CN102719934A - Method for preparing superfine dyeable polypropylene fiber by sea-island composite spinning method - Google Patents
Method for preparing superfine dyeable polypropylene fiber by sea-island composite spinning method Download PDFInfo
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Abstract
The invention discloses a method for preparing superfine dyeable polypropylene fiber by a sea-island composite spinning method. The method comprises the following steps: (1), copolyester additive is prepared through the method of combining melt phase polycondensation and solid phase polycondensation; (2), the additive, compatilizer for polyolefin elastomer to graft multiple monomers, and polypropylene resin are subjected to melt-blending granulation in a double-screw extruder, and the dyeable modified polypropylene resin with the dispersed phase grain diameter less than 1 mum is prepared; and (3), the dyeable modified polypropylene resin prepared in the step (2) is used as island, alkaline solubility polyester is used as sea, and the sea-island composite processing is carried out; and the fiber is subjected to decrement by the later alkali, and the superfine dyeable polypropylene fiber with the monofilament fineness less than 0.2dtex is prepared. According to the superfine dyeable polypropylene fiber prepared by the method, the thermostability is high, the spinning processability is good, and fabric woven by the fiber has the superior properties of lightness, mildness, breathability and warm keeping, and is particularly suitable for high-grade bedding, high-grade underwear and the like.
Description
Technical field
The present invention relates to the method that a kind of island composite spinning method prepares ultra-fine dyeable polypropylene fibre.Belong to the chemical fibre field.
Background technology
Conventional thick denier polypropylene fibers feel is the wax shape, and gas permeability, hygroscopicity are poor, adds that nonpolarity group on the conventional polypropylene molecular chain, degree of crystallinity are high, and the polypropylene fibre dyeability is poor, has limited it in the application of taking, the field is spun by family.Polypropylene filament yarn 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; Dyeable modifiedly then overcome present polypropylene fibre and generally adopt original liquid coloring to produce coloured silk, be difficult to adapt to small lot, the changeable market demand.Therefore, the thin dawnization of polypropylene fibre, the dyeable modified focus that becomes people's research and development.
Like publication number CN101736416A, " preparation technology of a kind of thin dawn and superfine denier polypropylene fibers " disclosed, adopt conventional spin processes to obtain the fine 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 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, the fibre single thread fiber number that obtains is greater than 0.5dtex.As to prepare the dyed super fine denier polypropylene fibre of filament number less than 0.2dtex, additive dispersed extremely important in the matrix polypropylene wherein as disperseing particle diameter too big, is prone to produce broken end, spinnability descends greatly even can't repiece first; 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 island composite spinning method to prepare the method for ultra-fine dyeable polypropylene fibre; The present invention has the heat endurance height, and the spinning process performance is good, the fabric of using this fiber to be made into; Have good slim and graceful, close skin, ventilative, warming performance, be particularly suitable for high-grade bedding, high-grade cold-proof underwear etc.
For reaching above-mentioned purpose, the present invention adopts following technical scheme:
A kind of island composite spinning method prepares the method for ultra-fine dyeable polypropylene fibre; Comprise the steps: 1) method that at first combines through melt polycondensation and solid phase polycondensation, make fusing point at 180～220 ℃, inherent viscosity 0.8～1.0dl/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 30～50g/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) with said step 2) the dyeable modified acrylic resin of preparation is as the island, and alkali soluble polyester is done the sea, carries out the island Compound Machining; Fiber through after after the road alkali decrement, the polypropylene filament fiber number is less than the ultra-fine dyeable polypropylene fibre of 0.2dtex, and can disperse dyeing and stamp.
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 0.4～0.6dl/g; Then with copolyesters under 170～210 ℃, the condition of vacuum less than 1kpa, the solid phase polycondensation through 24～48 hours is further brought up to 0.8～1.0dl/g with inherent viscosity.
Described aliphatic binary acid adopts a kind of in succinic acid, adipic acid, the decanedioic acid; Aliphatic dihydroxylic alcohols adopts 1, ammediol, 1, a kind of in 4-butanediol, 1, the 6-hexylene glycol; Aliphatic polyester adopt molecular weight 1000～2000 polyethylene glycol adipate, poly adipate succinic acid ester, gather a kind of in the adipic acid hexylene glycol ester.
Described aliphatic binary acid adopts adipic acid; Aliphatic dihydroxylic alcohols adopts 1, the 4-butanediol; Aliphatic polyester adopts poly adipate succinic acid 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 30～50g/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 a kind of among EPDM-g-MAH, the POE-g-(GMA-co-MAH).(purchasing) in the permanent brightness chemical industry of Yangzhou Co., Ltd
In the described step 3) with step 2) the dyeable modified acrylic resin of preparation is as the island, alkali soluble polyester (alkali soluble polyester chip that the brilliant magnificent high-new colored fiber in Shaoxin City Co., Ltd produces) is done the sea, carries out the island Compound Machining; Wherein dyeable modified acrylic resin and alkali soluble polyester weight ratio are 70～80:30～20, carry out the island Compound Machining; Fiber through after after the road alkali decrement, the polypropylene filament fiber number is less than the ultra-fine dyeable polypropylene fibre of 0.2dtex, and can disperse dyeing and stamp.
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 0.4～0.6dl/g; Through solid phase polycondensation, further inherent viscosity is brought up to the method for 0.8～1.0dl/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, through the method for island composite spinning, make filament number less than 0.2dtex, and the super fine denier dyeable polypropylene of available disperse dyeing and stamp.The fabric that is made into this fiber has good slim and graceful, close skin, performance such as ventilative, warming, is particularly suitable for high-grade bedding, high-grade cold-proof underwear etc.
The specific embodiment
Pass through specific embodiment below; The present invention is done further description, wherein: the method for testing of dispersed phase size: the blend batten that will extrude from twin-screw, brittle failure in liquid nitrogen; Then section is carried out ESEM (SEM) analysis, calculate average grain diameter with Photo shop at last; Inherent viscosity method of testing: press GB-T 14189-2008, detect as solvent with phenol and tetrachloroethanes 1:1.Haidao Si staining test: 7 liters of water and 70g 100g sock with sodium hydroxide, alkali reduction at 100 ℃ for 30min, then remove the sock belt, according to GB-T6508-2001 polyester filament yarn dyeing uniformity test method ratings.The terylene thread of shade and same specification contrasts.
Embodiment 1
A kind of island composite spinning method of present embodiment prepares the method for ultra-fine dyeable polypropylene fibre; 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 adipic 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 0.4dl/g; Then with copolyesters under 170 ℃, the condition of vacuum less than 1kpa, solid phase polycondensation through 36 hours is further brought up to 0.8dl/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 0.8dl/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 50g/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 0.87 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 described step 2) the dyeable modified acrylic resin that makes be island and inherent viscosity for the 0.7dl/g alkali soluble polyester for the sea, carry out drying respectively, make the section moisture content less than 50PPM.Melt extrude, carry, measure through double screw extruder then; Weight ratio in dyeable modified acrylic resin and polyamide fibre is the ratio entering island composite spining module of 80:20; 250 ℃ of control spinning temperatures; 2800 meters/minute of spinning speeds make the pre-oriented yarn (POY) on 180dtex/24f * 21 islands.POY makes the DTY silk on 100dtex/24f * 21 islands again through texturing craft.See shown in the table 2 that table 2 prepares the preparation technology of ultra-fine dyeable polypropylene fibre and display list as a result for island composite spinning method in the embodiment of the invention.
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 0.4～0.6dl/g; Through solid phase polycondensation, further inherent viscosity is brought up to the method for 0.8～1.0dl/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, through the method for island composite spinning, make filament number less than 0.2dtex, and the super fine denier dyeable polypropylene of available disperse dyeing and stamp.The fabric that is made into this fiber has good slim and graceful, close skin, performance such as ventilative, warming, is particularly suitable for high-grade bedding, high-grade cold-proof underwear 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 0.8dl/g; The acrylic resin of EPDM-g-MAH and melt index 50g/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 0.92 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.The weight ratio of dyeable modified acrylic resin and polyamide fibre is 70:30.Make the pre-oriented yarn (POY) on 180dtex/24f * 21 islands.POY makes the DTY silk on 100dtex/24f * 21 islands again through texturing craft.See shown in the table 2 that table 2 prepares the preparation technology of ultra-fine dyeable polypropylene fibre and display list as a result for island composite spinning method in the embodiment of the invention.
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 0.4～0.6dl/g; Through solid phase polycondensation, further inherent viscosity is brought up to the method for 0.8～1.0dl/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, through the method for island composite spinning, make filament number less than 0.2dtex, and the super fine denier dyeable polypropylene of available disperse dyeing and stamp.The fabric that is made into this fiber has good slim and graceful, close skin, performance such as ventilative, warming, is particularly suitable for high-grade bedding, high-grade cold-proof underwear 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 0.8dl/g; The acrylic resin of EPDM-g-MAH and melt index 50g/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 0.98 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.The weight ratio of dyeable modified acrylic resin and polyamide fibre is 75:25.Make the pre-oriented yarn (POY) on 180dtex/24f * 21 islands.POY makes the DTY silk on 100dtex/24f * 21 islands again through texturing craft.See shown in the table 2 that table 2 prepares the preparation technology of ultra-fine dyeable polypropylene fibre and display list as a result for island composite spinning method in the embodiment of the invention.
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 0.4～0.6dl/g; Through solid phase polycondensation, further inherent viscosity is brought up to the method for 0.8～1.0dl/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, through the method for island composite spinning, make filament number less than 0.2dtex, and the super fine denier dyeable polypropylene of available disperse dyeing and stamp.The fabric that is made into this fiber has good slim and graceful, close skin, performance such as ventilative, warming, is particularly suitable for high-grade bedding, high-grade cold-proof underwear 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 adipic 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 36 hours is further brought up to 1.0dl/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 1.0dl/g copolyesters additive and the compatilizer EPDM-g-MAH that accounts for the many monomers of polyolefin elastomer grafting of additive, compatilizer and fine acrylic resin total weight percent 2%; And melt index at the acrylic resin of 30g/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 0.95 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.3) with described step 2) the dyeable modified acrylic resin that makes be island and inherent viscosity for the 0.70dl/g alkali soluble polyester for the sea, carry out drying respectively, make the section moisture content less than 50PPM.Melt extrude, carry, measure through double screw extruder then; Weight ratio in dyeable modified acrylic resin and polyamide fibre is the ratio entering island composite spining module of 80:20; 250 ℃ of control spinning temperatures; 2800 meters/minute of spinning speeds make the pre-oriented yarn (POY) on 180dtex/24f * 21 islands.POY makes the DTY silk on 100dtex/24f * 21 islands again through texturing craft.See shown in the table 2 that table 2 prepares the preparation technology of ultra-fine dyeable polypropylene fibre and display list as a result for island composite spinning method in the embodiment of the invention.
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 0.4～0.6dl/g; Through solid phase polycondensation, further inherent viscosity is brought up to the method for 0.8～1.0dl/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, through the method for island composite spinning, make filament number less than 0.2dtex, and the super fine denier dyeable polypropylene of available disperse dyeing and stamp.The fabric that is made into this fiber has good slim and graceful, close skin, performance such as ventilative, warming, is particularly suitable for high-grade bedding, high-grade cold-proof underwear 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 poly adipate succinic acid ester, synthetic fusing point is at 205 ℃, the copolyesters of inherent viscosity 0.5dl/g; Then with copolyesters under 180 ℃, the condition of vacuum less than 1kpa, solid phase polycondensation through 36 hours is further brought up to 1.0dl/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 1.0dl/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 230 ℃ the temperature conditions; Make the dyeable modified acrylic resin that contains additive, the average grain diameter that records decentralized photo is 0.74 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 described step 2) the dyeable modified acrylic resin that makes be island and inherent viscosity for the 0.80dl/g alkali soluble polyester for the sea, carry out drying respectively, make the section moisture content less than 50PPM.Melt extrude, carry, measure through double screw extruder then; Weight ratio in dyeable modified acrylic resin and polyamide fibre is the ratio entering island composite spining module of 80:20; 260 ℃ of control spinning temperatures; 2800 meters/minute of spinning speeds make the pre-oriented yarn (POY) on 180dtex/24f * 21 islands.POY makes the DTY silk on 100dtex/24f * 21 islands again through texturing craft.See shown in the table 2 that table 2 prepares the preparation technology of ultra-fine dyeable polypropylene fibre and display list as a result for island composite spinning method in the embodiment of the invention.
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 0.4～0.6dl/g; Through solid phase polycondensation, further inherent viscosity is brought up to the method for 0.8～1.0dl/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, through the method for island composite spinning, make filament number less than 0.2dtex, and the super fine denier dyeable polypropylene of available disperse dyeing and stamp.The fabric that is made into this fiber has good slim and graceful, close skin, performance such as ventilative, warming, is particularly suitable for high-grade bedding, high-grade cold-proof underwear 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 1.0dl/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 30g/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 0.78 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.The weight ratio of dyeable modified acrylic resin and polyamide fibre is 72:28.Make the pre-oriented yarn (POY) on 180dtex/24f * 21 islands.POY makes the DTY silk on 100dtex/24f * 21 islands again through texturing craft.See shown in the table 2 that table 2 prepares the preparation technology of ultra-fine dyeable polypropylene fibre and display list as a result for island composite spinning method in the embodiment of the invention.
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 0.4～0.6dl/g; Through solid phase polycondensation, further inherent viscosity is brought up to the method for 0.8～1.0dl/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, through the method for island composite spinning, make filament number less than 0.2dtex, and the super fine denier dyeable polypropylene of available disperse dyeing and stamp.The fabric that is made into this fiber has good slim and graceful, close skin, performance such as ventilative, warming, is particularly suitable for high-grade bedding, high-grade cold-proof underwear 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 poly adipate succinic acid ester, synthetic fusing point is at 210 ℃, the copolyesters of inherent viscosity 0.5dl/g; Then with copolyesters under 185 ℃, the condition of vacuum less than 1kpa, solid phase polycondensation through 24 hours is further brought up to 0.9dl/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 0.9dl/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 40g/10mi n 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 0.70 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 described step 2) the dyeable modified acrylic resin that makes be island and inherent viscosity for the 0.80dl/g alkali soluble polyester for the sea, carry out drying respectively, make the section moisture content less than 50PPM.Melt extrude, carry, measure through double screw extruder then; Weight ratio in dyeable modified acrylic resin and polyamide fibre is the ratio entering island composite spining module of 70:30,260 ℃ of control spinning temperatures, 1500 meters/minute of the first hot-rolling speed; 75 ℃ of temperature; 3200 meters/minute of the second hot-rolling speed, 130 ℃ of temperature make the FDY on 75dtex/24f * 21 islands.See shown in the table 2 that table 2 prepares the preparation technology of ultra-fine dyeable polypropylene fibre and display list as a result for island composite spinning method in the embodiment of the invention.
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 0.4～0.6dl/g; Through solid phase polycondensation, further inherent viscosity is brought up to the method for 0.8～1.0dl/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, through the method for island composite spinning, make filament number less than 0.2dtex, and the super fine denier dyeable polypropylene of available disperse dyeing and stamp.The fabric that is made into this fiber has good slim and graceful, close skin, performance such as ventilative, warming, is particularly suitable for high-grade bedding, high-grade cold-proof underwear 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 3.75 μ m.As shown in table 1.With the dyeable modified acrylic resin and the inherent viscosity of gained is the alkali soluble polyester of 0.70dl/g, carries out drying respectively, makes the section moisture content less than 50PPM.Melt extrude, carry, measure through double screw extruder then; Ratio in island and extra large 80:20 gets into the island composite spining module, 250 ℃ of control spinning temperatures, 2800 meters/minute of spinning speeds; Carry out the production of the compound POY silk in island, 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 3.35 μ m.As shown in table 1.With the dyeable modified acrylic resin and the inherent viscosity of comparative example 2 gained is the alkali soluble polyester of 0.80dl/g, carries out drying respectively, makes the section moisture content less than 50PPM.Melt extrude, carry, measure through double screw extruder then, in the ratio entering island composite spining module of island and extra large 70:30,260 ℃ of control spinning temperatures; 1500 meters/minute of the first hot-rolling speed; 75 ℃ of temperature, 3200 meters/minute of the second hot-rolling speed, 130 ℃ of temperature; Carry out the production of the compound FDY silk in island, silk seriously can't be reeled because of wafing.
As shown in table 2.
Table 1
Table 2
Claims (7)
1. an island composite spinning method prepares the method for ultra-fine dyeable polypropylene fibre; 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 0.8～1.0dl/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 30～50g/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) with said step 2) the dyeable modified acrylic resin of preparation is as the island, and alkali soluble polyester is done the sea, carries out the island Compound Machining; Fiber through after after the road alkali decrement, the polypropylene filament fiber number is less than the ultra-fine dyeable polypropylene fibre of 0.2dtex.
2. a kind of island according to claim 1 composite spinning method prepares the method for ultra-fine dyeable polypropylene fibre; 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 0.4～0.6dl/g; Then with copolyesters under 170～210 ℃, the condition of vacuum less than 1 kpa, the solid phase polycondensation through 24～48 hours is further brought up to 0.8～1.0dl/g with inherent viscosity.
3. a kind of island according to claim 2 composite spinning method prepares the method for ultra-fine dyeable polypropylene fibre, it 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 island according to claim 3 composite spinning method prepares the method for ultra-fine dyeable polypropylene fibre, it 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 island according to claim 1 composite spinning method prepares the method for ultra-fine dyeable polypropylene fibre; 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 30～50g/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 island according to claim 5 composite spinning method prepares the method for ultra-fine dyeable polypropylene fibre, it 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 island according to claim 1 composite spinning method prepares the method for ultra-fine dyeable polypropylene fibre; It is characterized in that: in the described step 3) with step 2) preparation dyeable modified acrylic resin as the island; Alkali soluble polyester is done the sea, carries out the island Compound Machining; Wherein dyeable modified acrylic resin and alkali soluble polyester weight ratio are 70～80:30～20, carry out the island Compound Machining; Fiber through after after the road alkali decrement, the polypropylene filament fiber number is less than the ultra-fine dyeable polypropylene fibre of 0.2dtex, and can disperse dyeing and stamp.
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