CN101747624B - Hygroscopic fine denier/superfine denier nylon masterbatch, nylon and preparation method thereof - Google Patents
Hygroscopic fine denier/superfine denier nylon masterbatch, nylon and preparation method thereof Download PDFInfo
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- CN101747624B CN101747624B CN2009103112328A CN200910311232A CN101747624B CN 101747624 B CN101747624 B CN 101747624B CN 2009103112328 A CN2009103112328 A CN 2009103112328A CN 200910311232 A CN200910311232 A CN 200910311232A CN 101747624 B CN101747624 B CN 101747624B
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Abstract
The invention belongs to the field of spinning materials, first provides a hygroscopic fine denier/superfine denier nylon masterbatch which is prepared in the way that hygroscopic modifier, antioxidant and dispersing agent are proportionally added into a nylon 6 slice to be melt as well as blended and then be extruded, and the hygroscopic modifier is PVP; and the hygroscopic fine denier/superfine denier nylon masterbatch is proportionally mixed with the nylon 6 slice to carry out melt spinning, then are cooled, bundled and oiled as well as winded, and after twice drafting, hygroscopic fine denier/superfine denier nylon is prepared. The hygroscopic fine denier/superfine denier nylon provided by the invention has the filament number of 0.45 to 1.0dtex, breaking strength of 3.8 to 4.8 cN/dtex, elongation at break of 20 to 40 percent, and the moisture absorption of fibre of 4 to 10 percent, makes up the gap of preparing the hygroscopic fine denier/superfine denier nylon by adopting the conventional spinning method in both home and abroad, and meanwhile, the improved hygroscopicity of the nylon broadens the application range of the nylon.
Description
Technical field
The invention belongs to the spinning material field, be specifically related to special-purpose master batch of a kind of water absorbability denier/superfine denier nylon and preparation method thereof and water absorbability denier/superfine denier nylon prepared therefrom.
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.
Comfortableness is that clothes are by satisfying the prerequisite performance of Human Physiology health needs, also be the due fundamental propertys of clothes, particularly two season of summer in winter clothes, underwear and children's garment comfortableness is had relatively high expectations, the comfort of summer clothes depends primarily on the water absorbability and the water vapour permeability of material.Water absorbability is meant that dress materials absorb or emit the ability of vapourous water in air.Bibulous lining can in time absorb sweat vapour, the sweat that human body is discharged, and plays heat radiation and regulates the effect of miniclimate humidity between interior table of clothes and body surface, makes human body sensory comfortable.The index of weighing lining water absorbability quality is a moisture regain, and promptly material moisture content accounts for the percentage of material dry weight.When there was the relative humidity difference lining both sides, wet steam was called water vapour permeability from the performance that a side saw through, was diffused into opposite side.Human body was whether comfortable when water vapour permeability was directly connected to perspiration.When human body was perspired, there was certain psychrometric difference the lining both sides of clothes, and sweat vapour is transferred to opposite side from pressing close to skin one side.Natural fiber that water vapour permeability is good and regenerated fiber dress material are easy to seeing through of sweat vapour, reduce the humidity in the clothes miniclimate, keep dry and comfortable comfortable.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 close skin, and toughness is good, rebound resilience good, wear resisting property is good, also has certain moisture.But compare as cotton, hair, silk, fiber crops with traditional natural fiber, its water absorbability, water vapour permeability still exist not enough so cause snugness of fit relatively poor, have also limited it in the directly widespread use of the aspects such as underwear of contact skin.Therefore improve the moisture absorption water vapour permeability of polyamide fibre and improve the very necessity that just seems for its widespread use popularization.The thin dawnization of polyamide fibre can further improve the quality and the value of polyamide fibre on the one hand, can improve the wet thoroughly function of its moisture absorption.Can carry out modification to nylon 6 melt structures on the other hand, thereby improve its water absorbability.
Blend, compound and improve physico-chemical process such as technology is adopted in the production of fine count fiber at present usually, mainly comprises composite algorithm (the island method is peeled off method) and direct method (special-shaped method, hybrid system).The use of island method and special-shaped method is to conversion unit, Working environment, and aspects such as manufacturing process require all very harsh, island method complex process particularly, cost increases, the energy consumption height, and bring the potential problem of environmental pollution.A kind of technology of making fine count fiber in addition is on the spinning equipment of existing melt extrusion manufactured conventional fibre, by adjusting polymer property and spinning technology parameter, realizes fiber finer dawnization, belongs to the method for directly spinning.Compare with the island method, this method is a kind of eco-friendly, green high-performance fiber production technology.The equipment of external general using precision, harsh technology is come the fine denier nylon fiber of production filament number more than 0.8dtex, and cost is higher.And at home, comparing, because the characteristic of nylon itself with polypropylene fibre, terylene, contain a large amount of hydrogen bonds in the molecular structure, crystallization velocity is fast, the degree of crystallinity height, be difficult for tensile deformation, therefore cause the relatively situation of difficulty of the conventional spinning improved method of present utilization direct production fine-denier polyamide fiber.
The method of improving the nylon fibre hygroscopic property at present has: 1. with blend such as a small amount of hydrophilic component such as Polyvinylpyrolidone (PVP)s; 2. hydrophilic component and hexanolactam copolymerization; 3. be copolymerized into hydrophilic polyamide earlier, again with the nylon 6 slice co-blended spinning; 4. carboxyl grafting, amido, cyano group, hydroxyl isopolarity group on nylon 6 molecular backbone chains; 5. by changing the fibre section shape, make fiber heteromorphosis, super-refinement, surface roughening or make fiber form micropore increasing surface-area, thereby improve water absorbability; 6. with hydrophilic agent polyamide fibre or its fabric are carried out the post-treatment processing.In above various method of modifying, copolymerization and grafting method complex process, the implementation cost height is difficult to produce in batches.The physically modified method needs special profile spinneret, such as, application number provides a kind of production method and product of polyamide moisture-absorption perspiration fibre for the Chinese patent application of CN200710028788.7, it mainly is to pass through special production equipment, transform production technique and produce the improvement that the fiber of profiled-cross-section is realized polyamide moisture-absorption, in addition, its production is not fine-denier polyamide fiber; Application number provides a kind of moisture absorption polyamide 6 fibre for the Chinese patent application of CN200610155359.1, and it also is the rate of moisture absorption that improves daiamid-6 fiber by the fiber that production has a special cross-section.The fiber water absorbability that post treatment method obtains is difficult to lastingly.Blending method is because technology is simple, and modified effect obviously has been subjected to people's extensive attention.
In the hydrophilic polymer of various suitability for industrialized production, Polyvinylpyrolidone (PVP) has better heat-resisting, water absorbability, hypotoxicity and good physiological compatibility, is the moisture-absorption modified raw material of a kind of comparatively ideal nylon fibre.The patent No. of toray Co., Ltd. application is that the Chinese invention patent of ZL97109686.4 discloses the refining Polyvinylpyrolidone (PVP) (residual monomer content is less than 0.1%) of a kind of employing, with nylon 6 slice melt blending and spinning, make the nylon fibre that water absorbability obviously improves.But owing to be subjected to the restriction of the wettability power of Polyvinylpyrolidone (PVP) own, have only when the Polyvinylpyrolidone (PVP) mass content surpasses 15%, the standard moisture absorption rate score of modification nylon fibre just can reach the level of textile fiber.And after the Polyvinylpyrolidone (PVP) mass content surpassed 15%, modification polyamide fibre toughness sensation contact very uncomfortablely, and the while spinnability is also bad, can not stably carry out spinning.
The patent No. provides a kind of moisture-absorption modifier that is used for polyamide fibre for the Chinese invention patent of ZL200510037289.5: make PVP alkaline hydrolysis ring-opening reaction at normal temperatures and pressures with nanometer cupric ion catalyzer, to obtain moisture-absorption modifier.During application, this moisture-absorption modifier and Nylon 6 co-blended spinning are made nylon fibre on a small quantity.But this invented technology complexity easily causes environmental pollution, and the moisture-absorption modifier consumption is big, and the cost height is difficult for actually operating.In addition, this patent is not pointed out the specification of nylon fibre, and conventional fibre exists obviously different with fine count fiber.
Summary of the invention
The present invention is directed to the shortcoming and defect of prior art,,, make high-hygroscopicity super fine denier polyamide fibre by using the denier/superfine denier nylon master granule of development voluntarily from preparation denier/superfine denier water absorbability, high added value polyamide fibre purpose.Described technology simple possible is saved cost, and spinning process is stable; Simultaneously, the denier/superfine denier water absorbability polyamide fibre of making belongs to the high-performance high value added product, can bring considerable economic and social benefit.
The contriver is from the chinlon master batch angle, by in chinlon master batch, adding water absorbability properties-correcting agent, change nylon 6 melt structures, thereby can obviously improve the moisture absorption water vapour permeability of polyamide fibre, on conventional spinning equipment, can produce denier/superfine denier nylon with excellent moisture absorption property thereby provide a kind of.The present invention combines the advantage of PVP water absorbability and ultra-fine fibre water absorbability two aspects, thereby makes described denier/superfine denier nylon, and its rate of moisture absorption can reach 4～10% (20 ℃, 65%RH); The filament number of described moisture absorption polyamide fibre is 0.45～1.0dtex.
The objective of the invention is to be implemented by the following technical programs:
The contriver at first provides a kind of water absorbability denier/superfine denier nylon master granule, it is to be extruded by moisture-absorption modifier, antioxidant, dispersion agent and nylon 6 slice melt blending to make, wherein, add moisture-absorption modifier 1～10%, antioxidant 0.1～1%, dispersion agent 0.1～1% by nylon 6 slice weight, described moisture-absorption modifier is polyvinylpyrrolidone (PVP).
Why the present invention selects polyvinylpyrrolidone (PVP), based on three aspect reasons: the one, it is the lactan structure, can take place obviously to interact with nylon matrix, changes the nylon melt structure, makes it to be beneficial to spin the denier/superfine denier fiber; The 2nd, the hygroscopic property of PVP own is good, can improve the rate of moisture absorption of nylon fiber after compound with nylon; The 3rd, itself is active high, is easy to react with multiple dyestuff, can not influence the dyeing of nylon fiber, even can improve the nylon fiber dyeing behavior, and it is easier to make it dyeing, and it is more lasting to paint.Antioxidant of the present invention can guarantee nylon 6 slice not oxidative degradation in the high-temperature fusion process, nondiscoloration; The adding of dispersion agent can make PVP powder, antioxidant powder and nylon 6 slice mix, fully effect.Moisture-absorption modifier, antioxidant, dispersion agent and nylon 6 slice are made the water absorbability master batch under suitable proportioning, suitable conditions such as temperature, and then can spin out the good denier/superfine denier nylon of hygroscopic property on conventional spinning equipment.
As preferred version, according to water absorbability denier/superfine denier nylon master granule of the present invention, wherein, it is at least a in the plurality of specifications such as 1000～100000 that described polyvinylpyrrolidone is selected from molecular weight.Such as selecting PVP1000, PVP2000, PVP10000, PVP24000 or the like for use.
As preferred version, according to water absorbability 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.PVP is a kind of amphipathic organic polymer, can be dissolved in most of organic solvents (as ester class, alcohols, amine and acid etc.), can have an effect with above-mentioned antioxidant, strengthens the synergy ability.
As preferably, according to water absorbability denier/superfine denier nylon master granule of the present invention, wherein, described dispersion agent is selected from paraffin, the low-molecular weight polymer at least a.Described lower molecular weight is meant molecular weight at 200～2000 polymkeric substance, and described polymkeric substance comprises polyoxyethylene glycol (PEG), polyvinyl alcohol, poly(lactic acid) etc., is polyoxyethylene glycol of 600 etc. as molecular weight.These dispersion agents have good synergy, can have an effect with nylon matrix, also has good water absorbability, can well dissolve PVP again, guarantee that PVP reached molecular level and disperses before mixing with nylon matrix, enable fully and nylon interacts homodisperse, and then guarantee the carrying out that the thin dawn spinning process of nylon can steady and continuous, reach the purpose of production water absorbability denier/superfine denier nylon.
The preparation method that above-mentioned water absorbability denier/superfine denier nylon master granule also is provided of the present invention, described preparation method comprises: with moisture-absorption modifier, 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 water absorbability denier/superfine denier nylon master granule of the present invention, wherein, described nylon 6 slice water ratio is below 600ppm; The moisture-absorption modifier water ratio is below 1000ppm.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 moisture-absorption modifier can be dry as follows: the vacuum drum drying, and 85～95 ℃ of drying temperatures, time of drying, the section water ratio promptly can be controlled in the 600ppm at 18～24 hours; 100～110 ℃ of drying 12～24h in vacuum drying oven, the water ratio of moisture-absorption modifier PVP promptly can be controlled in below the 1000ppm.
The water absorbability denier/superfine denier nylon master granule that the present invention obtains, its melt flow index is 5～15g/10min, melting range is 100～200 ℃.
The present invention also provides a kind of water absorbability denier/superfine denier nylon, it is to add above-mentioned water absorbability denier/superfine denier nylon master granule by nylon 6 slice to make through the mixed melting spinning, the filament number of gained nylon fibre is 0.45～1.0dtex, wherein, the content of additive master batch accounts for 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, 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 water absorbability denier/superfine denier nylon of the present invention, wherein, the content of additive master batch accounts for 3～5% of nylon 6 slice weight.Described master batch adds scope when realizing that the object of the invention promptly provides the good denier/superfine denier nylon of water absorbability, also can make the production cost optimization.
According to water absorbability denier/superfine denier nylon of the present invention, wherein, the breaking tenacity of described water absorbability denier/superfine denier nylon is 3.8～4.8cN/dtex, and elongation at break is 20～40%, and the rate of moisture absorption of fiber is 4～10%.The rate of moisture absorption of this kind fiber can reach the real silk level, near cotton fine.Simultaneously, the fiber number of nylon fibre of the present invention is low, belongs to the differential fibre category, and is soft, and specific surface area is big and have unique wicking, and the moisture absorption performance of having a good sweat greatly improves, thereby dress is more comfortable, can be used for making various high-grade fabrics.
The present invention also provides the preparation method of above-mentioned water absorbability denier/superfine denier nylon, 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 15～30r/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: 28～40 ℃ of wind-warm syndrome, humidity 40～60%, wind speed 0.3～0.5m/s,
(3) oil, boundling: finish is the polyamide fibre finish second distillation water miscible liquid of 8～12wt%; The rate of oiling is 0.5～1.5%,
(4) reel: spinning speed is 300～1000m/min,
(5) secondary drawing-off: drafting multiple is that 2.5～3.8 times, drawing temperature are 80～190 ℃, promptly gets water absorbability denier/superfine denier nylon product.
Polyamide fibre finish second distillation water miscible liquid of the present invention is about to the polyamide fibre finish adds in proportion and makes emulsion in the redistilled water 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 finish of using among the embodiment, the trade mark is DELION HO-7.
As preferred version, according to the preparation method of water absorbability denier/superfine denier nylon 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, and has 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 85～95 ℃ of drying temperatures, time of drying, the section water ratio promptly can be controlled in the 600ppm at 18～24 hours; 100～110 ℃ of drying 12～24h in vacuum drying oven, the master batch water ratio promptly can be controlled in below the 1200ppm.
Water absorbability denier/superfine denier nylon master granule of the present invention is a kind of special-purpose master batch that is exclusively used in production water absorbability denier/superfine denier nylon, it utilizes moisture absorption improving agent and nylon 6 slice and other auxiliary agents (comprising antioxidant, dispersion agent) melt blending extruding pelletization, and moisture-absorption modified agent content is 1～10% of a 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 1～10% (preferred 3～5%) 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 production water absorbability denier/superfine denier nylon on conventional spinning-drawing machine.The filament number of gained fiber is 0.45～1.0dtex, and fibre breakage intensity is 3.8～4.8cN/dtex, and elongation at break is 20～40%, and the rate of moisture absorption of fiber is 4～10%.Water absorbability denier/superfine denier nylon constant product quality provided by the invention, water absorbability are good, and Color is better.
Water absorbability denier/superfine denier nylon master granule of the present invention is preparation as follows generally:
(1) gets the raw materials ready:, take by weighing the PVP of its weight 1～10%, 0.1～1% antioxidant, 0.1～1% dispersion agent in nylon 6 slice weight.
(2) preparation method: the nylon 6 slice that vacuum-drying is good mixes in agitator with PVP, and then in agitator, add antioxidant, dispersion agent stirs, mix.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 10～30kg/h.The melt flow index of gained master batch is 5～15g/10min, and melting range is 100～200 ℃.
Water absorbability denier/superfine denier nylon of the present invention is preparation as follows generally:
Nylon 6 slice after the vacuum-drying and water absorbability denier/superfine denier nylon master granule are transported in the conventional spinning-drawing machine of twin screw, the nylon chips pump is 30～50g/min for amount, the master batch pump is 0.3～5g/min for flow, is that 230～290 ℃, screw speed are that 15～30r/min and screw pressure are 60～90kg/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) again through metering.Then in spinning nozzle ring blowing device in the wind-warm syndrome that blows out be 28～40 ℃, humidity be 40～60% and wind speed be cross air blow cooling under 0.3～0.5m/s.Then oil through the oil thrower boundling through the cross air blow cooled fibers, the rate of oiling is 0.5～1.5wt%, and used finish is that concentration is the polyamide fibre finish second distillation water miscible liquid of 8～12wt%.The tow that oils enters winding head through bottom tumbler, top tumbler, rabbit silk head, begins the spinning of reeling, and spinning speed is 300～1000m/min.And then undrawn yarn carried out the secondary drawing-off, wherein the secondary drafting multiple is 2.5～3.8 times, hot drawing temperature: the heat dish is that 80～120 ℃, hot plate are 155～190 ℃.The filament number of gained water absorbability denier/superfine denier nylon is 0.45～1.0dtex, and breaking tenacity is 3.8～4.8cN/dtex, and elongation at break is 20～40%, and the fiber rate of moisture absorption is 4～10%.
What the present invention used is the conventional spinning-drawing machine of twin screw, 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 40～80 orders.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 water absorbability denier/superfine denier nylon finished silk performance of gained of the present invention is as follows:
1. filament number: 0.45～1.0dtex;
2. breaking tenacity: 3.8～4.8cN/dtex;
3. elongation at break is 20～40%;
4. water ratio: 1.2～1.5%;
5. oil length: 0.5～1.5%;
6. the rate of moisture absorption 4～10% of fiber.
Compared with prior art, the present patent application has the following advantages:
1. the present invention adopts the interpolation moisture-absorption modifier, changes the nylon melt structure, thereby can obviously improve the moisture absorption water vapour permeability of polyamide fibre, for the widespread use of fine-denier polyamide fiber provides technical support.
2. the present invention adopts the method for the special-purpose master batch of water absorbability denier/superfine denier nylon that interpolation develops voluntarily, on conventional spinning-drawing machine, produce fine-denier polyamide fiber, 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 spin processes production, and 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 water absorbability denier/superfine denier nylon adopts conventional spin processes 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 water absorbability denier/superfine denier nylon master granule of the present invention.
Fig. 2 is the technological process of production synoptic diagram of water absorbability denier/superfine denier nylon 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 chinlon filament HOY finish, and the trade mark is DELION HQ-7 (production of Suzhou this grease of bamboo company limited).
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)
The conventional spinning-drawing machine drawing-off of twin screw flexing test machine: (Nanchang friend's connection frame PQ668A of company limited)
Volume pump: specification: 0.6mL/rep (0.6 milliliter of melt of revolution), its rotating speed is according to calculating such as finished silk fiber number, proportioning raw materials, spinning speed, stretching ratios.
Embodiment 1
Get the raw materials ready: in nylon 6 slice weight, take by weighing the PVP (mass ratio is 2: 1 PVP10000 and the mixture of PVP24000) of its weight 1%, 0.5% antioxidant (antioxidant 1010 and oxidation inhibitor 168, ratio is 1: 1), 0.3% dispersion agent 1 (whiteruss) and dispersion agent 2 (PEG600), ratio is 1: 1.
The preparation method: the nylon 6 slice that vacuum-drying is good (water ratio 600ppm) mixes in agitator with PVP, and then in agitator, add antioxidant (antioxidant 1010 and oxidation inhibitor 168), dispersion agent 1 (whiteruss) and dispersion agent 2 (PEG600) and stir, mix.Then mixture is poured in the hopper of twin screw extruder, melt blending is extruded, and nylon 6 melt temperatures are that 278 ℃, screw speed 25r/min, extrusion mould-outlet temperature are 240 ℃, pelletizing behind the metal track cooling check rod, and throughput is 2～4kg/h.The melt flow index of gained master batch is 11.0g/10min, and melting range is 160～180 ℃.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 30.0g/min for amount, the master batch pump is 1.5g/min for flow, is that 280 ℃, screw speed are that 18r/min and screw pressure are 70～80kg/cm at spinning temperature
2Down fused mixture melt is pushed through screw rod (containing static state, dynamic mixer), pump into spinning pack, after 40 orders sea sand filters, extrude through orifice (orifice is characterized as: diameter 0.25mm, length-to-diameter ratio 2.7) again through metering.Then in spinning nozzle ring blowing device in the wind-warm syndrome that blows out be 32 ℃, humidity be 40% and wind speed be cross air blow cooling under the 0.3m/s.Then oil through the oil thrower boundling through the cross air blow cooled fibers, the rate of oiling is 0.9%, 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 600m/min; Undrawn yarn is carried out the secondary drawing-off, and the secondary drafting multiple is 3.2 times, and hot drawing temperature heat dish is 90 ℃, and hot plate is 165 ℃.The filament number of the conventional fine-denier polyamide fiber of gained is 0.9dtex, and breaking tenacity is 4.10cN/dtex, and elongation is 26%, and the fiber rate of moisture absorption is 5.0%, oil length: 0.6%.
Embodiment 3
Get the raw materials ready: in nylon 6 slice weight, take by weighing the PVP (mass ratio is 2: 1 PVP10000 and the mixture of PVP24000) of its weight 2.4%, 0.8% antioxidant (antioxidant BHT and anti-oxidant DLTP, ratio 1: 1), 0.6% dispersion agent 1 (whiteruss) and dispersion agent 2 (PEG600), ratio is 1: 1.
The preparation method: the nylon 6 slice that vacuum-drying is good (water ratio 600ppm) mixes in agitator with PVP, and then in agitator, add antioxidant (antioxidant BHT and anti-oxidant DLTP), dispersion agent 1 (whiteruss) and dispersion agent 2 (PEG600) and stir, mix.Then mixture is poured in the hopper of twin screw extruder, melt blending is extruded, nylon 6 melt temperatures are that 278 ℃, screw speed 25r/min, extrusion mould-outlet temperature are 240 ℃, pelletizing behind the metal track cooling check rod, throughput is 2～4kg/h, the melt flow index of gained master batch is 11.0g/10min, and melting range is 160～180 ℃.The gained master batch is used for embodiment 4.
Embodiment 4
Nylon 6 slice after the vacuum-drying, master batch (water ratio 800ppm) are transported in the conventional spinning-drawing machine of twin screw, the nylon chips pump is 25.0g/min for amount, the master batch pump is 2.5g/min for flow, is that 280 ℃, screw speed are that 18r/min and screw pressure are 70～80kg/cm at spinning temperature
2Down fused mixture melt is pushed through screw rod (containing static state, dynamic mixer), pump into spinning pack, after 80 orders sea sand filters, extrude through orifice (orifice is characterized as: diameter 0.20mm, length-to-diameter ratio 3) 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 cross air blow cooling under the 0.4m/s.Then oil through the oil thrower boundling through the cross air blow cooled fibers, the rate 1.0% 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 800m/min; Undrawn yarn is carried out the secondary drawing-off, and the secondary drafting multiple is 3.6 times, and hot drawing temperature heat dish is 105 ℃, and hot plate is 170 ℃.The filament number of the conventional fine-denier polyamide fiber of gained is 0.6dtex, and breaking tenacity is 4.25cN/dtex, and elongation is 27%, and the fiber rate of moisture absorption is 6.5%, oil length: 0.9%.
Embodiment 5
Get the raw materials ready: in nylon 6 slice weight, take by weighing the PVP (mass ratio is 2: 1 PVP10000 and the mixture of PVP24000) of its weight 10%, 1% antioxidant (antioxidant 1010 and oxidation inhibitor 168, ratio=1: 1), 1.0% dispersion agent 1 (whiteruss) and dispersion agent 2 (PEG600), ratio is 1: 1.
The preparation method: the nylon 6 slice that vacuum-drying is good (water ratio 600ppm) mixes in agitator with PVP, and then in agitator, add antioxidant (antioxidant 1010 and oxidation inhibitor 168), dispersion agent 1 (whiteruss) and dispersion agent 2 (PEG600) and stir, mix.Then mixture is poured in the hopper of twin screw extruder, melt blending is extruded, and nylon 6 melt temperatures are that 278 ℃, screw speed 25r/min, extrusion mould-outlet temperature are 240 ℃, pelletizing behind the metal track cooling check rod, and throughput is 2～4kg/h.The melt flow index of gained master batch is 13.0g/10min, and melting range is 160～180 ℃.The gained master batch is used for embodiment 6.
Embodiment 6
Nylon 6 slice after the vacuum-drying, master batch (water ratio 900ppm) are transported in the conventional spinning-drawing machine of twin screw, the nylon chips pump is 30.0g/min for amount, the master batch pump is 3.0g/min for flow, is that 280 ℃, screw speed are that 18r/min and screw pressure are 70～80kg/cm at spinning temperature
2Down fused mixture melt is pushed through screw rod (containing static state, dynamic mixer), pump into spinning pack, after 60 orders sea sand filters, extrude through orifice (orifice is characterized as: diameter 0.15mm, 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 38 ℃, humidity be 45% and wind speed be cross air blow cooling under the 0.5m/s.Then oil through the oil thrower boundling through the cross air blow cooled fibers, the rate of oiling is 1.3%, 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 900m/min; Undrawn yarn is carried out the secondary drawing-off, and the secondary drafting multiple is 3.8 times, and hot drawing temperature heat dish is 110 ℃, and hot plate is 175 ℃.The filament number of the conventional fine-denier polyamide fiber of gained is 0.45dtex, and breaking tenacity is 4.40cN/dtex, and elongation is 30%, and the fiber rate of moisture absorption is 8.8%, oil length: 1.2%.
Embodiment 7
Get the raw materials ready: in nylon 6 slice weight, take by weighing the PVP (mass ratio is 2: 1 PVP2000 and the mixture of PVP10000) of its weight 10%, 1% antioxidant (antioxidant 1010 and anti-oxidant DLTP, ratio=1: 1), 1.0% dispersion agent 1 (whiteruss) and dispersion agent 2 (poly(lactic acid)), ratio is 1: 1.
The preparation method: the nylon 6 slice that vacuum-drying is good (water ratio 600ppm) mixes in agitator with PVP, and then in agitator, add antioxidant (antioxidant 1010 and anti-oxidant DLTP), dispersion agent 1 (whiteruss) and dispersion agent 2 (poly(lactic acid)) and stir, mix.Then mixture is poured in the hopper of twin screw extruder, melt blending is extruded, and nylon 6 melt temperatures are that 278 ℃, screw speed 25r/min, extrusion mould-outlet temperature are 240 ℃, pelletizing behind the metal track cooling check rod, and throughput is 2～4kg/h.The melt flow index of gained master batch is 13.0g/10min, and melting range is 160～180 ℃.The gained master batch is used for embodiment 8.
Embodiment 8
Nylon 6 slice after the vacuum-drying, master batch (water ratio 900ppm) are transported in the conventional spinning-drawing machine of twin screw, the nylon chips pump is 30.0g/min for amount, the master batch pump is 1.5g/min for flow, is that 280 ℃, screw speed are that 18r/min and screw pressure are 70～80kg/cm at spinning temperature
2Down fused mixture melt is pushed through screw rod (containing static state, dynamic mixer), pump into spinning pack, after 40 orders and the extra large sand filtration of 60 orders (1: 1), extrude through orifice (orifice is characterized as: diameter 0.18mm, length-to-diameter ratio 3.5) again through metering.Then in spinning nozzle ring blowing device in the wind-warm syndrome that blows out be 38 ℃, humidity be 55% and wind speed be cross air blow cooling under the 0.5m/s.Then oil through the oil thrower boundling through the cross air blow cooled fibers, the rate of oiling is 0.9%, 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 800m/min; Undrawn yarn is carried out the secondary drawing-off, and the secondary drafting multiple is 3.3 times, and hot drawing temperature heat dish is 110 ℃, and hot plate is 175 ℃.The filament number of the conventional fine-denier polyamide fiber of gained is 0.60dtex, and breaking tenacity is 4.10cN/dtex, and elongation is 27%, and the fiber rate of moisture absorption is 6.4%, oil length: 0.8%.
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 (7)
1. water absorbability denier/superfine denier nylon master granule, it is characterized in that, it is to be extruded by moisture-absorption modifier, antioxidant, dispersion agent and nylon 6 slice melt blending to make, wherein, add moisture-absorption modifier 1 ~ 10%, antioxidant 0. 1 ~ 1%, dispersion agent 0. 1 ~ 1% by nylon 6 slice weight, described moisture-absorption modifier is a polyvinylpyrrolidone, and it is in 1000 ~ 100000 one or more that described polyvinylpyrrolidone is selected from molecular weight; 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 200-2000.
2. the preparation method of the described water absorbability denier/superfine denier nylon master granule of claim 1, it is characterized in that, described preparation method comprises: with moisture-absorption modifier, 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 ℃.
3. the preparation method of water absorbability denier/superfine denier nylon master granule as claimed in claim 2 is characterized in that, described nylon 6 slice water ratio is below 600ppm; The moisture-absorption modifier water ratio is below 1000ppm.
4. water absorbability denier/superfine denier nylon; it is characterized in that; it is to add the spinning of the described water absorbability denier/superfine denier nylon master granule of claim 1 mixed melting by nylon 6 slice to make; the filament number of gained fiber is 0.45 ~ 1.0dtex; wherein, described master batch addition is 1 ~ 10% of a nylon 6 slice weight.
5. water absorbability denier/superfine denier nylon as claimed in claim 4 is characterized in that, described water absorbability denier/superfine denier nylon breaking tenacity is 3.8 ~ 4.8 cN/dtex, and elongation at break is 20 ~ 40%, and the rate of moisture absorption of fiber is 4 ~ 10%.
6. the preparation method of claim 4 or 5 described water absorbability denier/superfine denier nylons is characterized in that, described preparation method comprises the steps: successively
(1) mixed melting spinning: nylon 6 slice adds master batch and carries out the mixed melting spinning, and wherein, the screw pressure during fusion is 90 ~ 120kg/cm
2, screw speed is 15 ~ 30 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: 28 ~ 40 ℃ of wind-warm syndrome, humidity 40 ~ 60%, wind speed 0.3 ~ 0.5m/s,
(3) oil, boundling: finish is the polyamide fibre finish second distillation water miscible liquid of 8 ~ 12wt%; The rate of oiling is 0.5 ~ 1.5%,
(4) reel: spinning speed is 300 ~ 1000m/min,
(5) secondary drawing-off: drafting multiple is that 2.5 ~ 3.8 times, drawing temperature are 80 ~ 190 ℃, promptly gets water absorbability denier/superfine denier nylon product.
7. the preparation method of water absorbability denier/superfine denier nylon as claimed in claim 6 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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| CN103122494B (en) * | 2011-11-18 | 2016-04-20 | 东丽纤维研究所（中国）有限公司 | A kind of moisture absorption type polyester fiber and preparation method thereof |
| CN102877141A (en) * | 2012-08-17 | 2013-01-16 | 苏州市兴吴工程塑胶有限公司 | Direct spinning method suitable for chemical fibers |
| KR101459973B1 (en) * | 2013-12-04 | 2014-11-07 | 지에스칼텍스 주식회사 | Nylon blend composition having improved moisture regain and shrinkage, nylon based fiber manufactured with the composition and method for preparing the same |
| CN105088386A (en) * | 2015-09-02 | 2015-11-25 | 太仓市宏亿化纤有限公司 | Hygroscopic polyamide fiber processing technology |
| CN106283336B (en) * | 2016-08-08 | 2018-04-10 | 福建万鸿纺织有限公司 | A kind of comfortable nylon fabric of antibacterial and preparation method thereof |
| DK201700367A1 (en) * | 2017-06-21 | 2019-01-30 | Jonsman Innovation Aps | A hydrophilic polymer material |
| CN109881298A (en) * | 2019-03-12 | 2019-06-14 | 苏州申久高新纤维有限公司 | A kind of superfine composite adds elater and its processing technology |
| CN111234515A (en) * | 2020-01-15 | 2020-06-05 | 福建中锦新材料有限公司 | Water-absorbing nylon master batch for spinning and preparation method thereof |
| CN111286801A (en) * | 2020-03-26 | 2020-06-16 | 南通苏源化纤有限公司 | Preparation process of smooth high-moisture-absorption polyamide fiber |
| CN114318733B (en) * | 2021-12-01 | 2023-08-22 | 福州市晟浩纺织科技有限公司 | Preparation method of antibacterial nylon fabric |
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