CN101070642A - Method for preparing polyester filament capable being dyed by continuous condensed direct-spinning cation dye - Google Patents
Method for preparing polyester filament capable being dyed by continuous condensed direct-spinning cation dye Download PDFInfo
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Abstract
A method for making a continuous polycondensation direct spinning cationic dye and tinctable polyester filament, it pertains to chemical art. Refining terephthalic acid and Glycol Monomer are raw materials, also including the preparation continuous polycondensation cationic dye and can-be-stained polyester and direct spinning dye tinctable polyester filament. In the present continuous polyester device, first beat the refining terephthalic acid and Glycol, then add Benzene PTA acid Glycol ester-5-Sodium and Ether-agent and stabilizer to get cationic dye tinctable polycondensation melt, then through pipeline, after measure, extrude, draw, wind to obtain cationic dye tinctable polyester pre-orientation silk or cationic dye can-be-stained polyester all-orientation silk. The invention has a short and less process, reasonable art. The quality of product is stable. And the fiber gained has high intensity, small deviation, and is dyed well-distributed, and has a better spinning quality. It can decrease production cost.
Description
Technical field
The present invention relates to a kind of preparation method of continuous condensed direct-spinning cation dye dyeable polyester long filament, belong to the manufacturing technology field of chemical fibre.
Background technology
As everyone knows, polyester (terylene) fiber has worldwide obtained development rapidly owing to have good physical and mechanical property and good comprehensive wearing characteristics.But because the tight packing of polyester molecule chain, the degree of crystallinity and the degree of orientation are higher, polarity is less, between the polyester long-chain molecule, there is not suitably to hold the gap of dye molecule, therefore dye particles is difficult for penetrating fiber, its dyeability is poor, can use the kind of dyestuff few, and general polyester fiber can only adopt DISPERSE DYES High Temperature High Pressure and higher temperature carrier dyeing.And cationic-dyeable polyester fibers is succeeded in developing in succession owing to have characteristics such as the look of suction is good, beautiful in colour, chromatogram is complete, and Application Areas is more and more wider.
At present, the preparation method of cationic-dyeable polyester fibers mainly contains following several:
1. first gap or the section of continuous condensed preparation cation dyeable polyester, cationic-dyeable polyester fibers is produced in slice spinning again.
The mode of production of gap polycondensation: opening clear 57-57054 communique, spy as the spy, to open disclosed in the clear 52-47098 communique all be on the interstitial polymerization device, by adding ethylene isophthalate-5-sodium sulfonate (SIPE), the section of preparation cation dyeable polyester.The said goods content of carboxyl end group of producing on the interstitial polymerization device is (COOH) higher, generally at 40～50mol/t, exist same batch of material simultaneously because the discharging time difference, expect that end to end inherent viscosity, colour indexs such as (b values) fluctuate bigger, and between criticizing and criticizing, because the cracking of the residual melt of reactor inwall etc., easily cause batch with criticize between the difference of product physical property.These problems all can directly influence the inherent quality of back processing spinning properties and final products.
The continuous condensed mode of production: open the method that discloses production cation dyeable polyester section on continuous polymerization unit in the 2002-80572 communique as the spy, make the indexs such as slicing characteristics viscosity that make more stable, back processing characteristics is improved greatly.Publication number CN1362548 discloses a kind of gap polycondensation and has produced cation dyeable polyester, the drying of cutting into slices then, spinning, drawing-off, adds the method that operation such as bullet is produced cationic-dyeable polyester fibers.
Below all be to make the cation dyeable polyester section earlier, and then produce cationic-dyeable polyester fibers with the method for slice spinning.It is many to exist production link, problem such as higher or product quality shakiness of production cost.
2. " polyester industrial " 2003 the 6th phases have been delivered the article of a piece " continuous condensed direct-spinning cation dye can dye the exploitation of polyester staple fiber ", its method is on the 50T/D continuous condensed direct spins, and prepares the The cation-dyeable polyester staple fibre by add the 3rd, the 4th monomer in Esterification Stage.Low, the steady quality of development product production cost.But this product of researching and producing only refers to polyester staple fiber.
Summary of the invention
The purpose of this invention is to provide a kind ofly at the deficiencies in the prior art, technology is reasonable, the preparation method of the continuous condensed direct-spinning cation dye dyeable polyester long filament that flow process is short, operation is few.
The present invention is the preparation method of continuous condensed direct-spinning cation dye dyeable polyester long filament, with p-phthalic acid and ethylene glycol monomer is raw material, comprise the preparation of continuous condensed cation dyeable polyester melt and the preparation of direct-spinning cation dye dyeable polyester long filament, it is characterized in that being undertaken by following manufacturing procedure:
The preparation of a, polyester fondant: on existing continuous polycondensation equipment, p-phthalic acid and ethylene glycol monomer are joined in the slurry still by 1: 1.18～1: 1.25 mol ratio pull an oar adding conventional catalyst in the slurry still earlier; Then above-mentioned slurry continous-stable is delivered in esterification-I reactor, control esterification yield 88%～92%, again carboxylate is sent into esterification-II reactor, add ethylene isophthalate-5-sodium sulfonate (SIPE) and the anti-agent of ether of p-phthalic acid's molal quantity 1.5-2.5 mole % in esterification-II reactor simultaneously continuously, stabilizing agent, 245～255 ℃ of temperature in control esterification-II reactor, 30～50 minutes time of staying, the carboxylate that mixes is pumped into polycondensation workshop section, polycondensating process makes the cation dyeable polyester melt 260～285 ℃ of temperature under the condition of vacuum 0.1～10KPr routinely;
The preparation of b, polyester filament: with above-mentioned cation dyeable polyester melt, by the melt Conveying pipeline, through measure, extrude, drawing-off, coiling make The cation-dyeable polyester pre-oriented yarn (POY) or The cation-dyeable polyester fully oriented filament (FDY).
The preparation of described The cation-dyeable polyester pre-oriented yarn (POY) can be on existing melt directly spinning filament production equipment, the temperature of control melt Conveying pipeline is 275～290 ℃, spinning body temperature is 280～290 ℃, lateral blowing wind speed 0.3～0.8 meter per second, 2500～3500 meters/minute of spinning speeds make pre-oriented yarn (POY).
The preparation of described The cation-dyeable polyester fully oriented filament (FDY) can be on existing melt directly spinning filament production equipment, the temperature of control melt Conveying pipeline is 275～290 ℃, spinning body temperature is 280～290 ℃, lateral blowing wind speed 0.3～0.8 meter per second, 140～180 ℃ of heat pipe temperatures, spinning speed 3500～5000m/minute, make fully oriented filament (FDY).
Described conventional catalyst can be antimony glycol or antimonous oxide etc., and its addition can be 350～500PPM of polyester fondant total amount.
The anti-agent of described ether can be sodium acetate or potassium acetate etc., and its addition can be 300～400PPM of polyester fondant total amount.
Described stabilizing agent can be phosphorous acid or trimethyl phosphate, triphenyl phosphite etc., and its addition can be 100～200PPM of polyester fondant total amount.
The present invention is directed to the deficiencies in the prior art, in the continuity method polyester manufacture process of routine, add ethylene isophthalate-5-sodium sulfonate (SIPE) of 1.5-2.5mol%, produce the cation dyeable polyester melt, above-mentioned polyester fondant directly by melt Conveying equipment (Melt Pump, melt pipe), makes The cation-dyeable polyester pre-oriented yarn (POY) and The cation-dyeable polyester fully oriented filament (FDY) respectively through measuring, extrude, cool off (heating), drawing-off, coiling.The preparation method of continuous condensed direct-spinning cation dye dyeable polyester long filament 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 fibre strength height that makes, deviation is little, even dyeing, good spinning performance, production cost obviously descends.
The specific embodiment
Owing to add the carboxylate behind ethylene isophthalate-5-sodium sulfonate (SIPE), easily at high temperature etherificate generates diethylene glycol (DEG) (DEG), the diethylene glycol (DEG) too high levels, the heat endurance of melt descends greatly, so in the method production technology of gap, the control of the temperature of esterification-II is very important, usually be chosen under the lower temperature and add SIPE, to be mixed evenly after, suitably improve temperature of charge again, send the reaction of polycondensation section then.And for continuous condensed production technology, the temperature of respectively distinguishing of reactor is constant, can not raise at any time or reduce, the Tai Gaoyi side reaction generates DEG, the too low esterification yield that can't guarantee carboxylate again, so must take all factors into consideration the various factors choose reasonable, generate DEG in order to suppress side reaction simultaneously, the ratio gap method suitably increases the addition of the anti-agent sodium acetate of ether.
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.
Embodiment 1, the preparation of cation dyeable polyester melt: the production capacity of on existing continuous polycondensation equipment, setting 7200kg/hr, with the p-phthalic acid, the ethylene glycol monomer joins in the slurry still by 1: 1.18 mol ratio, the polycondensation catalyst antimony glycol that adds 350PPM simultaneously in the slurry still, above-mentioned slurry continous-stable is delivered in esterification-I reactor, control esterification-I pressure is 0.12MPa, 258.0 ℃ of temperature, material level 50.0%, recording esterification yield is 88.0%, esterification-I material is sent into esterification-II, 255 ℃ of control esterifications-II temperature, material level 60.0%, the allotment concentration of adding 1.5mol% simultaneously continuously is ethylene isophthalate-5-sodium sulfonate (SIPE) of 40.0%, and the ether of 300PPM is prevented the agent sodium acetate, the stabilizing agent trimethyl phosphate of 100PPM, 50 minutes time of staying of control, be pumped into polycondensation workshop section with prepolymer then, polycondensating process makes the cation dyeable polyester melt routinely.
Embodiment 2: as described in embodiment 1, different is: with the p-phthalic acid, the ethylene glycol monomer joins in the slurry still by 1: 1.20 mol ratio, the polycondensation catalyst antimony glycol that adds 450PPM simultaneously in the slurry still, control esterification-I material level 55.0%, recording esterification yield is 90.2%, 250 ℃ of control esterifications-II temperature, material level 55.0%, the allotment concentration of adding 2.0mol% simultaneously continuously is ethylene isophthalate-5-sodium sulfonate (SIPE) of 40.0%, the ether of 350PPM is prevented the agent sodium acetate, the stabilizing agent trimethyl phosphate of 150PPM, 40 minutes time of staying of control, be pumped into polycondensation workshop section with prepolymer then, polycondensating process makes the cation dyeable polyester melt routinely.
Embodiment 3: as described in embodiment 1, different is: with the p-phthalic acid, the ethylene glycol monomer joins in the slurry still by 1: 1.25 mol ratio, the polycondensation catalyst antimony glycol that adds 500PPM simultaneously in the slurry still, control esterification-I material level 50.0%, recording esterification yield is 92.1%, 245 ℃ of control esterifications-II temperature, material level 50.0%, the allotment concentration of adding 2.5mol% simultaneously continuously is ethylene isophthalate-5-sodium sulfonate (SIPE) of 40.0%, the ether of 400PPM is prevented the agent sodium acetate, the stabilizing agent trimethyl phosphate of 200PPM, 30 minutes time of staying of control, be pumped into polycondensation workshop section with prepolymer then, polycondensating process makes the cation dyeable polyester melt routinely.
Embodiment 4: as described in embodiment 1, different is: with the p-phthalic acid, the ethylene glycol monomer joins in the slurry still by 1: 1.20 mol ratio, the polycondensation catalyst antimony glycol that adds 450PPM simultaneously in the slurry still, control esterification-I material level 55.0%, recording esterification yield is 90.3%, 250 ℃ of control esterifications-II temperature, material level 55.0%, the allotment concentration of adding 1.5mol% simultaneously continuously is ethylene isophthalate-5-sodium sulfonate (SIPE) of 40.0%, the ether of 350PPM is prevented the agent sodium acetate, the stabilizing agent trimethyl phosphate of 150PPM, 40 minutes time of staying of control, be pumped into polycondensation workshop section with prepolymer then, polycondensating process makes the cation dyeable polyester melt routinely.
Embodiment 5: the cation dyeable polyester melt that embodiment 1 is made, on existing melt directly spinning filament production equipment, the temperature of control melt Conveying pipeline is 275 ℃, spinning body temperature is 280 ℃, lateral blowing wind speed 0.6 meter per second, 2800 meters/minute of spinning speeds make 277dtex/48f pre-oriented yarn (POY).
Embodiment 6: the cation dyeable polyester melt that embodiment 2 is made, on existing melt directly spinning filament production equipment, the temperature of control melt Conveying pipeline is 280 ℃, spinning body temperature is 285 ℃, lateral blowing wind speed 0.6 meter per second, 3200 meters/minute of spinning speeds make 277dtex/48f pre-oriented yarn (POY).
Embodiment 7: the cation dyeable polyester melt that embodiment 3 is made, on existing melt directly spinning filament production equipment, the temperature of control melt Conveying pipeline is 275 ℃, spinning body temperature is 280 ℃, lateral blowing wind speed 0.5 meter per second, 160 ℃ of heat pipe temperatures, 4000 meters/minute of spinning speeds make 110dtex/48f fully oriented filament (FDY).
Embodiment 8: the cation dyeable polyester melt that embodiment 4 is made, on existing melt directly spinning filament production equipment, the temperature of control melt Conveying pipeline is 280 ℃, spinning body temperature is 285 ℃, lateral blowing wind speed 0.5 meter per second, 170 ℃ of heat pipe temperatures, 4500 meters/minute of spinning speeds make 110dtex/48f fully oriented filament (FDY).
Comparative Examples 1: in production capacity is on the gap polyester equipment criticized of 3500KG/, with the 3000KG p-phthalic acid, 1300L ethylene glycol monomer joins in the slurry still by 1: 1.20 mol ratio, the stabilizing agent triphenyl phosphite that adds 450ml in the making beating still, 1500g polycondensation catalyst antimony glycol, after mixing, above-mentioned slurry continous-stable is delivered in esterification-I reactor, 250.0 ℃ of control esterifications-I temperature, pressure is normal pressure, after treating that the water outlet of esterification water reaches 680L, esterification-I material is sent into esterification-II, 230～240 ℃ of control esterifications-II temperature, interpolation concentration is ethylene isophthalate-5-sodium sulfonate (SIPE) 230L (1.5mol%) of 40.0%, the ether of 250PPM is prevented the agent sodium acetate, 40～50 minutes time of staying of control, deliver to polycondensation workshop section with nitrogen pressure then, polycondensating process makes the cation dyeable polyester section routinely.
Comparative Examples 2: the cation dyeable polyester 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 277dtex/48f pre-oriented yarn (POY).
Comparative Examples 3: the cation dyeable polyester 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 0.5 meter per second, 170 ℃ of heat pipe temperatures, 4500 meters/minute of spinning speeds make 110dtex/48f fully oriented filament (FDY).
The every technical-economic index of the various embodiments described above and Comparative Examples is listed as follows:
Table 1
| Polymerization methods | Esterification-I esterification yield % | Esterification-II temperature ℃ | SIPE mol％ | COOH mol/t | DEG ％ | Inherent viscosity dl/g | Inherent viscosity deviation dl/g | ||
| Embodiment | 1 | Continuity method | 88.0 | 255 | 1.5 | 29.2 | 4.4 | 0.581 | 0.007 |
| 2 | Continuity method | 90.2 | 250 | 2.0 | 27.5 | 3.9 | 0.579 | 0.006 | |
| 3 | Continuity method | 92.1 | 245 | 2.5 | 26.4 | 3.5 | 0.579 | 0.008 | |
| 4 | Continuity method | 90.3 | 250 | 1.5 | 27.0 | 3.6 | 0.580 | 0.005 | |
| Comparative Examples | 1 | The gap method | 230～240 | 1.5 | 45.6 | 3.7 | 0.578 | 0.015 |
Table 2
| The spinning mode | Spinning body temperature ℃ | Spinning speed rice/minute | The spinning operation performance | Fibre strength cn/dtex | Dyeing uniformity | Production cost | |||||
| POY | FDY | POY | FDY | POY | FDY | ||||||
| Embodiment | 5 | Fused mass directly spinning | 280.0 | 2800 | Good | 1.82 | Good | Lower | |||
| 6 | Fused mass directly spinning | 285.0 | 3200 | Good | 1.95 | Good | Lower | ||||
| 7 | Fused mass directly spinning | 280.0 | 4000 | Good | 3.5 | Good | Lower | ||||
| 8 | Fused mass directly spinning | 285.0 | 4500 | Better | 3.4 | Good | Lower | ||||
| Comparative Examples | 2 | Section is spun | 285.0 | 3200 | Generally | 1.83 | Generally | High | |||
| 3 | Section is spun | 285.0 | 4500 | Generally | 3.1 | Generally | High | ||||
Claims (6)
1, a kind of preparation method of continuous condensed direct-spinning cation dye dyeable polyester long filament, with p-phthalic acid and ethylene glycol monomer is raw material, comprise the preparation of continuous condensed cation dyeable polyester melt and the preparation of direct-spinning cation dye dyeable polyester long filament, it is characterized in that being undertaken by following manufacturing procedure:
The preparation of a, polyester fondant: on existing continuous polycondensation equipment, p-phthalic acid and ethylene glycol monomer are joined in the slurry still by 1: 1.18～1: 1.25 mol ratio pull an oar adding conventional catalyst in the slurry still earlier; Then above-mentioned slurry continous-stable is delivered in esterification-I reactor, control esterification yield 88%～92%, again carboxylate is sent into esterification-II reactor, add ethylene isophthalate-5-sodium sulfonate and the anti-agent of ether of p-phthalic acid's molal quantity 1.5-2.5 mole % in esterification-II reactor simultaneously continuously, stabilizing agent, 245～255 ℃ of temperature in control esterification-II reactor, 30～50 minutes time of staying, the carboxylate that mixes is pumped into polycondensation workshop section, polycondensating process makes the cation dyeable polyester melt 260～285 ℃ of temperature under the condition of vacuum 0.1～10KPr routinely;
The preparation of b, polyester filament: with above-mentioned cation dyeable polyester melt, by 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.
2, press the preparation method of the described continuous condensed direct-spinning cation dye dyeable polyester of claim 1 long filament, the preparation that it is characterized in that described The cation-dyeable polyester pre-oriented yarn is on existing melt directly spinning filament production equipment, the temperature of control melt Conveying pipeline is 275～290 ℃, spinning body temperature is 280～290 ℃, lateral blowing wind speed 0.3～0.8 meter per second, 2500～3500 meters/minute of spinning speeds make pre-oriented yarn.
3, press the preparation method of the described continuous condensed direct-spinning cation dye dyeable polyester of claim 1 long filament, the preparation that it is characterized in that described The cation-dyeable polyester fully oriented filament is on existing melt directly spinning filament production equipment, the temperature of control melt Conveying pipeline is 275～290 ℃, spinning body temperature is 280～290 ℃, lateral blowing wind speed 0.3～0.8 meter per second, 140～180 ℃ of heat pipe temperatures, spinning speed 3500～5000m/minute, make fully oriented filament.
4, by the preparation method of the described continuous condensed direct-spinning cation dye dyeable polyester of claim 1 long filament, it is characterized in that described conventional catalyst is antimony glycol or antimonous oxide, its addition is 350～500PPM of polyester fondant total amount.
5, by the preparation method of the described continuous condensed direct-spinning cation dye dyeable polyester of claim 1 long filament, it is characterized in that the anti-agent of described ether is sodium acetate or potassium acetate, its addition is 300～400PPM of polyester fondant total amount.
6, by the preparation method of the described continuous condensed direct-spinning cation dye dyeable polyester of claim 1 long filament, it is characterized in that described stabilizing agent is phosphorous acid or trimethyl phosphate, triphenyl phosphite, its addition is 100～200PPM of polyester fondant total amount.
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| CNB2007100687409A CN100497772C (en) | 2007-05-22 | 2007-05-22 | Method for preparing polyester filament capable being dyed by continuously condensed direct-spinning cation dye |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101781811B (en) * | 2010-03-13 | 2011-12-07 | 浙江东华纤维制造有限公司 | Method for preparing continuous polymerization directly-spun cation-dyeable high-shrinkage polyester staple fibers |
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| US3649571A (en) * | 1970-06-01 | 1972-03-14 | Goodyear Tire & Rubber | Cationically dyeable polyester |
| JP3776024B2 (en) * | 2001-10-15 | 2006-05-17 | 帝人ファイバー株式会社 | Copolyester and cationic dyeable fiber |
| CN1631933A (en) * | 2004-11-30 | 2005-06-29 | 江苏盛虹化纤有限公司 | Process for continuous polycondensation preparation of fibrous polyethylene terephthalate |
| US20090131628A1 (en) * | 2005-03-07 | 2009-05-21 | Kb Seiren, Ltd. | Normal-pressure cation-dyeable polyester, textile product made from the same, and production method for the same |
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