rabbit silk head, begin the spinning of reeling, spinning speed is 4000m/min.The filament number of the conventional fine-denier polyamide fiber POY of gained long filament is 0.6dtex, and breaking tenacity is 3.65cN/dtex, and elongation is 78%, and the fiber rate of moisture absorption is 6.5%, oil length: 1.4%.The gained chinlon POY filaments is used for embodiment 6.
Embodiment 6
Denier/superfine denier nylon POY long filament through filar guide, the hot case of first roller to the first in 163 ℃ of heating of temperature; The heating of POY long filament enters scroll tube then and twists processing (D/Y ratio is 1.65, and the friction disc material is a pottery, and the assembling form is 1-5-3) after cooling plate cools off; After the overcooling false twisting, enter second roller, carry out suitable drawing-off (drafting multiple is 1.25), when increasing fibre strength, also can reduce elongation of fiber rate and fiber number; Enter oil nozzle then and oil, then be wound into barrier packaging (winding speed is 300m/min) again, promptly get denier/superfine denier nylon DTY stretch yarns, its filament number is 0.5dtex, and breaking tenacity is 4.25cN/dtex, and elongation is 30%, boiling water shrinkage is 7.8%, and the crimp shrinkage rate is 45%.
Embodiment 7
Get the raw materials ready: in nylon 6 slice weight, take by weighing the antioxidant (mass ratio is 1: 1 antioxidant BHT and an anti-oxidant DLTP) of its weight 0.8%, 0.8% dispersion agent (mass ratio is that 1: 1 whiteruss and molecular weight are 5000 PLA, and mass ratio is 2: 1), 4% metal-salt (anhydrous CaCl
2With Na
2SiO
3, ratio is 6: 1).
The preparation method: the nylon 6 slice that vacuum-drying is good (water ratio 600ppm) mixes in agitator with metal salt compositions, antioxidant, dispersion agent, mixes.Then mixture is poured in the hopper of twin screw extruder, melt blending is extruded, and nylon 6 melt temperatures are that 248 ℃, screw speed 58r/min, extrusion mould-outlet temperature are 247 ℃, pelletizing behind the metal track cooling check rod, and throughput is 10kg/h.The melt flow index of gained master batch is 2.6g/10min, and melting range is 170-190 ℃.The gained master batch is used for embodiment 8.
Embodiment 8
Nylon 6 slice after the vacuum-drying, master batch (water ratio 950ppm) are transported in the conventional spinning-drawing machine of twin screw, the nylon chips pump is 89g/min for amount, the master batch pump is 8.9g/min for flow, is that 283 ℃, screw speed are that 29r/min and screw pressure are 90-100kg/cm at spinning temperature
2Down fused mixture melt is pushed through screw rod (containing static state, dynamic mixer), pump into spinning pack, after 60-80 order sea sand filters, extrude through orifice (orifice is characterized as: diameter 0.30mm, length-to-diameter ratio 2.8) again through metering.Then in spinning nozzle ring blowing device in the wind-warm syndrome that blows out be 36 ℃, humidity be 55% and wind speed be to cool off under the 0.4m/s.Then oil through cooled fibers through the oil thrower boundling, the rate 1.2% that oils, the used finish amount of attaching most importance to mark is 12% polyamide fibre finish second distillation water miscible liquid, the tow that oils enters winding head through bottom tumbler, top tumbler, rabbit silk head, begin the spinning of reeling, spinning speed is 4050m/min.The filament number of the conventional fine-denier polyamide fiber POY of gained long filament is 0.7dtex, and breaking tenacity is 3.7cN/dtex, and elongation is 72%, oil length: 1.1%.The gained chinlon POY filaments is used for embodiment 9.
Embodiment 9
Denier/superfine denier nylon POY long filament through filar guide, the hot case of first roller to the first in 163 ℃ of heating of temperature; The heating of POY long filament enters scroll tube then and twists processing (D/Y ratio is 1.65, and the friction disc material is a pottery, and the assembling form is 1-5-3) after cooling plate cools off; After the overcooling false twisting, enter second roller, carry out suitable drawing-off (drafting multiple is 1.25), when increasing fibre strength, also can reduce elongation of fiber rate and fiber number; Enter oil nozzle then and oil, then be wound into barrier packaging (winding speed is 300m/min) again, promptly get denier/superfine denier nylon DTY stretch yarns, its filament number is 0.6dtex, and breaking tenacity is 4.30cN/dtex, and elongation is 28%, boiling water shrinkage is 8.2%, and the crimp shrinkage rate is 47%.
Embodiment 10
Get the raw materials ready: in nylon 6 slice weight, take by weighing the antioxidant (mass ratio is 1: 1 antioxidant BHT and an anti-oxidant DLTP) of its weight 1.0%, 1.0% dispersion agent (mass ratio is that 1: 1 whiteruss and molecular weight are 10000 PVA, and mass ratio is 3: 1), 6.8% metal-salt (anhydrous LiCl and MgSO
4, mass ratio is 5: 1).
The preparation method: the nylon 6 slice that vacuum-drying is good (water ratio 600ppm) mixes in agitator with metal-salt, antioxidant, dispersion agent, mixes.Then mixture is poured in the hopper of twin screw extruder, melt blending is extruded, and nylon 6 melt temperatures are that 250 ℃, screw speed 55r/min, extrusion mould-outlet temperature are 249 ℃, pelletizing behind the metal track cooling check rod, and throughput is 10kg/h.The melt flow index of gained master batch is 1.9g/10min, and melting range is 160-180 ℃.The gained master batch is used for embodiment 11.
Embodiment 11
Nylon 6 slice after the vacuum-drying, master batch (water ratio 1050ppm) are transported in the conventional spinning-drawing machine of twin screw, the nylon chips pump is 100g/min for amount, the master batch pump is 10g/min for flow, is that 286 ℃, screw speed are that 34r/min and screw pressure are 100-110kg/cm at spinning temperature
2Down fused mixture melt is pushed through screw rod (containing static state, dynamic mixer), pump into spinning pack, after 60-80 order sea sand filters, extrude through orifice (orifice is characterized as: diameter 0.35mm, length-to-diameter ratio 2.5) again through metering.Then in spinning nozzle ring blowing device in the wind-warm syndrome that blows out be 36 ℃, humidity be 55% and wind speed be to cool off under the 0.5m/s.Then oil through cooled fibers through the oil thrower boundling, the rate 1.1% that oils, the used finish amount of attaching most importance to mark is 12% polyamide fibre finish second distillation water miscible liquid, the tow that oils enters winding head through bottom tumbler, top tumbler, rabbit silk head, begin the spinning of reeling, spinning speed is 4050m/min.The filament number of the conventional fine-denier polyamide fiber POY of gained long filament is 0.8dtex, and breaking tenacity is 3.80cN/dtex, and elongation is 80%; Oil length: 1.0%.The gained chinlon POY filaments is used for embodiment 12.
Embodiment 12
Denier/superfine denier nylon POY long filament through filar guide, the hot case of first roller to the first in 163 ℃ of heating of temperature; The heating of POY long filament enters scroll tube then and twists processing (D/Y ratio is 1.65, and the friction disc material is a pottery, and the assembling form is 1-5-3) after cooling plate cools off; After the overcooling false twisting, enter second roller, carry out suitable drawing-off (drafting multiple is 1.25), when increasing fibre strength, also can reduce elongation of fiber rate and fiber number; Enter oil nozzle then and oil, then be wound into barrier packaging (winding speed is 300m/min) again, promptly get denier/superfine denier nylon DTY stretch yarns, its filament number is 0.7dtex, and breaking tenacity is 4.30cN/dtex, and elongation is 30%, boiling water shrinkage is 9.0%, and the crimp shrinkage rate is 48%.
Although the contriver has done comparatively detailed elaboration to technical scheme of the present invention and has enumerated, be to be understood that, for the those skilled in the art in this area, according to disclosed content, the foregoing description is modified and/or flexible or to adopt the replacement scheme that is equal to be obvious, the essence that all can not break away from spirit of the present invention, the term that occurs among the present invention are used for can not being construed as limiting the invention the elaboration of technical solution of the present invention and understanding.
Claims (4)
1. the preparation method of a denier/superfine denier nylon POY long filament, described denier/superfine denier nylon POY long filament is to add the direct high speed spinning method of master batch by nylon 6 slice to make, the filament number of gained fiber is 0.3-0.8dtex, wherein, described master batch addition is the 1-10% of nylon 6 slice weight, it is characterized in that described preparation method comprises the steps: successively
(1) melting high-speed spinning: nylon 6 slice adds master batch and carries out melting high-speed spinning, and wherein, the screw pressure during fusion is 90-120kg/cm
2, screw speed is 18-35 r/min, spinning temperature is 230-290 ℃; Its diameter of orifice that adopts is that 0.15-0.35mm, length-to-diameter ratio are 2.5-4.0,
(2) cross air blow cooling: the blowing of spinning nozzle ring, wind-warm syndrome 28-40 ℃, humidity 40-60%, wind speed 0.3-0.5m/s,
(3) oil, boundling: through the oil thrower boundling that oils, used finish is the polyamide fibre finish second distillation water miscible liquid of 8-12wt% through the cross air blow cooled fibers, and the rate of oiling is 0.8-1.8%,
(4) reel: the tow that oils enters winding head through bottom tumbler, top tumbler, rabbit silk head, begins the spinning of reeling, and spinning speed is 3500-4500m/min, promptly gets denier/superfine denier nylon POY long filament,
Wherein, described master batch is to be extruded by properties-correcting agent, antioxidant, dispersion agent and nylon 6 slice melt blending to make, wherein, add properties-correcting agent 0.5-10%, antioxidant 0.1-1%, dispersion agent 0.1-1% by nylon 6 slice weight, the metallic salt material of described properties-correcting agent for having an effect with nylon matrix, be selected from one or more combinations in the compound of the 1st, 2 main group elements, described metallic salt material is selected from one or more combinations in muriate, Sulfates, the metal carboxylate material; Described antioxidant is selected from one or more in Hinered phenols, triazole species, amine, phosphorous acid esters or the thioesters class antioxidant; Described dispersion agent is selected from paraffin, the low-molecular weight polymer at least a, and described lower molecular weight is meant the polymkeric substance of molecular weight at 200-10000.
2. preparation method as claimed in claim 1 is characterized in that, described nylon 6 slice water ratio is below 600ppm; The master batch water ratio is below 1200ppm.
3. the preparation method of a denier/superfine denier nylon DTY stretch yarns, described DTY stretch yarns is after adding the direct high speed spinning of master batch by nylon 6 slice, make through texturing craft again, the filament number of gained DTY stretch yarns is 0.25-0.70dtex, wherein, described master batch addition is the 1-10% of nylon 6 slice weight, it is characterized in that, described preparation method enters the following bullet operation that adds for the described preparation method of claim 1 after the coiling step:
1. seal wire heating: through filar guide, the hot case heating of first roller to the first, Heating temperature is 140-175 ℃ with denier/superfine denier nylon POY long filament;
2. cool off false twisting: the heating of POY long filament is after the cooling plate cooling enters scroll tube and twists, and D/Y ratio is between 1.50-1.75;
3. drawing-off: through step 2. after, the gained fiber enters second roller, carries out drawing-off, enters oil nozzle then and oils, and then doing the processing of reeling again, promptly gets denier/superfine denier nylon DTY stretch yarns, wherein, drafting multiple is between 1.05-1.25; Winding speed is 200-400m/min.
4. preparation method as claimed in claim 3 is characterized in that, described nylon 6 slice water ratio is below 600ppm; The master batch water ratio is below 1200ppm.
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