CN102733002B - 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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- CN102733002B CN102733002B CN2012102084534A CN201210208453A CN102733002B CN 102733002 B CN102733002 B CN 102733002B CN 2012102084534 A CN2012102084534 A CN 2012102084534A CN 201210208453 A CN201210208453 A CN 201210208453A CN 102733002 B CN102733002 B CN 102733002B
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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, wherein in sliver type composite spinning, mainly take polyester-nylon composite spinning as main, utilize the non-compatibility of terylene and polyamide fibre, lower minute fibre of the effect of Hou road alkali decrement or certain mechanical force, making superfine Denier fibre, is a kind of technology of comparative maturity.
Research shows, the polypropylene fibre after the thin dawn except the denominator with general fine count fiber as the advantages such as soft, elegant, pro-skin, also have good warming, breathe freely, lead wet, health, the characteristics such as relaxed and comfortable.But dyeed because polypropylene fibre be difficult for to adopt conventional dyeing, thereby affected polypropylene and other macromolecular material carries out composite spinning, prepared the exploitation of superfine Denier fibre.
Publication number CN101736416A, disclose " preparation technology of a kind of thin dawn and superfine denier polypropylene fibers ", adopts conventional spin processes to obtain thin dawn and the superfine 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 is controlled between 200～280 ℃, select the high-flowability polypropylene of good thermal stability and with the wire winding speed spinning below 2000 m/mins, and, by the 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 preparation method of resin specially for dyable fine denier polypropylene fibre and fiber also has more report, 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 directly through melt spinning, manufacture the method that filament number is (1.11～2.22) dtex dyable fine denier polypropylene fibre.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 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.
Above disclosed dyeable polypropylene fibre patent is mainly to prepare dyeable fine-denier polypropylene by conventional melt spinning technology path.As the holder part by sliver type composite spinning is replaced by dyeable modified polypropylene, prepare average filament number and be less than the dyeable polypropylene of 0.2dtex and the composite fibre of polyamide fibre, can realize better leading wet, moisture sorption effect.Wherein the dispersiveness of additive in the matrix polypropylene is extremely important for this, as too large in disperseed particle diameter, and easily producing first that broken end, spinnability descend even greatly can't repiece; Second mechanical property significantly descends, 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 superfine composite fiber preparation method with high wet transmitting performance, it is high that the present invention has heat endurance, and the spinning process performance is good, 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 by melt polycondensation and solid phase polycondensation, make fusing point at 180～220 ℃, inherent viscosity 1.0～1.2dl/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 (be purchased from 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 that Dispersed Phase Size is less than 1 μ m; 3) the sliver type is washed the preparation of the third composite fibre, using described step 2) the dyeable modified acrylic resin for preparing is as support, polyamide fibre is as sliver, and the mechanical force in fiber Jing Hou road alkali decrement or processing, split into the superfine composite fiber that filament number is less than 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 0.5～0.7dl/g; Then copolyesters is less than under the condition of 1kpa at 170～210 ℃, vacuum, the solid phase polycondensation through 36～48 hours, further bring up to 1.0～1.2dl/g by inherent viscosity.
Described aliphatic binary acid adopts a kind of in succinic acid, hexanedioic 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 poly-hexanedioic acid glycol ester of molecular weight 1000～2000, poly-hexanedioic acid butanediol ester, poly-hexanedioic acid hexylene glycol ester.
Described aliphatic binary acid adopts hexanedioic acid; Aliphatic dihydroxylic alcohols adopts BDO; Aliphatic polyester adopts poly-hexanedioic acid butanediol 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 10～30g/10min by additive and account 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 the temperature conditions of 200～250 ℃, make the dyeable modified acrylic resin containing additive, and its Dispersed Phase Size 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) (the polyolefin elastomer graft glycidyl methacrylate is a kind of in maleic anhydride altogether.(being purchased from the permanent brightness chemical industry of Yangzhou Co., Ltd)
In described step 3), the sliver type is washed the preparation process of the third composite fibre and is: by described 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.Mechanical force in fiber Jing Hou road alkali decrement or processing, split into the superfine fibre that filament number is less than 0.2dtex, and fiber can disperse dyeing.
Beneficial effect of the present invention is: the present invention due to the copolyesters that adopts 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 the polyether-type copolyesters, heat endurance improves greatly, therefore, greatly improves the spinning process performance.By taking first to make the copolyesters of inherent viscosity 0.5～0.7dl/g, then pass through solid phase polycondensation, further inherent viscosity is brought up to the method for 1.0～1.2dl/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 that better viscosity match be 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, make the particle diameter of decentralized photo be less than 1 μ m.With this dyeable modified acrylic resin, by the method for sliver type composite spinning, make super fine denier the third chinlon composite fiber that filament number is less than 0.2dtex and available disperse dyeing.The fabric be made into this fiber, have good softness, lead the performances such as wet, moisture absorption, is particularly suitable for making high-grade towel, bath towel etc.
The accompanying drawing explanation
Fig. 1 is the structural representation between support of the present invention and sliver.
The specific embodiment
Below by specific embodiment, the invention will be further described.Wherein: the method for testing of dispersed phase size: will be from the blend batten of twin-screw extrusion, brittle failure in liquid nitrogen, then carry out ESEM (SEM) analysis to section, finally with Photo shop, calculates average grain diameter; Inherent viscosity method of testing: press GB-T 14189-2008, as solvent detected at 1: 1 with phenol and tetrachloroethanes.The relative viscosity method of testing of polyamide fibre 6: take the concentrated sulfuric acid as solvent, detect with dark type viscometer.Propionate dyed nylon composite wire test: 7 liters of water, add 100g and 85g 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.Shade is main partly to be compared with polyamide fibre wherein.
Embodiment 1
A kind of superfine composite fiber preparation method with high wet transmitting performance of the present embodiment, comprise the steps: 1) method that at 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 hexanedioic 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 0.5dl/g; Then copolyesters is less than under the condition of 1kpa at 170 ℃, vacuum, the solid phase polycondensation through 36 hours, further bring up to inherent viscosity 1.0dl/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% 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 200 ℃, make the dyeable modified acrylic resin containing additive, the average grain diameter that records decentralized photo is 0.85 μ m.Be shown in Table 1 the preparation technology that table 1 is dyeable modified acrylic resin in the embodiment of the present invention and display list as a result.3) using described step 2) the dyeable modified acrylic resin for preparing is as support 1, and polyamide fibre is as sliver 2, as shown in Figure 1; First dyeable modified acrylic resin is carried out to drying, the moisture content that makes to cut into slices is less than 50PPM, and polyamide fibre is selected dry section, 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 to enter sliver type composite spining module at 60: 40, control 265 ℃ of spinning temperatures, 2500 m/mins 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, again through texturing craft, makes the DTY silk of cutting apart 100dtex/36f * 16.Be shown in Table 2 the preparation technology that table 2 is the superfine composite fiber of high wet transmitting performance in the embodiment of the present invention and display list as a result.
The present embodiment due to the copolyesters that adopts 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 the polyether-type copolyesters, heat endurance improves greatly, therefore, greatly improves the spinning process performance.By taking first to make the copolyesters of inherent viscosity 0.5～0.7dl/g, then pass through solid phase polycondensation, further inherent viscosity is brought up to the method for 1.0～1.2dl/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 that better viscosity match be 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, make the particle diameter of decentralized photo be less than 1 μ m.With this dyeable modified acrylic resin, by the method for sliver type composite spinning, make super fine denier the third chinlon composite fiber that filament number is less than 0.2dtex and available disperse dyeing.The fabric be made into this fiber, have good softness, lead the performances such as wet, moisture absorption, is particularly suitable for making high-grade towel, bath towel etc.
Embodiment 2
The preparation process of the present embodiment is substantially the same manner as Example 1, difference is: the copolyesters that the inherent viscosity that will account for additive, compatilizer and acrylic resin total weight percent 10% is 1.0dl/g, account for the polypropylene of the EPDM-g-MAH of additive, compatilizer and acrylic resin total weight percent 2% and melt index 30g/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 0.91 μ m.Be shown in Table 1 the preparation technology that table 1 is dyeable modified acrylic resin in the embodiment of the present invention and display list as a result.Dyeable modified acrylic resin and polyamide fibre percentage by weight are 70:30.Make the superfine composite fiber (pre-oriented yarn (POY) that 165dtex/36f * 16 are cut apart) with high wet transmitting performance.POY, again through texturing craft, makes the DTY silk of cutting apart 100dtex/36f * 16.Be shown in Table 2 the preparation technology that table 2 is the superfine composite fiber of high wet transmitting performance in the embodiment of the present invention and display list as a result.
The present embodiment due to the copolyesters that adopts 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 the polyether-type copolyesters, heat endurance improves greatly, therefore, greatly improves the spinning process performance.By taking first to make the copolyesters of inherent viscosity 0.5～0.7dl/g, then pass through solid phase polycondensation, further inherent viscosity is brought up to the method for 1.0～1.2dl/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 that better viscosity match be 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, make the particle diameter of decentralized photo be less than 1 μ m.With this dyeable modified acrylic resin, by the method for sliver type composite spinning, make super fine denier the third chinlon composite fiber that filament number is less than 0.2dtex and available disperse dyeing.The fabric be made into this fiber, have good softness, lead the performances such as wet, moisture absorption, is particularly suitable for making high-grade towel, bath towel etc.
Embodiment 3
The preparation process of the present embodiment is substantially the same manner as Example 1, difference is: the copolyesters that the inherent viscosity that will account for additive, compatilizer and acrylic resin total weight percent 15% is 1.0dl/g, account for the polypropylene of the EPDM-g-MAH of additive, compatilizer and acrylic resin total weight percent 2% and melt index 30g/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 0.95 μ m.Be shown in Table 1 the preparation technology that table 1 is dyeable modified acrylic resin in the embodiment of the present invention and display list as a result.Dyeable modified acrylic resin and polyamide fibre percentage by weight are 80: 20.Make the superfine composite fiber (pre-oriented yarn (POY) that 165dtex/36f * 16 are cut apart) with high wet transmitting performance.POY, again through texturing craft, makes the DTY silk of cutting apart 100dtex/36f * 16.Be shown in Table 2 the preparation technology that table 2 is the superfine composite fiber of high wet transmitting performance in the embodiment of the present invention and display list as a result.
The present embodiment due to the copolyesters that adopts 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 the polyether-type copolyesters, heat endurance improves greatly, therefore, greatly improves the spinning process performance.By taking first to make the copolyesters of inherent viscosity 0.5～0.7dl/g, then pass through solid phase polycondensation, further inherent viscosity is brought up to the method for 1.0～1.2dl/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 that better viscosity match be 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, make the particle diameter of decentralized photo be less than 1 μ m.With this dyeable modified acrylic resin, by the method for sliver type composite spinning, make super fine denier the third chinlon composite fiber that filament number is less than 0.2dtex and available disperse dyeing.The fabric be made into this fiber, have good softness, lead the performances 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 with high wet transmitting performance of the present embodiment, comprise the steps: 1) method that at 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 hexanedioic 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 48 hours, further bring up to inherent viscosity 1.2dl/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% prepared by step 1) 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 the temperature conditions of 230 ℃, 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 the preparation technology that table 1 is dyeable modified acrylic resin in the embodiment of the present invention and display list as a result.3) using described step 2) the dyeable modified acrylic resin for preparing is as support 1, and polyamide fibre is as sliver 2, as shown in Figure 1; First dyeable modified acrylic resin is carried out to drying, the moisture content that makes to cut into slices is less than 50PPM, and polyamide fibre is selected dry section, 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 to enter sliver type composite spining module at 75: 25, control 265 ℃ of spinning temperatures, 2500 m/mins 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, again through texturing craft, makes the DTY silk of cutting apart 100dtex/36f * 16.Be shown in Table 2 the preparation technology that table 2 is the superfine composite fiber of high wet transmitting performance in the embodiment of the present invention and display list as a result.
The present embodiment due to the copolyesters that adopts 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 the polyether-type copolyesters, heat endurance improves greatly, therefore, greatly improves the spinning process performance.By taking first to make the copolyesters of inherent viscosity 0.5～0.7dl/g, then pass through solid phase polycondensation, further inherent viscosity is brought up to the method for 1.0～1.2dl/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 that better viscosity match be 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, make the particle diameter of decentralized photo be less than 1 μ m.With this dyeable modified acrylic resin, by the method for sliver type composite spinning, make super fine denier the third chinlon composite fiber that filament number is less than 0.2dtex and available disperse dyeing.The fabric be made into this fiber, have good softness, lead the performances 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 with high wet transmitting performance of the present embodiment, comprise the steps: 1) method that at 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 poly-hexanedioic acid butanediol ester that molar percentage 6% molecular weight that accounts for described terephthalic acid (TPA) is 1000, synthetic fusing point is at 200 ℃, the copolyesters of inherent viscosity 0.7dl/g; Then copolyesters is less than under the condition of 1kpa at 175 ℃, vacuum, the solid phase polycondensation through 48 hours, further bring up to inherent viscosity 1.2dl/g, and fusing point is at the copolyesters additive of 200 ℃; 2) the described inherent viscosity that accounts for additive, compatilizer and acrylic resin total weight percent 10% prepared by step 1) 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 the temperature conditions of 230 ℃, make the dyeable modified acrylic resin containing additive, the average grain diameter that records decentralized photo is 0.81 μ m.Be shown in Table 1 the preparation technology that table 1 is dyeable modified acrylic resin in the embodiment of the present invention and display list as a result.3) using described step 2) the dyeable modified acrylic resin for preparing is as support 1, and polyamide fibre is as sliver 2, as shown in Figure 1; First dyeable modified acrylic resin is carried out to drying, the moisture content that makes to cut into slices is less than 50PPM, and polyamide fibre is selected dry section, 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 to enter sliver type composite spining module at 70: 30, control 265 ℃ of spinning temperatures, 2500 m/mins 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, again through texturing craft, makes the DTY silk of cutting apart 100dtex/36f * 16.Be shown in Table 2 the preparation technology that table 2 is the superfine composite fiber of high wet transmitting performance in the embodiment of the present invention and display list as a result.
The present embodiment due to the copolyesters that adopts 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 the polyether-type copolyesters, heat endurance improves greatly, therefore, greatly improves the spinning process performance.By taking first to make the copolyesters of inherent viscosity 0.5～0.7dl/g, then pass through solid phase polycondensation, further inherent viscosity is brought up to the method for 1.0～1.2dl/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 that better viscosity match be 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, make the particle diameter of decentralized photo be less than 1 μ m.With this dyeable modified acrylic resin, by the method for sliver type composite spinning, make super fine denier the third chinlon composite fiber that filament number is less than 0.2dtex and available disperse dyeing.The fabric be made into this fiber, have good softness, lead the performances such as wet, moisture absorption, is particularly suitable for making high-grade towel, bath towel etc.
Embodiment 6
The preparation process of the present embodiment is substantially the same manner as Example 5, difference is: the copolyesters that the inherent viscosity that will account for additive, compatilizer and acrylic resin total weight percent 10% is 1.2dl/g, 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 10g/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 0.79 μ m.Be shown in Table 1 the preparation technology that table 1 is dyeable modified acrylic resin in the embodiment of the present invention and display list as a result.Dyeable modified acrylic resin and polyamide fibre percentage by weight are 65: 35.Make the superfine composite fiber (pre-oriented yarn (POY) that 165dtex/36f * 16 are cut apart) with high wet transmitting performance.POY, again through texturing craft, makes the DTY silk of cutting apart 100dtex/36f * 16.Be shown in Table 2 the preparation technology that table 2 is the superfine composite fiber of high wet transmitting performance in the embodiment of the present invention and display list as a result.
The present embodiment due to the copolyesters that adopts 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 the polyether-type copolyesters, heat endurance improves greatly, therefore, greatly improves the spinning process performance.By taking first to make the copolyesters of inherent viscosity 0.5～0.7dl/g, then pass through solid phase polycondensation, further inherent viscosity is brought up to the method for 1.0～1.2dl/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 that better viscosity match be 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, make the particle diameter of decentralized photo be less than 1 μ m.With this dyeable modified acrylic resin, by the method for sliver type composite spinning, make super fine denier the third chinlon composite fiber that filament number is less than 0.2dtex and available disperse dyeing.The fabric be made into this fiber, have good softness, lead the performances 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 with high wet transmitting performance of the present embodiment, comprise the steps: 1) method that at 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 poly-hexanedioic acid butanediol ester that molar percentage 3% molecular weight that accounts for described terephthalic acid (TPA) is 2000, synthetic fusing point is at 205 ℃, the copolyesters of inherent viscosity 0.7dl/g; Then copolyesters is less than under the condition of 1kpa at 180 ℃, vacuum, the solid phase polycondensation through 36 hours, further bring up to inherent viscosity 1.1dl/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% prepared by step 1) 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 the temperature conditions of 230 ℃, 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 the preparation technology that table 1 is dyeable modified acrylic resin in the embodiment of the present invention and display list as a result.3) using described step 2) the dyeable modified acrylic resin for preparing is as support 1, and polyamide fibre is as sliver 2, as shown in Figure 1; First dyeable modified acrylic resin is carried out to drying, the moisture content that makes to cut into slices is less than 50PPM, and polyamide fibre is selected dry section, and inherent viscosity is 2.5dl/g.Melt extrude, carry, measure through double screw extruder respectively, percentage by weight by dyeable modified acrylic resin and polyamide fibre is to enter sliver type composite spining module at 80: 20, control 285 ℃ of spinning temperatures, the first 2000 m/mins of hot-rolling speed, 80 ℃ of temperature, the second 3800 m/mins of hot-rolling speed, 130 ℃ of temperature, make the superfine composite fiber (FDY that 75dtex/24f * 16 are cut apart) with high wet transmitting performance.Be shown in Table 2 the preparation technology that table 2 is the superfine composite fiber of high wet transmitting performance in the embodiment of the present invention and display list as a result.
The present embodiment due to the copolyesters that adopts 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 the polyether-type copolyesters, heat endurance improves greatly, therefore, greatly improves the spinning process performance.By taking first to make the copolyesters of inherent viscosity 0.5～0.7dl/g, then pass through solid phase polycondensation, further inherent viscosity is brought up to the method for 1.0～1.2dl/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 that better viscosity match be 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, make the particle diameter of decentralized photo be less than 1 μ m.With this dyeable modified acrylic resin, by the method for sliver type composite spinning, make super fine denier the third chinlon composite fiber that filament number is less than 0.2dtex and available disperse dyeing.The fabric be made into this fiber, have good softness, lead the performances such as wet, moisture absorption, is particularly suitable for making high-grade towel, bath towel 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 3.70 μ m.Dyeable modified acrylic resin by gained as shown in table 1 carries out drying, and the moisture content that makes to cut into slices is less than 50PPM, and polyamide fibre is selected dry section, and inherent viscosity is 2.3dl/g.Melt extrude, carry, measure through double screw extruder respectively, enter sliver type composite spining module in dyeable modified acrylic resin and the polyamide fibre ratio of 60: 40, control 285 ℃ of spinning temperatures, 2500 m/mins of spinning speeds, result seriously can't be reeled because of the silk that wafts.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 3.15 μ m.As shown in table 1.The polyester that is 0.68dl/g by the dyeable modified acrylic resin of gained and inherent viscosity, carry out respectively drying, and the moisture content that makes to cut into slices is less than 50PPM, and polyamide fibre is selected dry section, 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 enters sliver type composite spining module, control 285 ℃ of spinning temperatures, the first 2000 m/mins of hot-rolling speed, 80 ℃ of temperature, the second 3800 m/mins of hot-rolling speed, 130 ℃ of temperature, because wafing, silk seriously can't be reeled.As shown in table 2.
Table 1
Table 2
Claims (5)
1. the superfine composite fiber preparation method with high wet transmitting performance, it is characterized in that comprising the steps: 1) method that at first combines by melt polycondensation and solid phase polycondensation, make fusing point at 180～220 ℃, inherent viscosity 1.0～1.2dl/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 10～30g/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) preparation of sliver type the third chinlon composite fiber, using described step 2) the dyeable modified acrylic resin for preparing is as support, polyamide fibre is as sliver, and the mechanical force in fiber Jing Hou road alkali decrement or processing, split into the superfine composite fiber that filament number is less than 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 0.5～0.7dl/g; Then copolyesters is less than under the condition of 1kPa at 170～210 ℃, vacuum, the solid phase polycondensation through 36～48 hours, further bring up to 1.0～1.2dl/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.
2. a kind of superfine composite fiber preparation method with high wet transmitting performance according to claim 1, is characterized in that: described aliphatic binary acid employing adipic acid; Aliphatic dihydroxylic alcohols adopts BDO; Aliphatic polyester adopts poly adipate succinic acid ester.
3. a kind of superfine composite fiber preparation method with high wet transmitting performance according to claim 1, it is characterized in that described step 2) in the preparation process of dyeable modified acrylic resin be: 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 10～30g/10min by additive and account 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 the temperature conditions of 200～250 ℃, make the dyeable modified acrylic resin containing additive, and its Dispersed Phase Size is less than 1 μ m.
4. a kind of superfine composite fiber preparation method with high wet transmitting performance according to claim 3 is characterized in that: the compatilizer of the many monomers of described polyolefin elastomer grafting adopts EPDM-g-MAH, POE-g-(GMA-co-MAH) in a kind of.
5. a kind of superfine composite fiber preparation method with high wet transmitting performance according to claim 1, it is characterized in that: in described step 3), the preparation process of sliver type the third chinlon composite fiber is: by described step 2) the dyeable modified acrylic resin that makes is as support, polyamide fibre is as sliver, wherein dyeable modified acrylic resin accounts for 60～80% of dyeable modified acrylic resin and polyamide fibre total weight percent, carry out composite spinning, make POY-DTY; Mechanical force in fiber Jing Hou road alkali decrement or processing, split into the superfine fibre that filament number is less than 0.2dtex.
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| CN105862150B (en) * | 2016-05-25 | 2020-02-07 | 浙江理工大学 | Superfine composite fiber and processing technology thereof |
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