CN102733002A - Preparation method of ultrafine composite fiber with high wet transmitting performance - Google Patents
Preparation method of ultrafine composite fiber with high wet transmitting performance Download PDFInfo
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- CN102733002A CN102733002A CN2012102084534A CN201210208453A CN102733002A CN 102733002 A CN102733002 A CN 102733002A CN 2012102084534 A CN2012102084534 A CN 2012102084534A CN 201210208453 A CN201210208453 A CN 201210208453A CN 102733002 A CN102733002 A CN 102733002A
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Abstract
The invention discloses a preparation method of an ultrafine composite fiber with high wet transmitting performance, comprising the following steps of: 1) firstly preparing a copolyester additive having melting point of 180-220 DEG C and intrinsic viscosity of 1.0-1.2 dl/g and containing aliphatic dibasic acid and aliphatic dihydric alcohol by the combination of melt polycondensation and solid state polycondensation; 2) granulating by melt blending of the additive, a polyolefin elastomer graft multi-monomer compatilizer and polypropylene resin in a double screw extruder so as to prepare dyeable modified polypropylene resin with the particle size of dispersed phase being less than 1 micron; and 3) using the dyeable modified polypropylene resin prepared from the step 2) as a scaffold, using polyamide as splinter, and splitting fiber through mechanical force in subsequent alkali deweighting or processing into the ultrafine composite fiber with filament number being less than 0.2 dtex. The ultrafine composite fiber prepared by the method is soft, and has characteristics of high thermal stability, good spinning performance and excellent moisture conductivity and moisture absorption performance.
Description
Technical field
The present invention relates to a kind of superfine composite fiber preparation method with high wet transmitting performance.Belong to the chemical fibre field.
Background technology
The method of composite spinning spinning superfine Denier fibre mainly contains sea-island-type composite spun and sliver type composite spinning; Be main mainly in the sliver type composite spinning wherein with polyester-nylon composite spinning; Utilize the non-compatibility of terylene and polyamide fibre; Following minute fibre of effect in back road alkali decrement or certain mechanical force makes superfine Denier fibre, is a kind of technology of comparative maturity.
Research shows, the polypropylene fibre after the thin dawnization except that the denominator with general fine count fiber as the advantages such as soft, elegant, close skin, also have good warming, breathe freely, lead wet, health, characteristics such as relaxed and comfortable.But, prepare the exploitation of superfine Denier fibre because polypropylene fibre be difficult for to adopt conventional dyeing to dye, thereby has influenced polypropylene with other macromolecular material carries out composite spinning.
Publication number CN101736416A discloses " preparation technology of a kind of thin dawn and superfine denier polypropylene fibers ", adopts conventional spin processes to obtain the thin dawn and the superfine denier polypropylene fibers at 0.5～2 dawn.Publication number CN1068603 discloses " manufacturing approach of thin dawn and superfine denier polypropylene fibers ", adopts multiple measure to stablize spinning technique; As being controlled at spinning temperature between 200～280 ℃; Select the high-flowability polypropylene of good thermal stability for use and with the wire winding speed spinning below 2000 meters/minute, and with the undrawn yarn high drafting, can be made into filament number was 0.2～2 dawn; Tensile strength was 4～8 gram/dawn, and elongation at break is 15～70% thin dawn and superfine denier polypropylene fibers.In order to realize the dyeable modified of polypropylene fibre; Resin specially for dyable fine denier polypropylene fibre and fiber preparation method also have more report; Like publication number CN1164594, " manufacturing approach of dyable fine denier polypropylene fibre " disclosed, a kind of employing acrylic resin and the blend of dyeing, modifying additive; Through granulation, melt spinning, or be the method for (1.11～2.22) dtex dyable fine denier polypropylene fibre directly through melt spinning manufacturing filament number.The dyeing, modifying additive is formed by DMT, ethylene glycol and monomer A, B, C copolymerization, and the inherent viscosity of this copolyesters ［ η ］ is 0.451～0.6, and fusing point is (200～260) ℃, and the percentage by weight of this copolyesters is (51～15) % in the blend.Te Kaiping 4-209824; A kind of " stainability polypropylene fibre and manufacturing approach thereof " disclosed, earlier with melt blendings such as stainability polymer such as polyester, polyamide and compatilizers, then by certain addition and polypropene blended; Carry out melt spinning, make the alloy fiber of disperse dye dyeable.
More than disclosed dyeable polypropylene fibre patent, mainly be that the melt spinning technology path through routine prepares dyeable fine-denier polypropylene.Holder part as with sliver type composite spinning is replaced by dyeable modified polypropylene, prepares average filament number less than the dyeable polypropylene of 0.2dtex and the composite fibre of polyamide fibre, then can realize better leading wet, moisture sorption effect.This is additive dispersed extremely important in the matrix polypropylene wherein, as disperseing particle diameter too big, is prone to produce broken end first, spinnability descends greatly even can't repiece; Second mechanical property descends significantly, and fiber does not have practical value.
Summary of the invention
In order to address the above problem, the object of the present invention is to provide a kind of superfine composite fiber preparation method with high wet transmitting performance, the present invention has the heat endurance height, and the spinning process performance is good, and is soft, lead the characteristics wet, that moisture pick-up properties is good.
For reaching above-mentioned purpose, the present invention adopts following technical scheme:
A kind of superfine composite fiber preparation method with high wet transmitting performance; Comprise the steps: 1) method that at first combines through melt polycondensation and solid phase polycondensation, make fusing point at 180～220 ℃, inherent viscosity 1.0～1.2dl/g, contain the copolyesters additive of aliphatic dibasic acid, aliphatic dihydroxy alcohol; 2) then with the compatilizer of additive, the many monomers of polyolefin elastomer grafting, and melt index at the acrylic resin (purchase in group of middle section and produce polypropylene dedicated resin of thin dawn) of 10～30g/10min; In the granulation of double screw extruder melt blending, make the dyeable modified acrylic resin of decentralized photo particle diameter less than 1 μ m; 3) the sliver type is washed the preparation of third composite fibre; With said step 2) preparation dyeable modified acrylic resin as support; Polyamide fibre is as sliver, fiber through after mechanical force in road alkali decrement or the processing, split into the superfine composite fiber of filament number less than 0.2dtex.
The preparation process of copolyesters additive is in the described step 1): with terephthalic acid (TPA), ethylene glycol is raw material, and the mol ratio of terephthalic acid (TPA) and ethylene glycol is 1: 1.2; Add in aliphatic binary acid, aliphatic dihydroxylic alcohols and the aliphatic polyester one or more, and addition accounts for the molar percentage 10～60% of terephthalic acid (TPA); The synthetic fusing point of method through melt polycondensation is at 180～220 ℃, the copolyesters of inherent viscosity 0.5～0.7dl/g; Then with copolyesters under 170～210 ℃, the condition of vacuum less than 1kpa, the solid phase polycondensation through 36～48 hours is further brought up to 1.0～1.2dl/g with inherent viscosity.
Described aliphatic binary acid adopts a kind of in succinic acid, hexanedioic acid, the decanedioic acid; Aliphatic dihydroxylic alcohols adopts 1, ammediol, 1, a kind of in 4-butanediol, 1, the 6-hexylene glycol; Aliphatic polyester adopts gathering the hexanedioic acid glycol ester, gather the hexanedioic acid butanediol ester, gathering a kind of in the hexanedioic acid hexylene glycol ester of molecular weight 1000～2000.
Described aliphatic binary acid adopts hexanedioic acid; Aliphatic dihydroxylic alcohols adopts 1, the 4-butanediol; Aliphatic polyester adopts and gathers the hexanedioic acid butanediol ester.
Described step 2) preparation process of dyeable modified acrylic resin is in: with the copolyesters additive of step 1) preparation and the compatilizer of the many monomers of polyolefin elastomer grafting; And melt index adds compatilizer at the acrylic resin of 10～30g/10min by additive and accounts for additive, compatilizer and acrylic resin total weight percent 5～17%, and the compatilizer addition is less than additive, compatilizer and acrylic resin total weight percent 5%; On double screw extruder, melt blending granulation under 200～250 ℃ the temperature conditions makes the dyeable modified acrylic resin that contains additive, and its decentralized photo particle diameter is less than 1 μ m.
The compatilizer of the many monomers of described polyolefin elastomer grafting adopts EPDM-g-MAH (EP rubbers grafted maleic anhydride), POE-g-(GMA-co-MAH), and (the polyolefin elastomer graft glycidyl methacrylate is a kind of in the maleic anhydride altogether.(purchasing) in the permanent brightness chemical industry of Yangzhou Co., Ltd
The sliver type is washed the preparation process of third composite fibre and is in the described step 3): with said step 2) the dyeable modified acrylic resin that makes is as support; Polyamide fibre is as sliver; Wherein dyeable modified acrylic resin accounts for total weight percent (dyeable modified acrylic resin and polyamide fibre) 60～80%; Carry out composite spinning, make POY-DTY.Fiber through after road alkali decrement or processing in mechanical force, split into the superfine fibre of filament number less than 0.2dtex, fiber can disperse dyeing.
Beneficial effect of the present invention is: the present invention because adopt fatty family binary acid and the copolyesters of dihydroxylic alcohols as additive; Both can reduce additive and polyacrylic fusing point is poor, because of the existence of aliphatic chain, improve and polyacrylic compatibility again; And compare with the polyether-type copolyesters; Heat endurance improves greatly, therefore, improves the spinning process performance greatly.Through taking to make earlier the copolyesters of inherent viscosity 0.5～0.7dl/g; Through solid phase polycondensation, further inherent viscosity is brought up to the method for 1.0～1.2dl/g then, when having overcome multiple aliphatic binary acid, dihydroxylic alcohols participation copolymerization; Molecular weight is difficult to improve; Be prone to produce various side reactions, cause degradation problem under the copolyesters quality, make copolyesters additive and polypropylene base that better viscosity match arranged.The compatilizer of the many monomers of polyolefin elastomer grafting of better compatibility is preferably all arranged with polypropylene and copolyesters, further improved additive dispersion effect in polypropylene base, the particle diameter that makes decentralized photo is less than 1 μ m.With this dyeable modified acrylic resin,, make super fine denier third chinlon composite fiber of filament number less than 0.2dtex and available disperse dyeing through the method for sliver type composite spinning.The fabric that is made into this fiber has good softness, leads performance such as wet, moisture absorption, is particularly suitable for making high-grade towel, bath towel etc.
Description of drawings
Fig. 1 is the structural representation between support of the present invention and the sliver.
The specific embodiment
Through specific embodiment, the present invention is done further description below.Wherein: the method for testing of dispersed phase size: the blend batten that will extrude from twin-screw, brittle failure in liquid nitrogen is carried out ESEM (SEM) analysis to section then, at last with Photo shop calculating average grain diameter; Inherent viscosity method of testing: press GB-T 14189-2008, detect as solvent with phenol and tetrachloroethanes 1: 1.The relative viscosity method of testing of polyamide fibre 6: with the concentrated sulfuric acid is solvent, detects with dark type viscometer.C Kam composite yarn dyeing test: 7 liters of water 100g sock belt and 85g of sodium hydroxide, alkali reduction at 100 ℃ for 30min, then remove the sock belt, according to GB-T6508-2001 polyester filament yarn dyeing uniformity test methods rating.Shade polyamide fibre main and wherein partly contrasts.
Embodiment 1
A kind of superfine composite fiber preparation method of present embodiment with high wet transmitting performance; Comprise the steps: 1) method that at first combines through melt polycondensation and solid phase polycondensation; With terephthalic acid (TPA), ethylene glycol is raw material, and the mol ratio of terephthalic acid (TPA) and ethylene glycol is 1: 1.2; The hexanedioic acid and 1 of the molar percentage 30% that accounts for terephthalic acid (TPA) that add the molar percentage 30% account for described terephthalic acid (TPA), the 4-butanediol, synthetic fusing point is at 180 ℃, the copolyesters of inherent viscosity 0.5dl/g; Then with copolyesters under 170 ℃, the condition of vacuum less than 1kpa, solid phase polycondensation through 36 hours is further brought up to 1.0dl/g with inherent viscosity, fusing point is at 180 ℃ copolyesters additive; 2) the described inherent viscosity that accounts for additive, compatilizer and acrylic resin total weight percent 5% with the step 1) preparation is 1.0dl/g copolyesters additive and the compatilizer EPDM-g-MAH that accounts for the many monomers of polyolefin elastomer grafting of additive, compatilizer and acrylic resin total weight percent 2%; And melt index at the acrylic resin of 30g/10min on double screw extruder; Melt blending granulation under 200 ℃ the temperature conditions; Make the dyeable modified acrylic resin that contains additive, the average grain diameter that records decentralized photo is 0.85 μ m.See shown in the table 1 that table 1 is the preparation technology of dyeable modified acrylic resin in the embodiment of the invention and display list as a result.3) with said step 2) preparation dyeable modified acrylic resin as support 1, polyamide fibre is as sliver 2, and is as shown in Figure 1; Earlier dyeable modified acrylic resin is carried out drying, make the section moisture content less than 50PPM, polyamide fibre is then selected dry section for use, and inherent viscosity is 2.3dl/g.Melt extrude, carry, measure through double screw extruder respectively; Percentage by weight by dyeable modified acrylic resin and polyamide fibre is 60: 40 entering sliver type composite spining modules; 265 ℃ of control spinning temperatures; 2500 meters/minute of spinning speeds make the superfine composite fiber (pre-oriented yarn (POY) that 165dtex/36f * 16 are cut apart) with high wet transmitting performance.POY makes the DTY silk of cutting apart 100dtex/36f * 16 again through texturing craft.See shown in the table 2 that table 2 is the preparation technology of the superfine composite fiber of high wet transmitting performance in the embodiment of the invention and display list as a result.
Present embodiment because adopt fatty family binary acid and the copolyesters of dihydroxylic alcohols as additive; Both can reduce additive and polyacrylic fusing point is poor, because of the existence of aliphatic chain, improve and polyacrylic compatibility again; And compare with the polyether-type copolyesters; Heat endurance improves greatly, therefore, improves the spinning process performance greatly.Through taking to make earlier the copolyesters of inherent viscosity 0.5～0.7dl/g; Through solid phase polycondensation, further inherent viscosity is brought up to the method for 1.0～1.2dl/g then, when having overcome multiple aliphatic binary acid, dihydroxylic alcohols participation copolymerization; Molecular weight is difficult to improve; Be prone to produce various side reactions, cause degradation problem under the copolyesters quality, make copolyesters additive and polypropylene base that better viscosity match arranged.The compatilizer of the many monomers of polyolefin elastomer grafting of better compatibility is preferably all arranged with polypropylene and copolyesters, further improved additive dispersion effect in polypropylene base, the particle diameter that makes decentralized photo is less than 1 μ m.With this dyeable modified acrylic resin,, make super fine denier third chinlon composite fiber of filament number less than 0.2dtex and available disperse dyeing through the method for sliver type composite spinning.The fabric that is made into this fiber has good softness, leads performance such as wet, moisture absorption, is particularly suitable for making high-grade towel, bath towel etc.
Embodiment 2
The preparation process of present embodiment and embodiment 1 are basic identical; Different is: the inherent viscosity that will account for additive, compatilizer and acrylic resin total weight percent 10% is the copolyesters of 1.0dl/g; The polypropylene of EPDM-g-MAH and melt index 30g/10min that accounts for additive, compatilizer and acrylic resin total weight percent 2% is through double screw extruder; With 200 ℃ of blend granulations, make the dyeable modified acrylic resin that contains additive, the average grain diameter that records decentralized photo is 0.91 μ m.See shown in the table 1 that table 1 is the preparation technology of dyeable modified acrylic resin in the embodiment of the invention and display list as a result.Dyeable modified acrylic resin and polyamide fibre percentage by weight are 70:30.Make superfine composite fiber (pre-oriented yarn (POY) that 165dtex/36f * 16 are cut apart) with high wet transmitting performance.POY makes the DTY silk of cutting apart 100dtex/36f * 16 again through texturing craft.See shown in the table 2 that table 2 is the preparation technology of the superfine composite fiber of high wet transmitting performance in the embodiment of the invention and display list as a result.
Present embodiment because adopt fatty family binary acid and the copolyesters of dihydroxylic alcohols as additive; Both can reduce additive and polyacrylic fusing point is poor, because of the existence of aliphatic chain, improve and polyacrylic compatibility again; And compare with the polyether-type copolyesters; Heat endurance improves greatly, therefore, improves the spinning process performance greatly.Through taking to make earlier the copolyesters of inherent viscosity 0.5～0.7dl/g; Through solid phase polycondensation, further inherent viscosity is brought up to the method for 1.0～1.2dl/g then, when having overcome multiple aliphatic binary acid, dihydroxylic alcohols participation copolymerization; Molecular weight is difficult to improve; Be prone to produce various side reactions, cause degradation problem under the copolyesters quality, make copolyesters additive and polypropylene base that better viscosity match arranged.The compatilizer of the many monomers of polyolefin elastomer grafting of better compatibility is preferably all arranged with polypropylene and copolyesters, further improved additive dispersion effect in polypropylene base, the particle diameter that makes decentralized photo is less than 1 μ m.With this dyeable modified acrylic resin,, make super fine denier third chinlon composite fiber of filament number less than 0.2dtex and available disperse dyeing through the method for sliver type composite spinning.The fabric that is made into this fiber has good softness, leads performance such as wet, moisture absorption, is particularly suitable for making high-grade towel, bath towel etc.
Embodiment 3
The preparation process of present embodiment and embodiment 1 are basic identical; Different is: the inherent viscosity that will account for additive, compatilizer and acrylic resin total weight percent 15% is the copolyesters of 1.0dl/g; The polypropylene of EPDM-g-MAH and melt index 30g/10min that accounts for additive, compatilizer and acrylic resin total weight percent 2% is through double screw extruder; With 220 ℃ of blend granulations, make the dyeable modified acrylic resin that contains additive, the average grain diameter that records decentralized photo is 0.95 μ m.See shown in the table 1 that table 1 is the preparation technology of dyeable modified acrylic resin in the embodiment of the invention and display list as a result.Dyeable modified acrylic resin and polyamide fibre percentage by weight are 80: 20.Make superfine composite fiber (pre-oriented yarn (POY) that 165dtex/36f * 16 are cut apart) with high wet transmitting performance.POY makes the DTY silk of cutting apart 100dtex/36f * 16 again through texturing craft.See shown in the table 2 that table 2 is the preparation technology of the superfine composite fiber of high wet transmitting performance in the embodiment of the invention and display list as a result.
Present embodiment because adopt fatty family binary acid and the copolyesters of dihydroxylic alcohols as additive; Both can reduce additive and polyacrylic fusing point is poor, because of the existence of aliphatic chain, improve and polyacrylic compatibility again; And compare with the polyether-type copolyesters; Heat endurance improves greatly, therefore, improves the spinning process performance greatly.Through taking to make earlier the copolyesters of inherent viscosity 0.5～0.7dl/g; Through solid phase polycondensation, further inherent viscosity is brought up to the method for 1.0～1.2dl/g then, when having overcome multiple aliphatic binary acid, dihydroxylic alcohols participation copolymerization; Molecular weight is difficult to improve; Be prone to produce various side reactions, cause degradation problem under the copolyesters quality, make copolyesters additive and polypropylene base that better viscosity match arranged.The compatilizer of the many monomers of polyolefin elastomer grafting of better compatibility is preferably all arranged with polypropylene and copolyesters, further improved additive dispersion effect in polypropylene base, the particle diameter that makes decentralized photo is less than 1 μ m.With this dyeable modified acrylic resin,, make super fine denier third chinlon composite fiber of filament number less than 0.2dtex and available disperse dyeing through the method for sliver type composite spinning.The fabric that is made into this fiber has good softness, leads performance such as wet, moisture absorption, is particularly suitable for making high-grade towel, bath towel etc.
Embodiment 4
A kind of superfine composite fiber preparation method of present embodiment with high wet transmitting performance; Comprise the steps: 1) method that at first combines through melt polycondensation and solid phase polycondensation; With terephthalic acid (TPA), ethylene glycol is raw material, and the mol ratio of terephthalic acid (TPA) and ethylene glycol is 1: 1.2; The hexanedioic acid and 1 of the molar percentage 15% that accounts for terephthalic acid (TPA) that add the molar percentage 15% account for described terephthalic acid (TPA), the 4-butanediol, synthetic fusing point is at 220 ℃, the copolyesters of inherent viscosity 0.6dl/g; Then with copolyesters under 190 ℃, the condition of vacuum less than 1kpa, solid phase polycondensation through 48 hours is further brought up to 1.2dl/g with inherent viscosity, fusing point is at 220 ℃ copolyesters additive; 2) the described inherent viscosity that accounts for additive, compatilizer and acrylic resin total weight percent 10% with the step 1) preparation is 1.2dl/g copolyesters additive and the compatilizer EPDM-g-MAH that accounts for the many monomers of polyolefin elastomer grafting of additive, compatilizer and acrylic resin total weight percent 2%; And melt index at the acrylic resin of 10g/10min on double screw extruder; Melt blending granulation under 230 ℃ the temperature conditions; Make the dyeable modified acrylic resin that contains additive, the average grain diameter that records decentralized photo is 0.92 μ m.See shown in the table 1 that table 1 is the preparation technology of dyeable modified acrylic resin in the embodiment of the invention and display list as a result.3) with said step 2) preparation dyeable modified acrylic resin as support 1, polyamide fibre is as sliver 2, and is as shown in Figure 1; Earlier dyeable modified acrylic resin is carried out drying, make the section moisture content less than 50PPM, polyamide fibre is then selected dry section for use, and inherent viscosity is 2.3dl/g.Melt extrude, carry, measure through double screw extruder respectively; Percentage by weight by dyeable modified acrylic resin and polyamide fibre is 75: 25 entering sliver type composite spining modules; 265 ℃ of control spinning temperatures; 2500 meters/minute of spinning speeds make the superfine composite fiber (pre-oriented yarn (POY) that 165dtex/36f * 16 are cut apart) with high wet transmitting performance.POY makes the DTY silk of cutting apart 100dtex/36f * 16 again through texturing craft.See shown in the table 2 that table 2 is the preparation technology of the superfine composite fiber of high wet transmitting performance in the embodiment of the invention and display list as a result.
Present embodiment because adopt fatty family binary acid and the copolyesters of dihydroxylic alcohols as additive; Both can reduce additive and polyacrylic fusing point is poor, because of the existence of aliphatic chain, improve and polyacrylic compatibility again; And compare with the polyether-type copolyesters; Heat endurance improves greatly, therefore, improves the spinning process performance greatly.Through taking to make earlier the copolyesters of inherent viscosity 0.5～0.7dl/g; Through solid phase polycondensation, further inherent viscosity is brought up to the method for 1.0～1.2dl/g then, when having overcome multiple aliphatic binary acid, dihydroxylic alcohols participation copolymerization; Molecular weight is difficult to improve; Be prone to produce various side reactions, cause degradation problem under the copolyesters quality, make copolyesters additive and polypropylene base that better viscosity match arranged.The compatilizer of the many monomers of polyolefin elastomer grafting of better compatibility is preferably all arranged with polypropylene and copolyesters, further improved additive dispersion effect in polypropylene base, the particle diameter that makes decentralized photo is less than 1 μ m.With this dyeable modified acrylic resin,, make super fine denier third chinlon composite fiber of filament number less than 0.2dtex and available disperse dyeing through the method for sliver type composite spinning.The fabric that is made into this fiber has good softness, leads performance such as wet, moisture absorption, is particularly suitable for making high-grade towel, bath towel etc.
Embodiment 5
A kind of superfine composite fiber preparation method of present embodiment with high wet transmitting performance; Comprise the steps: 1) method that at first combines through melt polycondensation and solid phase polycondensation; With terephthalic acid (TPA), ethylene glycol is raw material, and the mol ratio of terephthalic acid (TPA) and ethylene glycol is 1: 1.2; Add molar percentage 6% molecular weight account for described terephthalic acid (TPA) and be 1000 gather the hexanedioic acid butanediol ester, synthetic fusing point is at 200 ℃, the copolyesters of inherent viscosity 0.7dl/g; Then with copolyesters under 175 ℃, the condition of vacuum less than 1kpa, solid phase polycondensation through 48 hours is further brought up to 1.2dl/g with inherent viscosity, fusing point is at 200 ℃ copolyesters additive; 2) the described inherent viscosity that accounts for additive, compatilizer and acrylic resin total weight percent 10% with the step 1) preparation is 1.2dl/g copolyesters additive and the compatilizer EPDM-g-MAH that accounts for the many monomers of polyolefin elastomer grafting of additive, compatilizer and acrylic resin total weight percent 2%; And melt index at the acrylic resin of 10g/10min on double screw extruder; Melt blending granulation under 230 ℃ the temperature conditions; Make the dyeable modified acrylic resin that contains additive, the average grain diameter that records decentralized photo is 0.81 μ m.See shown in the table 1 that table 1 is the preparation technology of dyeable modified acrylic resin in the embodiment of the invention and display list as a result.3) with said step 2) preparation dyeable modified acrylic resin as support 1, polyamide fibre is as sliver 2, and is as shown in Figure 1; Earlier dyeable modified acrylic resin is carried out drying, make the section moisture content less than 50PPM, polyamide fibre is then selected dry section for use, and inherent viscosity is 2.7dl/g.Melt extrude, carry, measure through double screw extruder respectively; Percentage by weight by dyeable modified acrylic resin and polyamide fibre is 70: 30 entering sliver type composite spining modules; 265 ℃ of control spinning temperatures; 2500 meters/minute of spinning speeds make the superfine composite fiber (pre-oriented yarn (POY) that 165dtex/36f * 16 are cut apart) with high wet transmitting performance.POY makes the DTY silk of cutting apart 100dtex/36f * 16 again through texturing craft.See shown in the table 2 that table 2 is the preparation technology of the superfine composite fiber of high wet transmitting performance in the embodiment of the invention and display list as a result.
Present embodiment because adopt fatty family binary acid and the copolyesters of dihydroxylic alcohols as additive; Both can reduce additive and polyacrylic fusing point is poor, because of the existence of aliphatic chain, improve and polyacrylic compatibility again; And compare with the polyether-type copolyesters; Heat endurance improves greatly, therefore, improves the spinning process performance greatly.Through taking to make earlier the copolyesters of inherent viscosity 0.5～0.7dl/g; Through solid phase polycondensation, further inherent viscosity is brought up to the method for 1.0～1.2dl/g then, when having overcome multiple aliphatic binary acid, dihydroxylic alcohols participation copolymerization; Molecular weight is difficult to improve; Be prone to produce various side reactions, cause degradation problem under the copolyesters quality, make copolyesters additive and polypropylene base that better viscosity match arranged.The compatilizer of the many monomers of polyolefin elastomer grafting of better compatibility is preferably all arranged with polypropylene and copolyesters, further improved additive dispersion effect in polypropylene base, the particle diameter that makes decentralized photo is less than 1 μ m.With this dyeable modified acrylic resin,, make super fine denier third chinlon composite fiber of filament number less than 0.2dtex and available disperse dyeing through the method for sliver type composite spinning.The fabric that is made into this fiber has good softness, leads performance such as wet, moisture absorption, is particularly suitable for making high-grade towel, bath towel etc.
Embodiment 6
The preparation process of present embodiment and embodiment 5 are basic identical; Different is: the inherent viscosity that will account for additive, compatilizer and acrylic resin total weight percent 10% is the copolyesters of 1.2dl/g; The POE-g-(GMA-co-MAH) that accounts for additive, compatilizer and acrylic resin total weight percent 2% and the acrylic resin of melt index 10g/10min are through double screw extruder; With 230 ℃ of blend granulations; Make the dyeable modified acrylic resin that contains additive, the average grain diameter that records decentralized photo is 0.79 μ m.See shown in the table 1 that table 1 is the preparation technology of dyeable modified acrylic resin in the embodiment of the invention and display list as a result.Dyeable modified acrylic resin and polyamide fibre percentage by weight are 65: 35.Make superfine composite fiber (pre-oriented yarn (POY) that 165dtex/36f * 16 are cut apart) with high wet transmitting performance.POY makes the DTY silk of cutting apart 100dtex/36f * 16 again through texturing craft.See shown in the table 2 that table 2 is the preparation technology of the superfine composite fiber of high wet transmitting performance in the embodiment of the invention and display list as a result.
Present embodiment because adopt fatty family binary acid and the copolyesters of dihydroxylic alcohols as additive; Both can reduce additive and polyacrylic fusing point is poor, because of the existence of aliphatic chain, improve and polyacrylic compatibility again; And compare with the polyether-type copolyesters; Heat endurance improves greatly, therefore, improves the spinning process performance greatly.Through taking to make earlier the copolyesters of inherent viscosity 0.5～0.7dl/g; Through solid phase polycondensation, further inherent viscosity is brought up to the method for 1.0～1.2dl/g then, when having overcome multiple aliphatic binary acid, dihydroxylic alcohols participation copolymerization; Molecular weight is difficult to improve; Be prone to produce various side reactions, cause degradation problem under the copolyesters quality, make copolyesters additive and polypropylene base that better viscosity match arranged.The compatilizer of the many monomers of polyolefin elastomer grafting of better compatibility is preferably all arranged with polypropylene and copolyesters, further improved additive dispersion effect in polypropylene base, the particle diameter that makes decentralized photo is less than 1 μ m.With this dyeable modified acrylic resin,, make super fine denier third chinlon composite fiber of filament number less than 0.2dtex and available disperse dyeing through the method for sliver type composite spinning.The fabric that is made into this fiber has good softness, leads performance such as wet, moisture absorption, is particularly suitable for making high-grade towel, bath towel etc.
Embodiment 7
A kind of superfine composite fiber preparation method of present embodiment with high wet transmitting performance; Comprise the steps: 1) method that at first combines through melt polycondensation and solid phase polycondensation; With terephthalic acid (TPA), ethylene glycol is raw material, and the mol ratio of terephthalic acid (TPA) and ethylene glycol is 1: 1.2; Add molar percentage 3% molecular weight account for described terephthalic acid (TPA) and be 2000 gather the hexanedioic acid butanediol ester, synthetic fusing point is at 205 ℃, the copolyesters of inherent viscosity 0.7dl/g; Then with copolyesters under 180 ℃, the condition of vacuum less than 1kpa, solid phase polycondensation through 36 hours is further brought up to 1.1dl/g with inherent viscosity, fusing point is at 205 ℃ copolyesters additive; 2) the described inherent viscosity that accounts for additive, compatilizer and acrylic resin total weight percent 10% with the step 1) preparation is 1.1dl/g copolyesters additive and the compatilizer POE-g-(GMA-co-MAH) that accounts for the many monomers of polyolefin elastomer grafting of additive, compatilizer and acrylic resin total weight percent 2%; And melt index at the acrylic resin of 20g/10min on double screw extruder; Melt blending granulation under 230 ℃ the temperature conditions; Make the dyeable modified acrylic resin that contains additive, the average grain diameter that records decentralized photo is 0.78 μ m.See shown in the table 1 that table 1 is the preparation technology of dyeable modified acrylic resin in the embodiment of the invention and display list as a result.3) with said step 2) preparation dyeable modified acrylic resin as support 1, polyamide fibre is as sliver 2, and is as shown in Figure 1; Earlier dyeable modified acrylic resin is carried out drying, make the section moisture content less than 50PPM, polyamide fibre is then selected dry section for use, and inherent viscosity is 2.5dl/g.Melt extruding, carry, measure through double screw extruder respectively, is to get into sliver type composite spining module, 285 ℃ of control spinning temperatures at 80: 20 by the percentage by weight of dyeable modified acrylic resin and polyamide fibre; 2000 meters/minute of the first hot-rolling speed, 80 ℃ of temperature, 3800 meters/minute of the second hot-rolling speed; 130 ℃ of temperature make the superfine composite fiber (FDY that 75dtex/24f * 16 are cut apart) with high wet transmitting performance.See shown in the table 2 that table 2 is the preparation technology of the superfine composite fiber of high wet transmitting performance in the embodiment of the invention and display list as a result.
Present embodiment because adopt fatty family binary acid and the copolyesters of dihydroxylic alcohols as additive; Both can reduce additive and polyacrylic fusing point is poor, because of the existence of aliphatic chain, improve and polyacrylic compatibility again; And compare with the polyether-type copolyesters; Heat endurance improves greatly, therefore, improves the spinning process performance greatly.Through taking to make earlier the copolyesters of inherent viscosity 0.5～0.7dl/g; Through solid phase polycondensation, further inherent viscosity is brought up to the method for 1.0～1.2dl/g then, when having overcome multiple aliphatic binary acid, dihydroxylic alcohols participation copolymerization; Molecular weight is difficult to improve; Be prone to produce various side reactions, cause degradation problem under the copolyesters quality, make copolyesters additive and polypropylene base that better viscosity match arranged.The compatilizer of the many monomers of polyolefin elastomer grafting of better compatibility is preferably all arranged with polypropylene and copolyesters, further improved additive dispersion effect in polypropylene base, the particle diameter that makes decentralized photo is less than 1 μ m.With this dyeable modified acrylic resin,, make super fine denier third chinlon composite fiber of filament number less than 0.2dtex and available disperse dyeing through the method for sliver type composite spinning.The fabric that is made into this fiber has good softness, leads performance such as wet, moisture absorption, is particularly suitable for making high-grade towel, bath towel etc.
Comparative example 1
The preparation process of present embodiment and embodiment 2 are basic identical, and different is: do not add compatilizer, and additive dispersed relatively poor in dyeable modified acrylic resin, the average grain diameter that records decentralized photo is 3.70 μ m.Dyeable modified acrylic resin with gained as shown in table 1 carries out drying, makes the section moisture content less than 50PPM, and polyamide fibre is then selected dry section for use, and inherent viscosity is 2.3dl/g.Melt extrude, carry, measure through double screw extruder respectively; Get into sliver type composite spining module in dyeable modified acrylic resin and 60: 40 ratio of polyamide fibre; 285 ℃ of control spinning temperatures, 2500 meters/minute of spinning speeds, the result seriously can't reel because of the silk that wafts.As shown in table 2.
Comparative example 2
The preparation process of present embodiment and embodiment 5 are basic identical, and different is: do not add compatilizer, and additive dispersed relatively poor in dyeable modified acrylic resin, the average grain diameter that records decentralized photo is 3.15 μ m.As shown in table 1.With the dyeable modified acrylic resin and the inherent viscosity of gained is the polyester of 0.68dl/g, carries out drying respectively, makes the section moisture content less than 50PPM, and polyamide fibre is then selected dry section for use, and inherent viscosity is 2.7dl/g.Melt extrude, carry, measure through double screw extruder respectively; Ratio in dyeable modified acrylic resin and polyamide fibre 80:20 gets into sliver type composite spining module, 285 ℃ of control spinning temperatures, 2000 meters/minute of the first hot-rolling speed; 80 ℃ of temperature; 3800 meters/minute of the second hot-rolling speed, 130 ℃ of temperature, silk seriously can't be reeled because of wafing.As shown in table 2.
Table 1
Table 2
Claims (7)
1. superfine composite fiber preparation method with high wet transmitting performance; It is characterized in that comprising the steps: 1) method that at first combines through melt polycondensation and solid phase polycondensation, make fusing point at 180～220 ℃, inherent viscosity 1.0～1.2dl/g, contain the copolyesters additive of aliphatic dibasic acid, aliphatic dihydroxy alcohol; 2) then with the compatilizer of additive, the many monomers of polyolefin elastomer grafting, and melt index at the acrylic resin of 10～30g/10min, in the granulation of double screw extruder melt blending, make the dyeable modified acrylic resin of decentralized photo particle diameter less than 1 μ m; 3) the sliver type is washed the preparation of third composite fibre; With said step 2) preparation dyeable modified acrylic resin as support; Polyamide fibre is as sliver, fiber through after mechanical force in road alkali decrement or the processing, split into the superfine composite fiber of filament number less than 0.2dtex.
2. a kind of superfine composite fiber preparation method according to claim 1 with high wet transmitting performance; The preparation process that it is characterized in that copolyesters additive in the described step 1) is: with terephthalic acid (TPA), ethylene glycol is raw material, and the mol ratio of terephthalic acid (TPA) and ethylene glycol is 1:1.2; Add in aliphatic binary acid, aliphatic dihydroxylic alcohols and the aliphatic polyester one or more, and addition accounts for the molar percentage 10～60% of terephthalic acid (TPA); The synthetic fusing point of method through melt polycondensation is at 180～220 ℃, the copolyesters of inherent viscosity 0.5～0.7dl/g; Then with copolyesters under 170～210 ℃, the condition of vacuum less than 1 kpa, the solid phase polycondensation through 36～48 hours is further brought up to 1.0～1.2dl/g with inherent viscosity.
3. a kind of superfine composite fiber preparation method with high wet transmitting performance according to claim 2 is characterized in that: described aliphatic binary acid adopts a kind of in succinic acid, hexanedioic acid, the decanedioic acid; Aliphatic dihydroxylic alcohols adopts 1, ammediol, 1, a kind of in 4-butanediol, 1, the 6-hexylene glycol; Aliphatic polyester adopts gathering the hexanedioic acid glycol ester, gather the hexanedioic acid butanediol ester, gathering a kind of in the hexanedioic acid hexylene glycol ester of molecular weight 1000～2000.
4. a kind of superfine composite fiber preparation method with high wet transmitting performance according to claim 3 is characterized in that: described aliphatic binary acid adopts hexanedioic acid; Aliphatic dihydroxylic alcohols adopts 1, the 4-butanediol; Aliphatic polyester adopts and gathers the hexanedioic acid butanediol ester.
5. a kind of superfine composite fiber preparation method according to claim 1 with high wet transmitting performance; It is characterized in that described step 2) in the preparation process of dyeable modified acrylic resin be: with the copolyesters additive of step 1) preparation and the compatilizer of the many monomers of polyolefin elastomer grafting; And melt index adds compatilizer at the acrylic resin of 10～30g/10min by additive and accounts for additive, compatilizer and acrylic resin total weight percent 5～17%, and the compatilizer addition is less than additive, compatilizer and acrylic resin total weight percent 5%; On double screw extruder, melt blending granulation under 200～250 ℃ the temperature conditions makes the dyeable modified acrylic resin that contains additive, and its decentralized photo particle diameter is less than 1 μ m.
6. a kind of superfine composite fiber preparation method with high wet transmitting performance according to claim 5 is characterized in that: the compatilizer of the many monomers of described polyolefin elastomer grafting adopts a kind of among EPDM-g-MAH, the POE-g-(GMA-co-MAH).
7. a kind of superfine composite fiber preparation method according to claim 1 with high wet transmitting performance; It is characterized in that: the sliver type is washed the preparation process of third composite fibre and is in the described step 3): with said step 2) the dyeable modified acrylic resin that makes is as support; Polyamide fibre is as sliver; Wherein dyeable modified acrylic resin account for dyeable modified acrylic resin and the polyamide fibre total weight percent 60～80%, carry out composite spinning, make POY-DTY; Fiber through after road alkali decrement or processing in mechanical force, split into the superfine fibre of filament number less than 0.2dtex.
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| CN103668669A (en) * | 2013-11-27 | 2014-03-26 | 江苏中新资源集团有限公司 | Moisture absorption wicking fabric and method for manufacturing same |
| CN103911684A (en) * | 2012-12-29 | 2014-07-09 | 海盐金霞化纤有限公司 | Method for preparation of colored special-shaped elastic monofilament by polyether ester/PTT composite spinning |
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| CN103572404B (en) * | 2012-08-08 | 2016-03-09 | 东丽纤维研究所（中国）有限公司 | A kind of island-in-sea type composite fiber |
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| CN103911683B (en) * | 2012-12-29 | 2016-03-02 | 浙江金霞新材料科技有限公司 | A kind of polyether ester/PTT Compound spinning prepares the method for colored profiled elasticity multifilament fiber |
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| CN105839248A (en) * | 2016-05-25 | 2016-08-10 | 浙江古纤道股份有限公司 | Differential-shrinkage superfine composite draw textured yarn and processing technology thereof |
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