CN102719934B - 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 a kind of island composite spinning method and prepare the method for ultra-fine dyeable polypropylene fibre.Belong to chemical fibre field.
Background technology
Conventional thick denier polypropylene fibers feel is wax-like, and gas permeability, hygroscopicity are poor, adds that nonpolarity group in conventional polypropylene molecular chain, degree of crystallinity are high, and Polypropylene Fibre Dyeing poor performance, has limited it in the application of taking, field is spun by family.Polypropylene filament yarn after the thin dawn is except the denominator with general fine count fiber is as the advantages such as soft, elegant, pro-skin, also have good warming, breathe freely, lead wet, health, the feature such as relaxed and comfortable; Dyeable modifiedly overcome current polypropylene fibre and generally adopt original liquid coloring to produce color silk, be difficult to adapt to small lot, the changeable market demand.Therefore, the thin dawn of polypropylene fibre, the dyeable modified focus that becomes people's research and development.
As 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, " manufacture method of thin dawn and superfine denier polypropylene fibers " disclosed, adopt many kinds of measures to stablize spinning technique, as spinning temperature being controlled between 200～280 ℃, select the high-flowability polypropylene of good thermal stability and with 2000 ms/min of following wire winding speed spinning, and by undrawn yarn high drafting, can be made into filament number was 0.2～2 dawn, tensile strength is 4～8 grams/dawn, thin dawn and superfine denier polypropylene fibers that elongation at break is 15～70%.
In order to realize the dyeable modified of polypropylene fibre, the existing more report of preparation method of resin specially for dyable fine denier polypropylene fibre and fiber, as publication number CN1164594, " manufacture method 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 through melt spinning manufacture filament number, be directly the method for (1.11 ~ 2.22) dtex dyable fine denier polypropylene fibre.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 in blend, the percentage by weight of this copolyesters is (51 ~ 15) %.Unexamined Patent 4-209824, a kind of " stainability polypropylene fibre and manufacture method thereof " disclosed, first by melt blendings such as the 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.
Disclosed dyeable polypropylene fibre patent, is mainly to prepare dyeable fine-denier polypropylene by conventional melt spinning technology path above, and the fibre single thread fiber number obtaining is greater than 0.5dtex.As prepared the dyed polypropylene fiber in carding process that filament number is less than 0.2dtex, wherein the dispersiveness of additive in matrix polypropylene is extremely important, as too large in disperseed particle diameter, and easily producing first that broken end, spinnability decline even greatly cannot repiece; Second mechanical property significantly declines, and fiber is without 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, it is high that the present invention has heat endurance, spinning process performance is good, the fabric being made into this fiber, there is good slim and graceful, pro-skin, ventilative, warming performance, be particularly suitable for high-grade bedding, high-grade cold-proof underwear etc.
For reaching above-mentioned object, the present invention adopts following technical scheme:
A kind of island composite spinning method is prepared the method for ultra-fine dyeable polypropylene fibre, comprise the steps: 1) method that first combines by melt polycondensation and solid phase polycondensation, make fusing point at 180～220 ℃, inherent viscosity 0.8～1.0dl/g, the copolyesters additive that contains aliphatic dibasic acid, aliphatic dihydroxy alcohol; 2) acrylic resin (be purchased from Zhong Ke group and produce polypropylene dedicated resin of thin dawn) at 30～50g/10min by the compatilizer of additive, the many monomers of polyolefin elastomer grafting and melt index then, in the granulation of double screw extruder melt blending, make the dyeable modified acrylic resin that Dispersed Phase Size is less than 1 μ m; 3) using described step 2) the dyeable modified acrylic resin prepared is as island, and alkali soluble polyester is done sea, carries out island Compound Machining; After fiber Jing Hou road alkali decrement, polypropylene filament fiber number is less than the ultra-fine dyeable polypropylene fibre of 0.2dtex, and can disperse dyeing and stamp.
In described step 1), the preparation process of copolyesters additive is: take terephthalic acid (TPA), ethylene glycol is raw material, and the mol ratio of terephthalic acid (TPA) and ethylene glycol is 1:1.2; Add one or more in aliphatic binary acid, aliphatic dihydroxylic alcohols and aliphatic polyester, and addition accounts for the molar percentage 10～60% of terephthalic acid (TPA); The synthetic fusing point of method by melt polycondensation is at 180～220 ℃, the copolyesters of inherent viscosity 0.4～0.6dl/g; Then copolyesters is less than under the condition of 1kpa at 170～210 ℃, vacuum, the solid phase polycondensation through 24～48 hours, further brings up to 0.8～1.0dl/g by inherent viscosity.
Described aliphatic binary acid adopts a kind of in succinic acid, adipic acid, decanedioic acid; Aliphatic dihydroxylic alcohols adopts a kind of in 1,3-PD, BDO, 1,6-hexylene glycol; Aliphatic polyester adopts a kind of in the polyethylene glycol adipate, poly adipate succinic acid ester, poly-adipic acid hexylene glycol ester of molecular weight 1000～2000.
Described aliphatic binary acid adopts adipic acid; Aliphatic dihydroxylic alcohols adopts BDO; Aliphatic polyester adopts poly adipate succinic acid ester.
Described step 2) in, the preparation process of dyeable modified acrylic resin is: the compatilizer of copolyesters additive prepared by step 1) and the many monomers of polyolefin elastomer grafting, and melt index adds compatilizer at the acrylic resin of 30～50g/10min by additive and account for additive, compatilizer and acrylic resin total weight percent 5～17%, and compatilizer addition is less than additive, compatilizer and acrylic resin total weight percent 5%; On double screw extruder, melt blending granulation under the temperature conditions of 200～250 ℃, makes the dyeable modified acrylic resin containing additive, and its Dispersed Phase Size is less than 1 μ m.
The compatilizer of the described many monomers of polyolefin elastomer grafting adopts EPDM-g-MAH, POE-g-(GMA-co-MAH) in a kind of.(being purchased from Yangzhou Heng Hui Chemical Co., Ltd.)
In described step 3) using step 2) the dyeable modified acrylic resin prepared is as island, alkali soluble polyester (alkali soluble polyester chip that Shaoxin City brilliant magnificent high-new colored fiber Co., Ltd produces) is done sea, carries out island Compound Machining; Wherein dyeable modified acrylic resin and alkali soluble polyester weight ratio are 70～80:30～20, carry out island Compound Machining; After fiber Jing Hou road alkali decrement, 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 is owing to adopting the copolyesters of fatty family binary acid and dihydroxylic alcohols as additive, both can reduce additive and polyacrylic fusing point is poor, again because of the existence of aliphatic chain, improve and polyacrylic compatibility, and compare with polyether-type copolyesters, heat endurance improves greatly, therefore, greatly improves spinning process performance.By taking first to make the copolyesters of inherent viscosity 0.4～0.6dl/g, then pass through solid phase polycondensation, further inherent viscosity is brought up to the method for 0.8～1.0dl/g, while having overcome multiple aliphatic binary acid, dihydroxylic alcohols participation copolymerization, molecular weight is difficult to improve, easily produce various side reactions, cause the problems such as copolyesters Quality Down, make copolyesters additive and polypropylene base have better viscosity match.Preferably all there is the compatilizer of the many monomers of polyolefin elastomer grafting of better compatibility with polypropylene and copolyesters, further improved additive dispersion effect in polypropylene base, make the particle diameter of decentralized photo be less than 1 μ m.With this dyeable modified acrylic resin, by the method for island composite spinning, make filament number and be less than 0.2dtex, and the super fine denier dyeable polypropylene of available disperse dyeing and stamp.The fabric being made into this fiber, has good slim and graceful, pro-skin, the performance such as ventilative, warming, is particularly suitable for high-grade bedding, high-grade cold-proof underwear etc.
The specific embodiment
Below by specific embodiment, the invention will be further described, wherein: the method for testing of dispersed phase size: by the blend batten from twin-screw extrusion, brittle failure in liquid nitrogen, then section is carried out to ESEM (SEM) analysis, finally with Photo shop, calculate average grain diameter; Inherent viscosity method of testing: press GB-T 14189-2008, detect as solvent with phenol and tetrachloroethanes 1:1.Haidao staining test: 7 liters of water added to 100g and 70g Sork with sodium hydroxide, an alkali reduction at 100 ℃ 30min, then remove Sork belt, according to GB-T6508-2001 polyester filament yarn dyeing uniformity test methods rating.The terylene thread of shade and same specification compares.
Embodiment 1
A kind of island composite spinning method of the present embodiment is prepared the method for ultra-fine dyeable polypropylene fibre, comprise the steps: 1) method that first combines by melt polycondensation and solid phase polycondensation, take terephthalic acid (TPA), ethylene glycol is raw material, and the mol ratio of terephthalic acid (TPA) and ethylene glycol is 1:1.2; Add the adipic acid of the molar percentage 30% that accounts for described terephthalic acid (TPA) and account for the BDO of the molar percentage 30% of terephthalic acid (TPA), synthetic fusing point is at 180 ℃, the copolyesters of inherent viscosity 0.4dl/g; Then copolyesters is less than under the condition of 1kpa at 170 ℃, vacuum, the solid phase polycondensation through 36 hours, further brings up to inherent viscosity 0.8dl/g, and fusing point is at the copolyesters additive of 180 ℃; 2) the described inherent viscosity that accounts for additive, compatilizer and acrylic resin total weight percent 5% of being prepared by step 1) 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 the temperature conditions of 200 ℃, make the dyeable modified acrylic resin containing additive, the average grain diameter that records decentralized photo is 0.87 μ m.Be shown in Table 1, table 1 is preparation technology and the result display list of dyeable modified acrylic resin in the embodiment of the present invention.3) by described step 2) the dyeable modified acrylic resin that makes be island and inherent viscosity be 0.7dl/g alkali soluble polyester for sea, be dried respectively, the moisture content that makes to cut into slices is less than 50PPM.Then through double screw extruder, melt extrude, carry, measure, the ratio that is 80:20 in the weight ratio of dyeable modified acrylic resin and polyamide fibre enters island composite spining module, control 250 ℃ of spinning temperatures, 2800 ms/min of spinning speeds, make the pre-oriented yarn (POY) on 180dtex/24f ×21 island.POY, again through texturing craft, makes the DTY silk on 100dtex/24f ×21 island.Be shown in Table 2, table 2 is preparation technology and the result display list that in the embodiment of the present invention, island composite spinning method is prepared ultra-fine dyeable polypropylene fibre.
The present embodiment is owing to adopting the copolyesters of fatty family binary acid and dihydroxylic alcohols as additive, both can reduce additive and polyacrylic fusing point is poor, again because of the existence of aliphatic chain, improve and polyacrylic compatibility, and compare with polyether-type copolyesters, heat endurance improves greatly, therefore, greatly improves spinning process performance.By taking first to make the copolyesters of inherent viscosity 0.4～0.6dl/g, then pass through solid phase polycondensation, further inherent viscosity is brought up to the method for 0.8～1.0dl/g, while having overcome multiple aliphatic binary acid, dihydroxylic alcohols participation copolymerization, molecular weight is difficult to improve, easily produce various side reactions, cause the problems such as copolyesters Quality Down, make copolyesters additive and polypropylene base have better viscosity match.Preferably all there is the compatilizer of the many monomers of polyolefin elastomer grafting of better compatibility with polypropylene and copolyesters, further improved additive dispersion effect in polypropylene base, make the particle diameter of decentralized photo be less than 1 μ m.With this dyeable modified acrylic resin, by the method for island composite spinning, make filament number and be less than 0.2dtex, and the super fine denier dyeable polypropylene of available disperse dyeing and stamp.The fabric being made into this fiber, has good slim and graceful, pro-skin, the performance such as ventilative, warming, is particularly suitable for high-grade bedding, high-grade cold-proof underwear etc.
Embodiment 2
The preparation process of the present embodiment is substantially the same manner as Example 1, difference is: the copolyesters that is 0.8dl/g by the inherent viscosity that accounts for additive, compatilizer and acrylic resin total weight percent 10%, account for the EPDM-g-MAH of additive, compatilizer and acrylic resin total weight percent 2% and the acrylic resin of melt index 50g/10min through double screw extruder, with 200 ℃ of blend granulations, make the dyeable modified acrylic resin containing additive, the average grain diameter that records decentralized photo is 0.92 μ m.Be shown in Table 1, table 1 is preparation technology and the result display list of dyeable modified acrylic resin in the embodiment of the present invention.The weight ratio of dyeable modified acrylic resin and polyamide fibre is 70:30.Make the pre-oriented yarn (POY) on 180dtex/24f ×21 island.POY, again through texturing craft, makes the DTY silk on 100dtex/24f ×21 island.Be shown in Table 2, table 2 is preparation technology and the result display list that in the embodiment of the present invention, island composite spinning method is prepared ultra-fine dyeable polypropylene fibre.
The present embodiment is owing to adopting the copolyesters of fatty family binary acid and dihydroxylic alcohols as additive, both can reduce additive and polyacrylic fusing point is poor, again because of the existence of aliphatic chain, improve and polyacrylic compatibility, and compare with polyether-type copolyesters, heat endurance improves greatly, therefore, greatly improves spinning process performance.By taking first to make the copolyesters of inherent viscosity 0.4～0.6dl/g, then pass through solid phase polycondensation, further inherent viscosity is brought up to the method for 0.8～1.0dl/g, while having overcome multiple aliphatic binary acid, dihydroxylic alcohols participation copolymerization, molecular weight is difficult to improve, easily produce various side reactions, cause the problems such as copolyesters Quality Down, make copolyesters additive and polypropylene base have better viscosity match.Preferably all there is the compatilizer of the many monomers of polyolefin elastomer grafting of better compatibility with polypropylene and copolyesters, further improved additive dispersion effect in polypropylene base, make the particle diameter of decentralized photo be less than 1 μ m.With this dyeable modified acrylic resin, by the method for island composite spinning, make filament number and be less than 0.2dtex, and the super fine denier dyeable polypropylene of available disperse dyeing and stamp.The fabric being made into this fiber, has good slim and graceful, pro-skin, the performance such as ventilative, warming, is particularly suitable for high-grade bedding, high-grade cold-proof underwear etc.
Embodiment 3
The preparation process of the present embodiment is substantially the same manner as Example 1, difference is: the copolyesters that is 0.8dl/g by the inherent viscosity that accounts for additive, compatilizer and acrylic resin total weight percent 15%, account for the EPDM-g-MAH of additive, compatilizer and acrylic resin total weight percent 2% and the acrylic resin of melt index 50g/10min through double screw extruder, with 220 ℃ of blend granulations, make the dyeable modified acrylic resin containing additive, the average grain diameter that records decentralized photo is 0.98 μ m.Be shown in Table 1, table 1 is preparation technology and the result display list of dyeable modified acrylic resin in the embodiment of the present invention.The weight ratio of dyeable modified acrylic resin and polyamide fibre is 75:25.Make the pre-oriented yarn (POY) on 180dtex/24f ×21 island.POY, again through texturing craft, makes the DTY silk on 100dtex/24f ×21 island.Be shown in Table 2, table 2 is preparation technology and the result display list that in the embodiment of the present invention, island composite spinning method is prepared ultra-fine dyeable polypropylene fibre.
The present embodiment is owing to adopting the copolyesters of fatty family binary acid and dihydroxylic alcohols as additive, both can reduce additive and polyacrylic fusing point is poor, again because of the existence of aliphatic chain, improve and polyacrylic compatibility, and compare with polyether-type copolyesters, heat endurance improves greatly, therefore, greatly improves spinning process performance.By taking first to make the copolyesters of inherent viscosity 0.4～0.6dl/g, then pass through solid phase polycondensation, further inherent viscosity is brought up to the method for 0.8～1.0dl/g, while having overcome multiple aliphatic binary acid, dihydroxylic alcohols participation copolymerization, molecular weight is difficult to improve, easily produce various side reactions, cause the problems such as copolyesters Quality Down, make copolyesters additive and polypropylene base have better viscosity match.Preferably all there is the compatilizer of the many monomers of polyolefin elastomer grafting of better compatibility with polypropylene and copolyesters, further improved additive dispersion effect in polypropylene base, make the particle diameter of decentralized photo be less than 1 μ m.With this dyeable modified acrylic resin, by the method for island composite spinning, make filament number and be less than 0.2dtex, and the super fine denier dyeable polypropylene of available disperse dyeing and stamp.The fabric being made into this fiber, has good slim and graceful, pro-skin, the 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 with high wet transmitting performance of the present embodiment, comprise the steps: 1) method that first combines by melt polycondensation and solid phase polycondensation, take terephthalic acid (TPA), ethylene glycol is raw material, and the mol ratio of terephthalic acid (TPA) and ethylene glycol is 1:1.2; Add the adipic acid of the molar percentage 15% that accounts for described terephthalic acid (TPA) and account for the BDO of the molar percentage 15% of terephthalic acid (TPA), synthetic fusing point is at 220 ℃, the copolyesters of inherent viscosity 0.6dl/g; Then copolyesters is less than under the condition of 1kpa at 190 ℃, vacuum, the solid phase polycondensation through 36 hours, further brings up to inherent viscosity 1.0dl/g, and fusing point is at the copolyesters additive of 220 ℃; 2) the described inherent viscosity that accounts for additive, compatilizer and acrylic resin total weight percent 10% of being prepared by step 1) 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 the temperature conditions of 230 ℃, make the dyeable modified acrylic resin containing additive, the average grain diameter that records decentralized photo is 0.95 μ m.Be shown in Table 1, table 1 is preparation technology and the result display list of dyeable modified acrylic resin in the embodiment of the present invention.3) by described step 2) the dyeable modified acrylic resin that makes be island and inherent viscosity be 0.70dl/g alkali soluble polyester for sea, be dried respectively, the moisture content that makes to cut into slices is less than 50PPM.Then through double screw extruder, melt extrude, carry, measure, the ratio that is 80:20 in the weight ratio of dyeable modified acrylic resin and polyamide fibre enters island composite spining module, control 250 ℃ of spinning temperatures, 2800 ms/min of spinning speeds, make the pre-oriented yarn (POY) on 180dtex/24f ×21 island.POY, again through texturing craft, makes the DTY silk on 100dtex/24f ×21 island.Be shown in Table 2, table 2 is preparation technology and the result display list that in the embodiment of the present invention, island composite spinning method is prepared ultra-fine dyeable polypropylene fibre.
The present embodiment is owing to adopting the copolyesters of fatty family binary acid and dihydroxylic alcohols as additive, both can reduce additive and polyacrylic fusing point is poor, again because of the existence of aliphatic chain, improve and polyacrylic compatibility, and compare with polyether-type copolyesters, heat endurance improves greatly, therefore, greatly improves spinning process performance.By taking first to make the copolyesters of inherent viscosity 0.4～0.6dl/g, then pass through solid phase polycondensation, further inherent viscosity is brought up to the method for 0.8～1.0dl/g, while having overcome multiple aliphatic binary acid, dihydroxylic alcohols participation copolymerization, molecular weight is difficult to improve, easily produce various side reactions, cause the problems such as copolyesters Quality Down, make copolyesters additive and polypropylene base have better viscosity match.Preferably all there is the compatilizer of the many monomers of polyolefin elastomer grafting of better compatibility with polypropylene and copolyesters, further improved additive dispersion effect in polypropylene base, make the particle diameter of decentralized photo be less than 1 μ m.With this dyeable modified acrylic resin, by the method for island composite spinning, make filament number and be less than 0.2dtex, and the super fine denier dyeable polypropylene of available disperse dyeing and stamp.The fabric being made into this fiber, has good slim and graceful, pro-skin, the 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 with high wet transmitting performance of the present embodiment, comprise the steps: 1) method that first combines by melt polycondensation and solid phase polycondensation, take terephthalic acid (TPA), ethylene glycol is raw material, and the mol ratio of terephthalic acid (TPA) and ethylene glycol is 1:1.2; Add and account for the poly adipate succinic acid ester that molar percentage 6% molecular weight of described terephthalic acid (TPA) is 1000, synthetic fusing point is at 205 ℃, the copolyesters of inherent viscosity 0.5dl/g; Then copolyesters is less than under the condition of 1kpa at 180 ℃, vacuum, the solid phase polycondensation through 36 hours, further brings up to inherent viscosity 1.0dl/g, and fusing point is at the copolyesters additive of 205 ℃; 2) the described inherent viscosity that accounts for additive, compatilizer and acrylic resin total weight percent 10% of being prepared by step 1) 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 the temperature conditions of 230 ℃, make the dyeable modified acrylic resin containing additive, the average grain diameter that records decentralized photo is 0.74 μ m.Be shown in Table 1, table 1 is preparation technology and the result display list of dyeable modified acrylic resin in the embodiment of the present invention.3) by described step 2) the dyeable modified acrylic resin that makes be island and inherent viscosity be 0.80dl/g alkali soluble polyester for sea, be dried respectively, the moisture content that makes to cut into slices is less than 50PPM.Then through double screw extruder, melt extrude, carry, measure, the ratio that is 80:20 in the weight ratio of dyeable modified acrylic resin and polyamide fibre enters island composite spining module, control 260 ℃ of spinning temperatures, 2800 ms/min of spinning speeds, make the pre-oriented yarn (POY) on 180dtex/24f ×21 island.POY, again through texturing craft, makes the DTY silk on 100dtex/24f ×21 island.Be shown in Table 2, table 2 is preparation technology and the result display list that in the embodiment of the present invention, island composite spinning method is prepared ultra-fine dyeable polypropylene fibre.
The present embodiment is owing to adopting the copolyesters of fatty family binary acid and dihydroxylic alcohols as additive, both can reduce additive and polyacrylic fusing point is poor, again because of the existence of aliphatic chain, improve and polyacrylic compatibility, and compare with polyether-type copolyesters, heat endurance improves greatly, therefore, greatly improves spinning process performance.By taking first to make the copolyesters of inherent viscosity 0.4～0.6dl/g, then pass through solid phase polycondensation, further inherent viscosity is brought up to the method for 0.8～1.0dl/g, while having overcome multiple aliphatic binary acid, dihydroxylic alcohols participation copolymerization, molecular weight is difficult to improve, easily produce various side reactions, cause the problems such as copolyesters Quality Down, make copolyesters additive and polypropylene base have better viscosity match.Preferably all there is the compatilizer of the many monomers of polyolefin elastomer grafting of better compatibility with polypropylene and copolyesters, further improved additive dispersion effect in polypropylene base, make the particle diameter of decentralized photo be less than 1 μ m.With this dyeable modified acrylic resin, by the method for island composite spinning, make filament number and be less than 0.2dtex, and the super fine denier dyeable polypropylene of available disperse dyeing and stamp.The fabric being made into this fiber, has good slim and graceful, pro-skin, the performance such as ventilative, warming, is particularly suitable for high-grade bedding, high-grade cold-proof underwear etc.
Embodiment 6
The preparation process of the present embodiment is substantially the same manner as Example 5, difference is: the copolyesters that is 1.0dl/g by the inherent viscosity that accounts for additive, compatilizer and acrylic resin total weight percent 10%, account for the POE-g-(GMA-co-MAH of additive, compatilizer and acrylic resin total weight percent 2%) with the acrylic resin of melt index 30g/10min through double screw extruder, with 230 ℃ of blend granulations, make the dyeable modified acrylic resin containing additive, the average grain diameter that records decentralized photo is 0.78 μ m.Be shown in Table 1, table 1 is preparation technology and the result display list of dyeable modified acrylic resin in the embodiment of the present invention.The weight ratio of dyeable modified acrylic resin and polyamide fibre is 72:28.Make the pre-oriented yarn (POY) on 180dtex/24f ×21 island.POY, again through texturing craft, makes the DTY silk on 100dtex/24f ×21 island.Be shown in Table 2, table 2 is preparation technology and the result display list that in the embodiment of the present invention, island composite spinning method is prepared ultra-fine dyeable polypropylene fibre.
The present embodiment is owing to adopting the copolyesters of fatty family binary acid and dihydroxylic alcohols as additive, both can reduce additive and polyacrylic fusing point is poor, again because of the existence of aliphatic chain, improve and polyacrylic compatibility, and compare with polyether-type copolyesters, heat endurance improves greatly, therefore, greatly improves spinning process performance.By taking first to make the copolyesters of inherent viscosity 0.4～0.6dl/g, then pass through solid phase polycondensation, further inherent viscosity is brought up to the method for 0.8～1.0dl/g, while having overcome multiple aliphatic binary acid, dihydroxylic alcohols participation copolymerization, molecular weight is difficult to improve, easily produce various side reactions, cause the problems such as copolyesters Quality Down, make copolyesters additive and polypropylene base have better viscosity match.Preferably all there is the compatilizer of the many monomers of polyolefin elastomer grafting of better compatibility with polypropylene and copolyesters, further improved additive dispersion effect in polypropylene base, make the particle diameter of decentralized photo be less than 1 μ m.With this dyeable modified acrylic resin, by the method for island composite spinning, make filament number and be less than 0.2dtex, and the super fine denier dyeable polypropylene of available disperse dyeing and stamp.The fabric being made into this fiber, has good slim and graceful, pro-skin, the 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 with high wet transmitting performance of the present embodiment, comprise the steps: 1) method that first combines by melt polycondensation and solid phase polycondensation, take terephthalic acid (TPA), ethylene glycol is raw material, and the mol ratio of terephthalic acid (TPA) and ethylene glycol is 1:1.2; Add and account for the poly adipate succinic acid ester that molar percentage 3% molecular weight of described terephthalic acid (TPA) is 2000, synthetic fusing point is at 210 ℃, the copolyesters of inherent viscosity 0.5dl/g; Then copolyesters is less than under the condition of 1kpa at 185 ℃, vacuum, the solid phase polycondensation through 24 hours, further brings up to inherent viscosity 0.9dl/g, and fusing point is at the copolyesters additive of 205 ℃; 2) the described inherent viscosity that accounts for additive, compatilizer and acrylic resin total weight percent 10% of being prepared by step 1) 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 the temperature conditions of 230 ℃, make the dyeable modified acrylic resin containing additive, the average grain diameter that records decentralized photo is 0.70 μ m.Be shown in Table 1, table 1 is preparation technology and the result display list of dyeable modified acrylic resin in the embodiment of the present invention.3) by described step 2) the dyeable modified acrylic resin that makes be island and inherent viscosity be 0.80dl/g alkali soluble polyester for sea, be dried respectively, the moisture content that makes to cut into slices is less than 50PPM.Then through double screw extruder, melt extrude, carry, measure, the ratio that is 70:30 in the weight ratio of dyeable modified acrylic resin and polyamide fibre enters island composite spining module, control 260 ℃ of spinning temperatures, the first 1500 ms/min of hot-rolling speed, 75 ℃ of temperature, the second 3200 ms/min of hot-rolling speed, 130 ℃ of temperature, make the FDY on 75dtex/24f ×21 island.Be shown in Table 2, table 2 is preparation technology and the result display list that in the embodiment of the present invention, island composite spinning method is prepared ultra-fine dyeable polypropylene fibre.
The present embodiment is owing to adopting the copolyesters of fatty family binary acid and dihydroxylic alcohols as additive, both can reduce additive and polyacrylic fusing point is poor, again because of the existence of aliphatic chain, improve and polyacrylic compatibility, and compare with polyether-type copolyesters, heat endurance improves greatly, therefore, greatly improves spinning process performance.By taking first to make the copolyesters of inherent viscosity 0.4～0.6dl/g, then pass through solid phase polycondensation, further inherent viscosity is brought up to the method for 0.8～1.0dl/g, while having overcome multiple aliphatic binary acid, dihydroxylic alcohols participation copolymerization, molecular weight is difficult to improve, easily produce various side reactions, cause the problems such as copolyesters Quality Down, make copolyesters additive and polypropylene base have better viscosity match.Preferably all there is the compatilizer of the many monomers of polyolefin elastomer grafting of better compatibility with polypropylene and copolyesters, further improved additive dispersion effect in polypropylene base, make the particle diameter of decentralized photo be less than 1 μ m.With this dyeable modified acrylic resin, by the method for island composite spinning, make filament number and be less than 0.2dtex, and the super fine denier dyeable polypropylene of available disperse dyeing and stamp.The fabric being made into this fiber, has good slim and graceful, pro-skin, the 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 the present embodiment is substantially the same manner as Example 2, and difference is: do not add compatilizer, the dispersiveness of additive in dyeable modified acrylic resin is poor, and the average grain diameter that records decentralized photo is 3.75 μ m.As shown in table 1.The alkali soluble polyester that is 0.70dl/g by the dyeable modified acrylic resin of gained and inherent viscosity, is dried respectively, and the moisture content that makes to cut into slices is less than 50PPM.Then through double screw extruder, melt extrude, carry, measure, in the ratio of island and extra large 80:20, enter island composite spining module, control 250 ℃ of spinning temperatures, 2800 ms/min of spinning speeds, carry out the production of the compound POY silk in island, result because of waft silk seriously cannot reel.As shown in table 2.
Comparative example 2
The preparation process of the present embodiment is substantially the same manner as Example 5, and difference is: do not add compatilizer, the dispersiveness of additive in dyeable modified acrylic resin is poor, and the average grain diameter that records decentralized photo is 3.35 μ m.As shown in table 1.The alkali soluble polyester that is 0.80dl/g by the dyeable modified acrylic resin of comparative example 2 gained and inherent viscosity, is dried respectively, and the moisture content that makes to cut into slices is less than 50PPM.Then through double screw extruder, melt extrude, carry, measure, in the ratio of island and extra large 70:30, enter island composite spining module, control 260 ℃ of spinning temperatures, the first 1500 ms/min of hot-rolling speed, 75 ℃ of temperature, the second 3200 ms/min of hot-rolling speed, 130 ℃ of temperature, carry out the production of the compound FDY silk in island, because wafing, silk seriously cannot be reeled.
As shown in table 2.
Table 1
Table 2
Claims (5)
1. an island composite spinning method is prepared the method for ultra-fine dyeable polypropylene fibre, it is characterized in that comprising the steps: 1) method that first combines by melt polycondensation and solid phase polycondensation, make fusing point at 180～220 ℃, inherent viscosity 0.8～1.0dl/g, the copolyesters additive that contains aliphatic dibasic acid, aliphatic dihydroxy alcohol; 2) then by 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 that Dispersed Phase Size is less than 1 μ m; 3) using described step 2) the dyeable modified acrylic resin prepared is as island, and alkali soluble polyester is done sea, carries out island Compound Machining; After fiber Jing Hou road alkali decrement, polypropylene filament fiber number is less than the ultra-fine dyeable polypropylene fibre of 0.2dtex; In described step 1), the preparation process of copolyesters additive is: take terephthalic acid (TPA), ethylene glycol is raw material, and the mol ratio of terephthalic acid (TPA) and ethylene glycol is 1:1.2; Add one or more in aliphatic binary acid, aliphatic dihydroxylic alcohols and aliphatic polyester, and addition accounts for the molar percentage 10～60% of terephthalic acid (TPA); The synthetic fusing point of method by melt polycondensation is at 180～220 ℃, the copolyesters of inherent viscosity 0.4～0.6dl/g; Then copolyesters is less than under the condition of 1kpa at 170～210 ℃, vacuum, the solid phase polycondensation through 24～48 hours, further brings up to 0.8～1.0dl/g by inherent viscosity; Described step 2) in, the preparation process of dyeable modified acrylic resin is: the compatilizer of copolyesters additive prepared by step 1) and the many monomers of polyolefin elastomer grafting, and melt index adds compatilizer at the acrylic resin of 30～50g/10min by additive and account for additive, compatilizer and acrylic resin total weight percent 5～17%, and compatilizer addition is less than additive, compatilizer and acrylic resin total weight percent 5%; On double screw extruder, melt blending granulation under the temperature conditions of 200～250 ℃, makes the dyeable modified acrylic resin containing additive, and its Dispersed Phase Size is less than 1 μ m.
2. a kind of island according to claim 1 composite spinning method is prepared the method for ultra-fine dyeable polypropylene fibre, it is characterized in that: described aliphatic binary acid adopts a kind of in succinic acid, adipic acid, decanedioic acid; Aliphatic dihydroxylic alcohols adopts a kind of in 1,3-PD, BDO, 1,6-hexylene glycol; Aliphatic polyester adopts a kind of in the polyethylene glycol adipate, poly adipate succinic acid ester, poly-adipic acid hexylene glycol ester of molecular weight 1000～2000.
3. a kind of island according to claim 2 composite spinning method is prepared the method for ultra-fine dyeable polypropylene fibre, it is characterized in that: described aliphatic binary acid adopts adipic acid; Aliphatic dihydroxylic alcohols adopts BDO; Aliphatic polyester adopts poly adipate succinic acid ester.
4. a kind of island according to claim 1 composite spinning method is prepared the method for ultra-fine dyeable polypropylene fibre, it is characterized in that: the compatilizer of the described many monomers of polyolefin elastomer grafting adopts EPDM-g-MAH, POE-g-(GMA-co-MAH) in a kind of.
5. a kind of island according to claim 1 composite spinning method is prepared the method for ultra-fine dyeable polypropylene fibre, it is characterized in that: in described step 3) using step 2) the dyeable modified acrylic resin prepared is as island, alkali soluble polyester is done sea, carries out island Compound Machining; Wherein dyeable modified acrylic resin and alkali soluble polyester weight ratio are 70～80:30～20, carry out island Compound Machining; After fiber Jing Hou road alkali decrement, 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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| CN106149094B (en) * | 2015-03-25 | 2021-04-16 | 东丽纤维研究所（中国）有限公司 | Polypropylene nanofiber and preparation method thereof |
| CN106609402B (en) * | 2015-10-21 | 2019-05-28 | 厦门翔鹭化纤股份有限公司 | Dense dye superfine fibre of one kind and preparation method thereof |
| ES2865386T3 (en) * | 2016-03-11 | 2021-10-15 | Toray Industries | Dyeable polyolefin fiber and fibrous structure comprising the same |
| JP7056153B2 (en) * | 2016-10-25 | 2022-04-19 | 東レ株式会社 | Polymer alloy fibers and fiber structures made of them |
| CN108048922A (en) * | 2017-12-25 | 2018-05-18 | 四川大学 | A kind of environmental-friendly preparation method of not figured type polypropylene superfine fiber |
| JP6934451B2 (en) * | 2018-06-05 | 2021-09-15 | 株式会社豊田中央研究所 | Fiber reinforced resin composition and its manufacturing method |
| CN110872417B (en) * | 2018-08-29 | 2022-07-15 | 国家能源投资集团有限责任公司 | Spinning master batch, polypropylene fiber, preparation method of spinning master batch and polypropylene fiber, and polypropylene fiber product |
| CN112553710A (en) * | 2020-11-24 | 2021-03-26 | 绍兴文理学院 | Superfine ultrashort different-section polypropylene fiber and preparation method thereof |
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