CN101781812B - Method for preparing continuous polymerization directly-spun cation-dyeable high-shrinkage polyester filaments - Google Patents
Method for preparing continuous polymerization directly-spun cation-dyeable high-shrinkage polyester filaments Download PDFInfo
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- CN101781812B CN101781812B CN2010101245296A CN201010124529A CN101781812B CN 101781812 B CN101781812 B CN 101781812B CN 2010101245296 A CN2010101245296 A CN 2010101245296A CN 201010124529 A CN201010124529 A CN 201010124529A CN 101781812 B CN101781812 B CN 101781812B
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- 229920000728 polyester Polymers 0.000 title claims abstract description 51
- 238000000034 method Methods 0.000 title claims abstract description 39
- 238000006116 polymerization reaction Methods 0.000 title claims abstract description 16
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 55
- 229920001634 Copolyester Polymers 0.000 claims abstract description 45
- 239000000835 fiber Substances 0.000 claims abstract description 37
- 238000009987 spinning Methods 0.000 claims abstract description 35
- 238000004519 manufacturing process Methods 0.000 claims abstract description 26
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 claims abstract description 22
- QQVIHTHCMHWDBS-UHFFFAOYSA-N isophthalic acid Chemical compound OC(=O)C1=CC=CC(C(O)=O)=C1 QQVIHTHCMHWDBS-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000000178 monomer Substances 0.000 claims abstract description 17
- 239000000155 melt Substances 0.000 claims abstract description 8
- 239000002994 raw material Substances 0.000 claims abstract description 6
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims abstract description 5
- 238000002360 preparation method Methods 0.000 claims description 25
- 238000005516 engineering process Methods 0.000 claims description 18
- 238000006068 polycondensation reaction Methods 0.000 claims description 15
- OFOBLEOULBTSOW-UHFFFAOYSA-N Malonic acid Chemical compound OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 claims description 13
- 238000006243 chemical reaction Methods 0.000 claims description 13
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 12
- 238000001816 cooling Methods 0.000 claims description 11
- 238000009998 heat setting Methods 0.000 claims description 11
- 239000002002 slurry Substances 0.000 claims description 11
- 229910052708 sodium Inorganic materials 0.000 claims description 11
- 239000011734 sodium Substances 0.000 claims description 11
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 claims description 11
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 claims description 10
- 239000005977 Ethylene Substances 0.000 claims description 10
- 238000007664 blowing Methods 0.000 claims description 10
- 230000036760 body temperature Effects 0.000 claims description 10
- 238000005098 hot rolling Methods 0.000 claims description 10
- 239000003381 stabilizer Substances 0.000 claims description 8
- 238000004804 winding Methods 0.000 claims description 8
- 239000003054 catalyst Substances 0.000 claims description 7
- 241000209094 Oryza Species 0.000 claims description 6
- 235000007164 Oryza sativa Nutrition 0.000 claims description 6
- 239000003795 chemical substances by application Substances 0.000 claims description 6
- 235000009566 rice Nutrition 0.000 claims description 6
- 150000001298 alcohols Chemical class 0.000 claims description 5
- 229910052787 antimony Inorganic materials 0.000 claims description 4
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 claims description 4
- 238000010009 beating Methods 0.000 claims description 4
- SCVFZCLFOSHCOH-UHFFFAOYSA-M potassium acetate Chemical compound [K+].CC([O-])=O SCVFZCLFOSHCOH-UHFFFAOYSA-M 0.000 claims description 4
- WVLBCYQITXONBZ-UHFFFAOYSA-N trimethyl phosphate Chemical compound COP(=O)(OC)OC WVLBCYQITXONBZ-UHFFFAOYSA-N 0.000 claims description 4
- HVLLSGMXQDNUAL-UHFFFAOYSA-N triphenyl phosphite Chemical compound C=1C=CC=CC=1OP(OC=1C=CC=CC=1)OC1=CC=CC=C1 HVLLSGMXQDNUAL-UHFFFAOYSA-N 0.000 claims description 4
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 3
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 claims description 3
- 239000001632 sodium acetate Substances 0.000 claims description 3
- 235000017281 sodium acetate Nutrition 0.000 claims description 3
- 229910000410 antimony oxide Inorganic materials 0.000 claims description 2
- 150000007942 carboxylates Chemical class 0.000 claims description 2
- JVLRYPRBKSMEBF-UHFFFAOYSA-K diacetyloxystibanyl acetate Chemical compound [Sb+3].CC([O-])=O.CC([O-])=O.CC([O-])=O JVLRYPRBKSMEBF-UHFFFAOYSA-K 0.000 claims description 2
- VTRUBDSFZJNXHI-UHFFFAOYSA-N oxoantimony Chemical compound [Sb]=O VTRUBDSFZJNXHI-UHFFFAOYSA-N 0.000 claims description 2
- 235000011056 potassium acetate Nutrition 0.000 claims description 2
- 239000000843 powder Substances 0.000 claims description 2
- ISIJQEHRDSCQIU-UHFFFAOYSA-N tert-butyl 2,7-diazaspiro[4.5]decane-7-carboxylate Chemical compound C1N(C(=O)OC(C)(C)C)CCCC11CNCC1 ISIJQEHRDSCQIU-UHFFFAOYSA-N 0.000 claims description 2
- 238000005303 weighing Methods 0.000 claims description 2
- 238000004043 dyeing Methods 0.000 abstract description 6
- NWJKPSLXLQLUTC-UHFFFAOYSA-N ethane-1,2-diol;sodium Chemical compound [Na].OCCO NWJKPSLXLQLUTC-UHFFFAOYSA-N 0.000 abstract 1
- 238000007493 shaping process Methods 0.000 abstract 1
- 230000004048 modification Effects 0.000 description 10
- 238000012986 modification Methods 0.000 description 10
- 239000000975 dye Substances 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 7
- 230000008602 contraction Effects 0.000 description 7
- 239000000463 material Substances 0.000 description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- 238000009835 boiling Methods 0.000 description 4
- 150000001768 cations Chemical class 0.000 description 4
- 238000007334 copolymerization reaction Methods 0.000 description 4
- 238000001035 drying Methods 0.000 description 4
- 230000032050 esterification Effects 0.000 description 4
- 238000005886 esterification reaction Methods 0.000 description 4
- 230000004927 fusion Effects 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- 125000002091 cationic group Chemical group 0.000 description 3
- 238000007385 chemical modification Methods 0.000 description 3
- 239000000986 disperse dye Substances 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 description 2
- 229920004933 Terylene® Polymers 0.000 description 2
- 238000013459 approach Methods 0.000 description 2
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 2
- 239000004744 fabric Substances 0.000 description 2
- 239000005020 polyethylene terephthalate Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 125000004203 4-hydroxyphenyl group Chemical group [H]OC1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- 125000001931 aliphatic group Chemical group 0.000 description 1
- 150000004703 alkoxides Chemical class 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010036 direct spinning Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 239000001294 propane Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
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- Polyesters Or Polycarbonates (AREA)
- Artificial Filaments (AREA)
Abstract
The invention discloses a method for preparing continuous polymerization directly-spun cation-dyeable high-shrinkage polyester filaments, which comprises a process for preparing continuous polymerization modified copolyester melt and a process for preparing directly-spun cation-dyeable high-shrinkage polyester filaments. In the process for preparing the continuous polymerization modified copolyester melt, purified terephthalic acid and glycol monomers are taken as raw materials, isophthalic acid and sodium ethylene glycol isophthalate-5-sulfonate are added to serve as raw materials of third monomer and fourth monomer, and the modified copolyester melt is prepared; and the modified copolyester melt directly passes through a melt conveying piping equipment, and is metered, extruded, blown to be cooled, drawn for heat shaping, and wound to prepare one of cation-dyeable high-shrinkage polyester preoriented yarns and cation-dyeable high-shrinkage polyester drawn yarns. The method has the advantages of short flow, less working procedures, reasonable process, stable melt quality, and good spinning performance; and the prepared high-shrinkage fibers have the characteristics of good shrinkage stability, even dyeing, and low production cost.
Description
Technical field
The present invention relates to a kind of manufacturing approach of modified copolyester long filament, particularly a kind of preparation method of continuous polymerization directly-spun cation-dyeable high-shrinkage polyester filaments belongs to the chemical fibre field.
Background technology
Because the numerous premium properties of polyester (terylene) fiber, therefore, it has worldwide obtained development rapidly.But the tight packing of polyester molecule chain; The degree of crystallinity and the degree of orientation are higher, and polarity is less, between the polyester long-chain molecule, do not have suitably to hold the gap of dye molecule; Therefore dye particles is difficult for getting into fiber; Its dyeability is poor, can use the kind of dyestuff few, and general polyester fiber can only adopt DISPERSE DYES high temperature or dyeing in the presence of carrier.The cationic dye capable of dyeing modified polyester fiber owing to have characteristics such as the look property of suction is good, beautiful in colour, chromatogram is complete, has become the maximum modification kind of present polyesters.Along with continually developing of the continuous expansion of its Application Areas, fabric new product, increasing than the demand of the cation-dyeable high-shrinkage polyester fiber of high shrinkage to having, application prospect is good.
High-shrinkage fibre is meant that fiber boiling water is greater than 25% chemical fibre.According to the difference of its thermal contraction degree, can obtain the final products of different-style and performance.Like high-shrinkage polyester fiber and other fiber composite, utilize interfibrous contraction poor, can increase third dimension, bulkiness of fabric etc., on products such as clothes, woollen blanket, Fake Furs, dermatine, be widely used
The preparation of terylene high-shrinkage fibre mainly contains physical modification or chemical modification and the physical modification two kinds of methods that combine.Physical modification mainly realizes to change the spinning draw conditions, but this its stable contraction rate property of high-shrinkage fibre that only makes through physical modification is relatively poor, fibre strength is low, so many at present methods that combines with chemical modification and physical modification are produced; Promptly in the production process of normal polyester, pass through to add the 3rd, the 4th monomer; Destroy macromolecular regularity, reduce crystallizing power, and combine the physical modification of spinning drafting process; Make the high-shrinkage fibre that makes; Boiling water shrinkage height and stable contraction rate, the strength and elongation index is good, satisfies the requirement of back processing better.Disclosed like Japan Patent (spy opens flat 5-302210) is a kind of " production method of polyester high-shrinkage fibre "; It is adopt to add the section that the M-phthalic acid copolymerization of 6.0-10.0% makes; Through fusion again, heat pipe drafting forming, high speed spinning, make boiling water shrinkage greater than 12% fiber.Japan Patent (spy opens 2002-20930) is disclosed to be a kind of " polyester high-shrinkage fibre ", and it is to make the copolyesters that adds M-phthalic acid and two (4-hydroxy phenyl) the propane copolymerization components of 2.2-earlier, adopts spinning drawing-off one-step method to produce high-shrinkage fibre then.But this series products can only adopt DISPERSE DYES to dye; In order to realize cationic dye capable of dyeing; Japan Patent (spy opens flat 11-93020) discloses a kind of " cationic dyeable polyester fiber and manufacturing approach "; It is to adopt the copolyester section that adds ethylene isophthalate-5-sodium sulfonate and other copolymerization component, and fusion low speed spinning then, drawing-off two step method make the high-shrinkage polyester filaments of cationic-dyeable.Publication number 200710040570.3; Disclosed is " a kind of copolyester section of modification or fiber and preparation method thereof "; The copolyester section or fiber and the preparation method that relate to a kind of modification; This copolyester section is to be formed by terephthalic acid (TPA), ethylene glycol, a benzene binary acid alkane esters sodium sulfonate (or potassium) and aliphatic dihydroxy alcohol (or its alkoxide) the four component copolymerization that contain side chain, and the fiber of spinning all can be dyed dark color to cation dyes and disperse dyes, and the tool highly shrinkable.
Above-mentioned cation-dyeable high-shrinkage polyester fiber preparation method; All be on the discontinuous polycondensation device, to make the modified copolyester section earlier through chemical modification; Then with modified copolyester cut into slices crystallization again, drying, fusion, through spinning, after the physical modification of processing produce high-shrinkage fiber.The modified copolyester section of on the batchwise polymerization device, producing; Exist same batch of material because discharging time is different; The fluctuation of indexs such as viscosity is bigger, and between criticizing and criticizing, because the cracking of the residual melt of agitated reactor inwall etc.; Be prone to cause the difference of properties of product between criticizing and criticizing, these problems all can directly influence the inherent quality of back processing spinning properties and final products.Modified copolyester section simultaneously needs crystallizing and drying and fusion again, and technological process is long, production link is many, production cost is higher.
Publication number 200710068740.9; A kind of " preparation method of continuous condensed direct-spinning cation dye dyeable polyester long filament " disclosed; On continuous polycondensation equipment,, add ethylene isophthalate-5-sodium sulfonate and the anti-agent of ether in Esterification Stage then earlier with p-phthalic acid and the making beating of ethylene glycol monomer; Stabilizing agent makes the cation dyeable polyester melt; Again through the melt Conveying pipeline, through measure, extrude, drawing-off, coiling make The cation-dyeable polyester pre-oriented yarn or The cation-dyeable polyester fully oriented filament, but this production is conventional cation dyeable polyester long filament.
Summary of the invention
In order to address the above problem, the object of the present invention is to provide a kind of preparation method of continuous polymerization directly-spun cation-dyeable high-shrinkage polyester filaments.Flow process of the present invention is short, operation is few, technology is reasonable, and melt quality is stable, good spinning performance; The high-shrinkage fibre stable contraction rate property that makes is good, even dyeing, the characteristics that production cost is low.
For reaching above-mentioned purpose, the present invention adopts following technical scheme:
A kind of preparation method of continuous polymerization directly-spun cation-dyeable high-shrinkage polyester filaments adopts continuity method polyester manufacture technology, comprises the preparation technology of continuous polymerization modified copolyester melt and the preparation technology of directly-spun cation-dyeable high-shrinkage polyester filaments; And in the preparation technology of continuous polymerization modified copolyester melt, adopting p-phthalic acid (PTA), ethylene glycol (EG) monomer is raw material; Add M-phthalic acid (IPA) and ethylene isophthalate-5-sodium sulfonate (SIPE) respectively as the raw material of the 3rd monomer and the 4th monomer; Make the modified copolyester melt; Above-mentioned then modified copolyester melt is directly through melt Conveying pipeline equipment, makes a kind of in cationic-dyeable high-shrinkage polyester pre-oriented yarn (POY) or the cationic-dyeable high-shrinkage polyester drafted fibre (FDY) respectively through the cooling of measuring, extrude, dry, drawing and heat-setting, coiling step.
The preparation technology of described continuous polymerization modified copolyester melt comprises the steps: at first on continuous polycondensation equipment; Adopt p-phthalic acid (PTA), M-phthalic acid (IPA), ethylene glycol (EG) and ethylene isophthalate-5-sodium sulfonate (SIPE) monomer; Account for the mol ratio 1 of molar percentage 6.0-10.0, total dicarboxylic acid and the dihydroxylic alcohols (ethylene glycol) of total dicarboxylic acid (summation of p-phthalic acid, M-phthalic acid and ethylene isophthalate-5-sodium sulfonate): 1.15-1 in M-phthalic acid (IPA): 1.20 ratio is measured p-phthalic acid (PTA), M-phthalic acid (IPA), ethylene glycol (EG) continuously and stably separately and is joined in the slurry still and pull an oar earlier, adds catalyst in the making beating still; Above-mentioned slurry continous-stable is delivered in esterification-I, the esterification-II agitated reactor; Ethylene isophthalate-5-the sodium sulfonate and the ether that add the molar percentage 2.0-4.0 that accounts for total dicarboxylic acid simultaneously continuously in esterification-II agitated reactor are prevented agent, stabilizing agent; 245-255 ℃ of control esterification-II temperature of reaction kettle; Time of staying 30-50 minute; The carboxylate that mixes is pumped into polycondensation workshop section, at temperature 260-285 ℃, makes the modified copolyester melt by conventional polycondensating process under the condition of vacuum 0.1-10KPa.
The preparation technology of described cation-dyeable high-shrinkage polyester filaments comprises the steps: above-mentioned modified copolyester melt; Through melt Conveying pipeline equipment; Be transported on the corresponding melt directly spinning filament production equipment, through measuring, extrude, dry cooling, drawing and heat-setting, winding process, the temperature of wherein controlling the melt Conveying pipeline is 270-280 ℃; Spinning body temperature is 280-290 ℃; Lateral blowing wind speed 0.3-0.8 meter per second, spinning speed 2500-3500 rice/minute, make cationic-dyeable high-shrinkage polyester pre-oriented yarn (POY).
The preparation technology of described cation-dyeable high-shrinkage polyester filaments comprises the steps: above-mentioned modified copolyester melt, through melt Conveying pipeline equipment, is transported on the corresponding melt directly spinning filament production equipment; Through measuring, extrude, dry cooling, drawing and heat-setting, winding process, the temperature of control melt Conveying pipeline is 270-280 ℃, and spinning body temperature is 280-290 ℃; Lateral blowing wind speed 0.3-0.8 meter per second; The first hot-rolling speed 800-1500 rice/minute, temperature 60-85 ℃, the second hot-rolling speed 3500-4200 rice/minute; Temperature 90-110 ℃, make cationic-dyeable high-shrinkage polyester drafted fibre (FDY).
Described catalyst adopts a kind of in antimony glycol, antimony oxide and the antimony acetate.
The anti-agent of described ether is for adopting a kind of in sodium acetate, the potassium acetate.
Described stabilizing agent adopts a kind of in phosphorous acid, trimethyl phosphate and the triphenyl phosphite.
Screw consecutive weighings conveying equipment is adopted in the conveying of described M-phthalic acid powder.
The invention has the beneficial effects as follows: integrated cost of the present invention and performance factor; Preferred M-phthalic acid (IPA) is as the 3rd monomer; Ethylene isophthalate-5-sodium sulfonate (SIPE) is the 4th monomer, in the continuity method polyester manufacture process of routine, through add the IPA of 6.0-10.0% in the slurry preparation process; SIPE (crowd refers to account for the molar percentage of total dicarboxylic acid) at Esterification Stage interpolation 2.0-4.0% makes the modified copolyester melt; Above-mentioned modified copolyester melt is directly through melt Conveying equipment (pipeline), and cooling, drawing and heat-setting, coiling make high-shrinkage polyester pre-oriented yarn (POY) and high-shrinkage polyester drafted fibre (FDY) respectively through measuring, extruding, dry.The preparation method of continuous polymerization directly-spun high-shrinkage polyester filaments of the present invention, because flow process is short, operation is few, technology is reasonable, the content of carboxyl end group of melt (COOH)≤30.0mol/t; Inherent viscosity [η] deviation ± 0.010, constant product quality, the filament contraction rate that makes is greater than 40%; And stable contraction rate; Even dyeing, good spinning performance, production cost obviously descends.
The specific embodiment
Through specific embodiment, the present invention is done further description below.Inherent viscosity deviation dl/g wherein, continuity method refers to inherent viscosity maximum and minimum of a value poor in 24 hours; Batch process refers to that the head material is poor with the inherent viscosity of tailing in the same batch of material.The mensuration of boiling water shrinkage is the endless tow of getting before cutting off, and is undertaken by the method for testing of general polyester filament.IPA in following examples, the addition of SIPE all refer to account for the molar percentage of total dicarboxylic acid (PTA, IPA and SIPE summation); The content of catalyst, stabilizing agent all refers to account for the percentage by weight of aggregated capacity.
Embodiment 1
The preparation technology of modified copolyester: the production capacity of on continuous polycondensation equipment, setting 6000kg/hr; Molar percentage 6.0, total dicarboxylic acid and the dihydroxylic alcohols (EG) that PTA, IPA and EG monomer is accounted for total dicarboxylic acid (PTA, IPA and SIPE summation) by IPA joins in the slurry still by 1: 1.20 mol ratio, adds the polycondensation catalyst antimony glycol of 450PPM (percentage by weight of aggregated capacity) in the still of pulling an oar simultaneously; Above-mentioned slurry continous-stable is delivered in esterification-I agitated reactor; Control esterification-I agitated reactor pressure is 0.12MPa, 258.0 ℃ of temperature, material level 60.0%; Material in esterification-I agitated reactor is sent in esterification-II agitated reactor; 255 ℃ of control esterifications-II temperature of reaction kettle, material level 60.0%, 50 minutes time of staying; The allotment concentration of adding the molar percentage 4.0 that accounts for total dicarboxylic acid simultaneously continuously is 40.0% SIPE; The ether of 300PPM (accounting for the percentage by weight of aggregated capacity) is prevented the stabilizing agent trimethyl phosphate of agent sodium acetate, 100PPM (accounting for the percentage by weight of aggregated capacity), is pumped into polycondensation workshop section with prepolymer then, makes modified copolyester by conventional polycondensating process.(result sees table 1)
Embodiment 2
The method of present embodiment is basic identical with embodiment 1; Different is: the addition of IPA is 8.0%; 259.0 ℃ of esterifications-I temperature of reaction kettle, 258 ℃ of esterifications-II temperature of reaction kettle, the addition of SIPE is 3.0%; Be pumped into polycondensation workshop section with prepolymer then, make modified copolyester by conventional polycondensating process.(result sees table 1)
Embodiment 3
The method of present embodiment is basic identical with embodiment 1; Different is: the addition of IPA is 10.0%; 260.0 ℃ of esterifications-I temperature of reaction kettle, 260 ℃ of esterifications-II temperature of reaction kettle, the addition of SIPE is 2.0%; Be pumped into polycondensation workshop section with prepolymer then, make modified copolyester by conventional polycondensating process.(result sees table 1)
Embodiment 4
The method of present embodiment is basic identical with embodiment 1; Different is: the addition of IPA is 8.0%, and total dicarboxylic acid and dihydroxylic alcohols join in the slurry still by 1: 1.18 mol ratio, 259.0 ℃ of esterifications-I temperature of reaction kettle; 258 ℃ of esterifications-II temperature of reaction kettle; The addition of SIPE is 3.0%, is pumped into polycondensation workshop section with prepolymer then, makes modified copolyester by conventional polycondensating process.(result sees table 1)
Embodiment 5
The method of present embodiment is basic identical with embodiment 1; Different is: the addition of IPA is 8.0%, and total dicarboxylic acid and dihydroxylic alcohols join in the slurry still by 1: 1.15 mol ratio, 260.0 ℃ of esterifications-I temperature of reaction kettle; 260 ℃ of esterifications-II temperature of reaction kettle; The addition of SIPE is 3.0%, is pumped into polycondensation workshop section with prepolymer then, makes modified copolyester by conventional polycondensating process.(result sees table 1)
Embodiment 6
Of embodiment 4: the modified copolyester melt that embodiment 4 is made; Be delivered directly on the corresponding melt directly spinning filament production equipment, through measuring, extrude, dry cooling, drawing and heat-setting, winding process, the temperature of wherein controlling the melt Conveying pipeline is 275 ℃; Spinning body temperature is 285 ℃; Lateral blowing wind speed 0.6 meter per second, 2800 meters/minute of spinning speeds make 110dtex/48f pre-oriented yarn (POY).(result sees table 2)
Embodiment 7
Of embodiment 4: the modified copolyester melt that embodiment 4 is made; Be delivered directly on the corresponding melt directly spinning filament production equipment, through measuring, extrude, dry cooling, drawing and heat-setting, winding process, the temperature of wherein controlling the melt Conveying pipeline is 275 ℃; Spinning body temperature is 290 ℃; Lateral blowing wind speed 0.6 meter per second, 3200 meters/minute of spinning speeds make 110dtex/48f pre-oriented yarn (POY).(result sees table 2)
Embodiment 8
Of embodiment 4: as with the modified copolyester melt that embodiment 4 makes, to be delivered directly on the corresponding melt directly spinning filament production equipment, through measuring, extrude, dry cooling, drawing and heat-setting, winding process; The temperature of wherein controlling the melt Conveying pipeline is 275 ℃, and spinning body temperature is 285 ℃, lateral blowing wind speed 0.5 meter per second; 1000 meters/minute of the first hot-rolling speed, 65 ℃ of temperature, 3600 meters/minute of the second hot-rolling speed; 80 ℃ of temperature make 35dtex/24f drafted fibre (FDY).(result sees table 2)
Embodiment 9
Of embodiment 4: as with the modified copolyester melt that embodiment 4 makes, to be delivered directly on the corresponding melt directly spinning filament production equipment, through measuring, extrude, dry cooling, drawing and heat-setting, winding process; The temperature of wherein controlling the melt Conveying pipeline is 275 ℃, and spinning body temperature is 290 ℃, lateral blowing wind speed 0.5 meter per second; 1200 meters/minute of the first hot-rolling speed, 70 ℃ of temperature, 3800 meters/minute of the second hot-rolling speed; 85 ℃ of temperature make drafted fibre (FDY).Make 35dtex/24f drafted fibre (FDY).(result sees table 2)
Comparative example 1
On production capacity is criticized for about 3500KG/ intermittence polyester equipment, the TPA of 2700KG, the IPA of 300KG, the EG monomer of 1500L are joined in the slurry still, add the stabilizing agent (trimethyl phosphate) of 450ml in the making beating still; 1500g polycondensation catalyst (antimony glycol), after mixing, above-mentioned slurry continous-stable is delivered in esterification-I agitated reactor; 255.0 ℃ of control esterifications-I temperature of reaction kettle, pressure is normal pressure, treat that the water outlet of esterification water reaches 680L after; Esterification-I material in reactor is sent in esterification-II agitated reactor, and 40.0% SIPE460L is added concentration and is in 240-250 ℃ of control esterification-II temperature of reaction kettle; Control time of staying 40-50 minute; Esterification finishes, and delivers to polycondensation workshop section with nitrogen pressure then, makes modified copolyester by conventional polycondensating process.(result sees table 1)
Comparative example 2
Of comparative example 1: that the modified copolyester that comparative example 1 makes is cut into slices; Through crystallizing and drying, section moisture content≤50PPM is done in control, and extruder temperature is 270-285 ℃; Spinning body temperature is 285 ℃; Lateral blowing wind speed 0.6 meter per second, 3200 meters/minute of spinning speeds make 110dtex/48f pre-oriented yarn (POY).(result sees table 2)
Comparative example 3
Of comparative example 1: with the modified copolyester section that comparative example 1 makes, through crystallizing and drying, section moisture content≤50PPM is done in control; Extruder temperature is 270-285 ℃, and spinning body temperature is 285 ℃, lateral blowing wind speed 0.5 meter per second; 1200 meters/minute of the first hot-rolling speed, 70 ℃ of temperature, 3800 meters/minute of the second hot-rolling speed; 85 ℃ of temperature make drafted fibre (FDY).Make 35dtex/24f drafted fibre (FDY).(result sees table 2)
Table 1
Table 2
Claims (1)
1. the preparation method of a continuous polymerization fused mass directly spinning cation-dyeable high-shrinkage polyester filaments; Adopt continuity method polyester manufacture technology, it is characterized in that: comprise the preparation technology of continuous polymerization modified copolyester melt and the preparation technology of directly-spun cation-dyeable high-shrinkage polyester filaments; And in the preparation technology of continuous polymerization modified copolyester melt, adopting p-phthalic acid, ethylene glycol monomer is raw material; Add M-phthalic acid and ethylene isophthalate-5-sodium sulfonate respectively as the raw material of the 3rd monomer and the 4th monomer, make the modified copolyester melt; Above-mentioned modified copolyester melt is directly through melt Conveying pipeline equipment, makes a kind of in cationic-dyeable high-shrinkage polyester pre-oriented yarn or the cationic-dyeable high-shrinkage polyester drafted fibre respectively through the cooling of measuring, extrude, dry, drawing and heat-setting, coiling step; The preparation technology of described modified copolyester melt comprises the steps: at first on continuous polycondensation equipment; Adopt p-phthalic acid, M-phthalic acid, ethylene glycol and ethylene isophthalate-5-sodium sulfonate monomer; Mol ratio 1 in molar percentage 6.0-10.0, total dicarboxylic acid and the dihydroxylic alcohols of isophthalic acid comprises total dicarboxylic acid: 1.15-1: 1.20 ratio is measured p-phthalic acid, M-phthalic acid, ethylene glycol continuously and stably separately and is joined in the slurry still earlier and pulls an oar, and adds catalyst in the making beating still; Then above-mentioned slurry continous-stable is delivered in esterification-I, the esterification-II agitated reactor; Ethylene isophthalate-5-the sodium sulfonate and the ether that add the molar percentage 2.0-4.0 that accounts for total dicarboxylic acid simultaneously continuously in esterification-II agitated reactor are prevented agent, stabilizing agent; 245-255 ℃ of control esterification-II temperature of reaction kettle; Time of staying 30-50 minute; The carboxylate that mixes is pumped into polycondensation workshop section, at temperature 260-285 ℃, makes the modified copolyester melt by conventional polycondensating process under the condition of vacuum 0.1-10KPa; The preparation technology of described cation-dyeable high-shrinkage polyester filaments comprises the steps: above-mentioned modified copolyester melt; Through melt Conveying pipeline equipment; Be transported on the corresponding melt directly spinning filament production equipment, through measuring, extrude, dry cooling, drawing and heat-setting, winding process, the temperature of wherein controlling the melt Conveying pipeline is 270-280 ℃; Spinning body temperature is 280-290 ℃; Lateral blowing wind speed 0.3-0.8 meter per second, spinning speed 2500-3500 rice/minute, make cationic-dyeable high-shrinkage polyester pre-oriented yarn; The preparation technology of described cation-dyeable high-shrinkage polyester filaments comprises the steps: above-mentioned modified copolyester melt, through melt Conveying pipeline equipment, is transported on the corresponding melt directly spinning filament production equipment; Through measuring, extrude, dry cooling, drawing and heat-setting, winding process, the temperature of control melt Conveying pipeline is 270-280 ℃, and spinning body temperature is 280-290 ℃; Lateral blowing wind speed 0.3-0.8 meter per second; The first hot-rolling speed 800-1500 rice/minute, temperature 60-85 ℃, the second hot-rolling speed 3500-4200 rice/minute; Temperature 90-110 ℃, make cationic-dyeable high-shrinkage polyester drafted fibre; Described catalyst adopts a kind of in antimony glycol, antimony oxide and the antimony acetate; The anti-agent of described ether can be adopts a kind of in sodium acetate, the potassium acetate; Described stabilizing agent adopts a kind of in phosphorous acid, trimethyl phosphate and the triphenyl phosphite; Screw consecutive weighings conveying equipment is adopted in the conveying of described M-phthalic acid powder.
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| CN102828262A (en) * | 2012-07-20 | 2012-12-19 | 江苏盛虹科技股份有限公司 | Processing method for producing differential shrinkage composite fibers through melt direct spinning |
| CN110983596B (en) * | 2019-12-31 | 2021-02-09 | 深圳市宏翔新材料发展有限公司 | Preparation method of sports knitted fabric |
| CN111875786B (en) * | 2020-08-07 | 2023-06-30 | 安徽皖维高新材料股份有限公司 | Polyester for acrylic fiber one-bath dyeing type boson and preparation method thereof |
| CN113897695A (en) * | 2021-09-27 | 2022-01-07 | 杭州观晨实业有限公司 | Preparation method of continuous polymerization direct spinning cation dyeable high-shrinkage polyester pre-oriented yarn POY |
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