CN101787583A - Method for preparing continuous polymerization directly-spun high-shrinkage polyester filaments - Google Patents
Method for preparing continuous polymerization directly-spun high-shrinkage polyester filaments Download PDFInfo
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Abstract
The invention discloses a method for preparing continuous polymerization directly-spun 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, isophthalic acid and glycol monomers are taken as raw materials to prepare the modified copolyester melt; and the 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 high-shrinkage polyester preoriented yarns and 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 good shrinkage stability and even dyeing, and the production cost is reduced obviously.
Description
Technical field
The present invention relates to the preparation method of a kind of manufacture method of modified copolyester long filament, particularly a kind of continuous polymerization directly-spun high-shrinkage polyester filaments, belong to the chemical fibre field.
Background technology
Conventional polyester fiber, degree of crystallinity is higher, and percent thermal shrinkage is lower, generally is lower than 10%.Along with continually developing of the continuous expansion of polyester fiber Application Areas, fabric new product, increasing than the demand of the high-shrinkage fiber of high shrinkage to having, all kinds of high-shrinkage fibers are succeeded in developing in succession.
High-shrinkage fibre is meant that fiber boiling water or xeothermic contraction are greater than 25% chemical fibre.According to the difference of its thermal contraction degree, can obtain the final products of different-style and performance.Utilize these characteristics can produce various fabric with mannerism, as this fiber and other fibre-coated, mix fine, and twist with the fingers, can weave strong, the stylish bubble of third dimension, crepe fabrics, particularly interweave and to produce high-grade SUEDE FABRIC, imitative peach face, high-density fabric etc. with composite ultrafine fiber.
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 is mainly realized to change the spinning draw conditions, disclosed as Japan Patent (spy opens 2000-248425) is a kind of " production method of high-shrinkage fiber ", it is to use normal polyester, by special drawing-off after-processing technology, make the high-shrinkage fibre of fiber excellent in uniform.But this its stable contraction rate of high-shrinkage fibre that only makes by physical modification is relatively poor, fibre strength is low, so many at present methods that combine with chemical modification and physical modification are produced, promptly in the production process of normal polyester, pass through to add the 3rd monomer, destroy macromolecular regularity, reduce crystallizing power, and in conjunction with 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 as 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, by 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 ", 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.Japan Patent (spy opens flat 6-280114) is disclosed to be a kind of " high-shrinkage fiber ", it is to add the section that the 3rd monomer copolymerization of 8.0-25.0 mole % makes, improve the inherent viscosity of section earlier through solid phase polycondensation,, make the fiber of high-strength and high contraction then through the multistage drawing-off.Publication number CN1566176 is disclosed to be a kind of " the system high-shrinkage fiber preparation method of modified poly ester ", is monomer with terephthalic acid (TPA), M-phthalic acid and ethylene glycol, and precondensation and polycondensation reaction are carried out in the presence of a kind of composite catalyst.Publication number CN1896346 is disclosed to be a kind of " method of preparation of multi-stage shrinkage polyester fibre by one-step ", it is the key reaction raw material with terephthalic acid (TPA), M-phthalic acid, ethylene glycol and ethoxylation bisphenol-A, the preparation inherent viscosity is about 0.67～0.695, the copolyesters of 220 ℃～235 ℃ of fusing points, copolyesters is extruded through crystallization, drying, screw rod, adopt low speed spinning, low temperature high magnification drawing process, prepare multistage contraction copolyester fiber, its boiling water shrinkage 〉=35%.
The preparation method of above-mentioned high-shrinkage fiber, all be on the discontinuous polycondensation device, to make the modified copolyester section earlier by chemical modification, then modified copolyester is 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 the discharging time difference, the fluctuation of indexs such as viscosity is bigger, and between criticizing and criticizing, because the cracking of the residual melt of reactor inwall etc., easily 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.
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 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 that makes is good, even dyeing, and production cost obviously descends.
For reaching above-mentioned purpose, the present invention adopts following technical scheme:
A kind of preparation method of continuous polymerization directly-spun high-shrinkage polyester filaments comprises the preparation technology of continuous condensed modified copolyester melt and the preparation technology of directly-spun high-shrinkage polyester filaments; And adopting p-phthalic acid (PTA), M-phthalic acid (IPA), ethylene glycol (EG) monomer in the preparation technology of continuous condensed modified copolyester melt is raw material, make the modified copolyester melt, above-mentioned polyester fondant is directly by melt Conveying equipment (pipeline), makes a kind of in high-shrinkage polyester pre-oriented yarn (POY) or the high-shrinkage polyester drafted fibre (FDY) respectively through measuring, extrude, dry cooling, drawing and heat-setting, coiling.
The preparation technology of described modified copolyester melt comprises the steps: at first on continuous polycondensation equipment, adopt p-phthalic acid (PTA), M-phthalic acid (IPA), ethylene glycol (EG) monomer, account for the mol ratio 1 of molar percentage 8.0-14.0, total dicarboxylic acid and the dihydroxylic alcohols (EG) of total dicarboxylic acid (summation of p-phthalic acid and M-phthalic acid): 1.15-1 in M-phthalic acid (IPA): 1.20 ratio is measured continuously and stably separately and is joined in the slurry still and pulls an oar, and adds catalyst in the making beating still; Above-mentioned slurry continous-stable is delivered in esterification-I, the esterification-II reactor, adds stabilizing agent, control esterification yield 96.5%-98.5% in esterification-II reactor simultaneously continuously; Carboxylate is pumped into polycondensation workshop section, and polycondensating process makes the modified copolyester melt at temperature 260-285 ℃ under the condition of vacuum 0.1-10KPa routinely.
The preparation technology of described high-shrinkage polyester filaments comprises the steps: above-mentioned modified copolyester melt, by 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 265-275 ℃, spinning body temperature is 275-285 ℃, lateral blowing wind speed 0.3-0.8 meter per second, spinning speed 2500-3500 rice/minute, make high-shrinkage polyester pre-oriented yarn (POY).
The preparation technology of described high-shrinkage polyester filaments comprises the steps: above-mentioned modified copolyester melt, by melt Conveying pipeline equipment, be transported on the corresponding melt directly spinning filament production equipment, through metering, extrude, the blowing cooling, drawing and heat-setting, winding process, the temperature of wherein controlling the melt Conveying pipeline is 265-275 ℃, spinning body temperature is 275-285 ℃, 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 3500-4500 rice/minute, temperature 90-110 ℃, make high-shrinkage polyester drafted fibre (FDY).
Described catalyst adopts a kind of in antimony glycol, antimonous oxide and the antimony 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: the present invention is directed to the deficiencies in the prior art, a kind of preparation method of continuous polymerization fused mass directly spinning high-shrinkage polyester filaments is provided.The preferred M-phthalic acid of the present invention is as the 3rd monomer, in the continuity method polyester manufacture process of routine, by adding the M-phthalic acid of 8.0-14.0mol% (molar percentage of isophthalic acid comprises total dicarboxylic acid), produce the modified copolyester melt, above-mentioned polyester fondant directly by melt Conveying equipment (pipeline), makes high-shrinkage polyester pre-oriented yarn (POY) and high-shrinkage polyester drafted fibre (FDY) respectively through measuring, extrude, dry cooling, drawing and heat-setting, coiling.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 35%, and stable contraction rate, even dyeing, good spinning performance, production cost obviously descends.
The specific embodiment
Below by specific embodiment, the invention will be further described.Inherent viscosity deviation dl/g wherein: continuity method refers to the poor of inherent viscosity maximum in 24 hours and minimum of a value; The gap method 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.The addition of IPA in following examples all refers to account for the molar percentage of total dicarboxylic acid (PTA and IPA 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 5000kg/hr, with the p-phthalic acid, M-phthalic acid and ethylene glycol monomer are by the molar percentage 8.0 of isophthalic acid comprises total dicarboxylic acid, total dicarboxylic acid (summation of p-phthalic acid and M-phthalic acid) joins in the slurry still with the mol ratio of dihydroxylic alcohols (EG) by 1: 1.20, pull an oar simultaneously and add the polycondensation catalyst antimony glycol of 450PPM (percentage by weight of aggregated capacity) in the still, above-mentioned slurry continous-stable is delivered in esterification-I reactor, control esterification-I reactor pressure is 0.12MPa, 258.0 ℃ of temperature, material level 60.0%, recording esterification yield is 88.1%, material in esterification-I reactor is sent in esterification-II reactor, add the stabilizing agent trimethyl phosphate of 100PPM (percentage by weight of aggregated capacity) simultaneously continuously, 260 ℃ of the temperature of control esterification-II reactor, material level 60.0%, recording esterification yield is 97.5%, be pumped into polycondensation workshop section with prepolymer then, polycondensating process makes modified copolyester routinely.(the results are shown in Table 1)
Embodiment 2
The method of present embodiment is basic identical with embodiment 1, different is: the molar percentage 11.0 of isophthalic acid comprises total dicarboxylic acid, 259.0 ℃ of control esterifications-I temperature of reaction kettle, recording esterification yield is 88.5%, 261 ℃ of control esterifications-II temperature of reaction kettle, recording esterification yield is 98.2%, is pumped into polycondensation workshop section with prepolymer then, and polycondensating process makes modified copolyester routinely.(the results are shown in Table 1)
Embodiment 3
The method of present embodiment is basic identical with embodiment 1, different is: the molar percentage 14.0 of isophthalic acid comprises total dicarboxylic acid, 260.0 ℃ of control esterifications-I temperature of reaction kettle, recording esterification yield is 90.1%, 262 ℃ of control esterifications-II temperature of reaction kettle, recording esterification yield is 98.5%, is pumped into polycondensation workshop section with prepolymer then, and polycondensating process makes modified copolyester routinely.(the results are shown in Table 1)
Embodiment 4
The method of present embodiment is basic identical with embodiment 1, different is: the molar percentage 11.0 of isophthalic acid comprises total dicarboxylic acid, total dicarboxylic acid and dihydroxylic alcohols join in the slurry still by 1: 1.18 mol ratio, 259.0 ℃ of control esterifications-I temperature of reaction kettle, recording esterification yield is 88.0%, 261 ℃ of control esterifications-II temperature of reaction kettle, and recording esterification yield is 97.9%, be pumped into polycondensation workshop section with prepolymer then, polycondensating process makes modified copolyester routinely.(the results are shown in Table 1)
Embodiment 5
The method of present embodiment is basic identical with embodiment 1, different is: the molar percentage 11.0 of isophthalic acid comprises total dicarboxylic acid, total dicarboxylic acid and dihydroxylic alcohols join in the slurry still by 1: 1.15 mol ratio, 260.0 ℃ of control esterifications-I temperature of reaction kettle, recording esterification yield is 87.5%, 262 ℃ of control esterifications-II temperature of reaction kettle, and recording esterification yield is 97.6%, be pumped into polycondensation workshop section with prepolymer then, polycondensating process makes modified copolyester routinely.(the results are shown in Table 1)
Embodiment 6
As described in 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 270 ℃, spinning body temperature is 280 ℃, lateral blowing wind speed 0.6 meter per second, 2800 meters/minute of spinning speeds make 167dtex/48f pre-oriented yarn (POY).(the results are shown in Table 2)
Embodiment 7
As described in 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 270 ℃, spinning body temperature is 85 ℃, lateral blowing wind speed 0.6 meter per second, 3200 meters/minute of spinning speeds make 167dtex/48f pre-oriented yarn (POY).(the results are shown in Table 2)
Embodiment 8
As described in 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 270 ℃, and spinning body temperature is 280 ℃, lateral blowing wind speed 0.5 meter per second, 1000 meters/minute of the first hot-rolling speed, 65 ℃ of temperature, 3500 meters/minute of the second hot-rolling speed, 85 ℃ of temperature make 56dtex/24f drafted fibre (FDY).(the results are shown in Table 2)
Embodiment 9
As described in 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 270 ℃, and spinning body temperature is 285 ℃, lateral blowing wind speed 0.5 meter per second, 1200 meters/minute of the first hot-rolling speed, 75 ℃ of temperature, 4000 meters/minute of the second hot-rolling speed, 95 ℃ of temperature make drafted fibre (FDY).Make 56dtex/24f drafted fibre (FDY).(the results are shown in Table 2)
Comparative example 1
On production capacity is criticized for about 3500KG/ intermittence polyester equipment, with the 3000KG p-phthalic acid, the 330KG M-phthalic acid, 1500L ethylene glycol monomer joins in the slurry still, the stabilizing agent (trimethyl phosphate) that adds 350ml in the making beating still, 1500g polycondensation catalyst (antimony glycol), after mixing, above-mentioned slurry continous-stable is delivered in esterification-I reactor, 255.0 ℃ of control esterifications-I reactor temperature, pressure is normal pressure, after treating that the water outlet of esterification water reaches 700L, esterification finishes, and delivers to polycondensation workshop section with nitrogen pressure then, and polycondensating process makes modified copolyester routinely.(the results are shown in Table 1)
Comparative example 2
As described in comparative example 1: the modified copolyester that comparative example 1 makes is cut into slices, through crystallizing and drying, section moisture content≤50PPM is done in control, 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 167dtex/48f pre-oriented yarn (POY).(the results are shown in Table 2)
Comparative example 3
As described in comparative example 1: 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 ℃, and spinning body temperature is 285 ℃, lateral blowing wind speed 0.5 meter per second, 1200 meters/minute of the first hot-rolling speed, 75 ℃ of temperature, 4000 meters/minute of the second hot-rolling speed, 95 ℃ of temperature make drafted fibre (FDY).Make 56dtex/24f drafted fibre (FDY).(the results are shown in Table 2)
Table 1
Table 2
Claims (7)
1. the preparation method of a continuous polymerization directly-spun high-shrinkage polyester filaments is characterized in that: comprise the preparation technology of continuous condensed modified copolyester melt and the preparation technology of directly-spun high-shrinkage polyester filaments; And adopting p-phthalic acid, M-phthalic acid, ethylene glycol monomer in the preparation technology of continuous condensed modified copolyester melt is raw material, make the modified copolyester melt, above-mentioned polyester fondant is directly by melt Conveying pipeline equipment, makes a kind of in high-shrinkage polyester pre-oriented yarn or the high-shrinkage polyester drafted fibre respectively through measuring, extrude, dry cooling, drawing and heat-setting, coiling.
2. the preparation method of continuous polymerization directly-spun high-shrinkage polyester filaments according to claim 1, it is characterized in that: 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 monomer, mol ratio 1 in molar percentage 8.0-14.0, total dicarboxylic acid and the dihydroxylic alcohols of isophthalic acid comprises total dicarboxylic acid: 1.15-1: 1.20 ratio is measured continuously and stably separately and is joined in the slurry still and pulls an oar, and adds catalyst in the making beating still; Above-mentioned slurry continous-stable is delivered in esterification-I, the esterification-II reactor, adds stabilizing agent, control esterification yield 96.5%-98.5% in esterification-II reactor simultaneously continuously; Carboxylate is pumped into polycondensation workshop section, and polycondensating process makes the modified copolyester melt at temperature 260-285 ℃ under the condition of vacuum 0.1-10KPa routinely.
3. the preparation method of continuous polymerization directly-spun high-shrinkage polyester filaments according to claim 1, it is characterized in that: the preparation technology of described high-shrinkage polyester filaments comprises the steps: above-mentioned modified copolyester melt, by melt Conveying pipeline equipment, be transported on the corresponding melt directly spinning filament production equipment, through metering, extrude, the blowing cooling, drawing and heat-setting, winding process, the temperature of wherein controlling the melt Conveying pipeline is 265-275 ℃, spinning body temperature is 275-285 ℃, lateral blowing wind speed 0.3-0.8 meter per second, spinning speed 2500-3500 rice/minute, make the high-shrinkage polyester pre-oriented yarn.
4. the preparation method of continuous polymerization directly-spun high-shrinkage polyester filaments according to claim 1, it is characterized in that: the preparation technology of described high-shrinkage polyester filaments comprises the steps: above-mentioned modified copolyester melt, by melt Conveying pipeline equipment, be transported on the corresponding melt directly spinning filament production equipment, through metering, extrude, the blowing cooling, drawing and heat-setting, winding process, the temperature of wherein controlling the melt Conveying pipeline is 265-275 ℃, spinning body temperature is 275-285 ℃, 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 3500-4500 rice/minute, temperature 90-110 ℃, make the high-shrinkage polyester drafted fibre.
5. the preparation method of continuous polymerization directly-spun high-shrinkage polyester filaments according to claim 2 is characterized in that: described catalyst adopts a kind of in antimony glycol, antimonous oxide and the antimony acetate.
6. the preparation method of continuous polymerization directly-spun high-shrinkage polyester filaments according to claim 2 is characterized in that: described stabilizing agent adopts a kind of in phosphorous acid, trimethyl phosphate and the triphenyl phosphite.
7. the preparation method of continuous polymerization directly-spun high-shrinkage polyester filaments according to claim 2 is characterized in that: the conveying employing screw consecutive weighings conveying equipment of described M-phthalic acid powder.
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