CN102691131A - Manufacturing equipment system of flame-retardant polyester fiber - Google Patents
Manufacturing equipment system of flame-retardant polyester fiber Download PDFInfo
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- CN102691131A CN102691131A CN201210203013XA CN201210203013A CN102691131A CN 102691131 A CN102691131 A CN 102691131A CN 201210203013X A CN201210203013X A CN 201210203013XA CN 201210203013 A CN201210203013 A CN 201210203013A CN 102691131 A CN102691131 A CN 102691131A
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Abstract
The invention provides a manufacturing equipment system of flame-retardant polyester fiber. The system comprises a flame retardant preparation unit, a catalyst and auxiliary mixed solution preparation unit, a slurry preparation unit, a first-stage esterification unit, a second-stage esterification unit, a first pre-polycondensation unit, a second pre-polycondensation unit, a prepolymer conveying and filtering unit, a final polycondensation unit, a final polymer conveying and filtering unit, a spinning melt conveying and distribution unit, a spinning unit and a drafting unit. The manufacturing equipment system of flame-retardant polyester fiber, provided by the invention, is applied to the continuous polymerization direct spinning technology, so that the synthetic fiber has lasting flame retardance, is nontoxic and environment-friendly and has the advantages of high production efficiency, low consumption and loss and low production cost; the synthetic fiber has excellent spinnability and fiber physical properties and excellent polymer flame retardance; the flame retardance of the textile is better and lasting; the limit oxygen index (LOI) is greater than 34; and the synthetic fiber has perfect washing durability and is safe and harmless to human bodies.
Description
Technical field
The present invention relates to a kind of equipment systems of flame-retardant polyester fiber.
Background technology
Because the textiles great majority have inflammable characteristic, more and more become the main hidden danger that causes inside fire, become a serious social concern.
Fire resistance fibre is meant that fiber has the characteristic that slows down, stops or prevent flaming combustion, and flame retardant textiles mainly is to be used for preventing the generation of fire and to protect human body to avoid burn.Spin in clothes, family, gathering around of field such as auto parts machinery, industry and health have broad application prospects and huge development space, the future market has a high potential.
Along with growth in the living standard with to the attention of safety, the progressively foundation of the flame-retardant standard of textiles and rules and perfect has promoted research, the development and application of flame retardant textiles.
Polyester accounts for synthetic fiber output more than 60%, is textile application chemical fibre kind the most widely.Present domestic fire-retardant polyester industry forms scale far away; Its main cause be present flame-retardant polyester fiber production technology and equipment all or rest on intermittently or semi-continuous polymerization production section; " two-step method " poor efficiency of producd fibers, high loss, small-scale production stage are spun in section again; And spinnability bad (section crystallizing and drying difficulty, melt CPF voltage rise are fast, and spinning tear drop, the silk that wafts, broken end are many) is spun in section, has seriously restricted the flame-retardant polyester fiber industrialization process.More external companies also still adopt the intermittence type polymerization Processes and apparatus, and the fire-retardant phase of its synthetic fiber is short and have a mild toxicity.
Summary of the invention
The technical problem that the present invention will solve is to provide a kind of equipment systems of flame-retardant polyester fiber, is used for continuous polymerization melt Direct Spinning technology, makes the fire-retardant lasting and asepsis environment-protecting of its synthetic fiber.
The present invention is achieved in that a kind of equipment systems of flame-retardant polyester fiber, it is characterized in that: comprise that fire retardant preparation unit, catalyst & auxiliary agent mixed solution preparation unit, slurry preparation unit, phase I esterification unit, second stage esterification unit, the first prepolymerization reaction unit, the second prepolymerization reaction unit, prepolymer conveying and filter element, final minification gather reaction member, whole polymers conveying and filter element, spinning melt conveying and allocation units, spinning unit and drafting unit; Said slurry preparation unit, phase I esterification unit, second stage esterification unit, the first prepolymerization reaction unit, the second prepolymerization reaction unit, prepolymer conveying and filter element, final minification gather reaction member, whole polymers conveying and filter element, spinning melt conveying and allocation units, spinning unit and drafting unit and are connected successively; Said fire retardant preparation unit is a second stage esterification unit continuous feeding; Said catalyst & auxiliary agent mixed solution preparation unit is a slurry preparation unit continuous feeding.
Further, said fire retardant is prepared making beating jar, screw pump, esterifying kettle, still, first cooler, the lime set feeder that the unit comprises connection successively; Said esterifying kettle also connects second cooler, first filter, first feeder channel and first charging pump successively; Preparing tank, second filter, second feeder channel and second charging pump that connects successively drawn together in said catalyst & auxiliary agent mixed solution preparation unit; Said slurry preparation unit comprises PTA continuous feeding device, weighing apparatus, slurry preparation groove and the slurry screw pump that connects successively; Said phase I esterification unit comprises first esterifier and first wastewater treatment equipment that connects successively; Said second stage esterification unit bag connects successively draws together second esterifier and second wastewater treatment equipment; The said first prepolymerization reaction unit comprises first Prepolycondensating reactor, first gas phase thing treating apparatus and the liquid-ring vacuum pump that connects successively; The said second prepolymerization reaction unit comprises second Prepolycondensating reactor, the second gas phase thing treating apparatus, ethylene glycol steam jet pump and the liquid rotary pump that connects successively; Said prepolymer is carried and filter element comprises pre-polymer melt discharging pump, the pre-polymer melt filter that connects successively; Said final minification gathers reaction member and comprises successively the final polycondensation reactor that connects and the 3rd gas phase thing treating apparatus, said ethylene glycol steam jet pump; Said whole polymers is carried and is comprised whole polymers melt discharging pump and the fondant filter that is connected successively with filter element; Said spinning melt is carried and allocation units comprise booster pump, melt cooler, first static mixer, distributing valve and second static mixer that connects successively through the spinning threadling melt pipe; Said spinning unit comprises a plurality of spinning manifolds; Each spinning manifold connects a up-coiler, and is provided with filament spinning component in the spinning manifold, and these a plurality of up-coilers are through a hauling machine and a feeding-wheel; The below of feeding-wheel is provided with a barrel machine, and barrel machine that falls is provided with fiber barrel; Said drafting unit comprises wire feeder, soaker, preheating machine, first drawing machine, water-bath drawing-off groove, second drawing machine, Steam Heating case, tension-setting machine, oil spout cooler, the 4th elongator, the folded silk of a tow warp machine, steam preheating case, crimping machine, shop silk machine, drying machine, cutting machine and the baling press that connects successively; Wherein, said slurry preparation groove, slurry screw pump, first esterifier, second esterifier, first Prepolycondensating reactor, second Prepolycondensating reactor, pre-polymer melt discharging pump, pre-polymer melt filter, final polycondensation reactor, whole polymers melt discharging pump and fondant filter connect successively; First charging pump of said fire retardant preparation unit connects said second esterifier; Second charging pump of said catalyst & auxiliary agent mixed solution preparation unit connects said slurry preparation groove.
Further, said first wastewater treatment equipment comprises process tower, the overhead condenser that connects successively; The bottom of said process tower also connects a delivery pump, and this delivery pump also connects first esterifier and second esterifier; Said second wastewater treatment equipment is said first wastewater treatment equipment; The said first gas phase thing treating apparatus comprises the first scraper plate condenser, first liquid seal trough, the first glycol circulation pump and the first glycol-cooled device that is connected in successively between said first Prepolycondensating reactor and the liquid-ring vacuum pump; The said second gas phase thing treating apparatus comprises the second scraper plate condenser, second liquid seal trough, the second glycol circulation pump and the second glycol-cooled device that is connected in successively between said second Prepolycondensating reactor and the said ethylene glycol steam jet pump; Said the 3rd gas phase thing treating apparatus comprises the second scraper plate condenser, second liquid seal trough, the second glycol circulation pump and the second glycol-cooled device that is connected in successively between said final polycondensation reactor and the said glycol steam jet pump of second; Wherein, said overhead condenser, liquid-ring vacuum pump, liquid rotary pump all connect a waste water stripping system.
Wherein, said first esterifier and second esterifier are the esterifier that vertical band stirs, and the second esterifier inside is provided with inner sleeve.
Wherein, said pre-polymer melt filter be can online switching twin pre-polymer melt filter; The gear pump that said pre-polymer melt discharging pump is two jacketed moves simultaneously, adopts frequency control.
Wherein, Said final polycondensation reactor is horizontal band combination collar plate shape reactor; The employing twin shaft drives; Frequency control, and final polycondensation reactor inlet side and outlet side respectively be provided with a radioactivity level-sensing device all is provided with temperature-detecting device at inlet side, cylindrical shell middle part and the outlet side of final polycondensation reactor.
Wherein, said whole polymers melt discharging pump is the gear pump that two jacketed are also moved simultaneously, and this gear pump adopts frequency control; Said fondant filter is duplex and fondant filter that can online switching, i.e. two filter chamber the using and the reserved.
Wherein, said whole polymers is carried and also is connected a pelletizing system with the fondant filter of filter element.
Wherein, the PTA continuous feeding device of said slurry preparation unit further comprise one feed intake cucurbit, deliver to feed hopper, pipe carrier bar induction system and feed storehouse, said weighing apparatus is connected the exit of bottom, feed storehouse.
The present invention has following advantage: adopt fire retardant preparation unit, be used to prepare BACN CEPPA-EG esterifying liquid, make the heat resistance of preparation people fire retardant better; The science that is set to form more of each component units, continuous polymerization melt Direct Spinning " one-step method " fibre manufacturing technique provides the basis efficiently; Compare current intermittence of generally adopting or semi-continuous polymerization production section; " two-step method " technology of producd fibers is spun in section again, has following significant beneficial effect:
1, production efficiency is high, and consumption and loss are all low, and production cost is low;
2, good spinnability and fiber physical property;
3, have the fire resistance of good polymer own, the fabrics flame resistance performance is excellent durable more, limited oxygen index LOI>34;
4, the washing resistance of brilliance;
5, safe and harmless to human body.
Description of drawings
Combine embodiment that the present invention is further described with reference to the accompanying drawings.
Fig. 1 is that each unit of the present invention is greatly to structure connection sketch map.
Fig. 2 is fire retardant preparation unit connection structure sketch map of the present invention.
Fig. 3 is catalyst & auxiliary agent mixed solution preparation unit connection structure sketch map of the present invention.
Fig. 4 carries and filter element syndeton sketch map for slurry preparation of the present invention unit to whole polymers.
Fig. 5 carries and allocation units syndeton sketch map for spinning melt of the present invention.
Fig. 6 is the syndeton sketch map of spinning of the present invention unit and drafting unit.
The specific embodiment
See also Fig. 1 to shown in Figure 6; The equipment systems of flame-retardant polyester fiber of the present invention comprises fire retardant preparation unit 1, catalyst & auxiliary agent mixed solution preparation unit 2, slurry preparation unit 3, phase I esterification unit 4, second stage esterification unit 5, the first prepolymerization reaction unit 6, the second prepolymerization reaction unit 7, prepolymer carries and filter element 8, final minification gather reaction member 9, whole polymers carries and filter element 10, spinning melt are carried and allocation units 11, spinning unit 12 and drafting unit 13; Said slurry preparation unit 3, phase I esterification unit 4, second stage esterification unit 5, the first prepolymerization reaction unit 6, the second prepolymerization reaction unit 7, prepolymer carries and filter element 8, final minification gather reaction member 9, whole polymers carries, and and filter element 10, spinning melt carry and allocation units 11, spinning unit 12 and drafting unit 13 are connected successively; Said fire retardant preparation unit 1 is second stage esterification unit 5 continuous feedings; Said catalyst & auxiliary agent mixed solution preparation unit 2 is slurry preparation unit 3 continuous feedings.
Further, said fire retardant preparation unit 1 comprises the making beating jar 11 that connects successively, screw pump 12, esterifying kettle 13, still 141, first cooler 142, lime set feeder 143; Said esterifying kettle 13 also connects second cooler 15, first filter 16, first feeder channel 17 and first charging pump 18 successively.Also can connect a medial launder 19 between said second cooler 15 and first filter 16.
The preparing tank that connects successively 21, second filter 22, second feeder channel 23 and second charging pump 24 are drawn together in said catalyst & auxiliary agent mixed solution preparation unit 2;
As shown in Figure 4, said slurry preparation unit 3 comprises PTA continuous feeding device 31, weighing apparatus 32, slurry preparation groove 33 and the slurry screw pump 34 that connects successively; Said PTA continuous feeding device 31 further comprise one feed intake cucurbit 311, deliver to feed hopper 312, pipe carrier bar induction system 313 and feed storehouse 314, said weighing apparatus 32 is connected the exit of 314 bottoms, feed storehouse.
Said phase I esterification unit 4 comprises first esterifier 41 and first wastewater treatment equipment 42 that connects successively; Said first wastewater treatment equipment 42 comprises process tower 421, the overhead condenser 422 that connects successively; The bottom of said process tower 421 also connects a delivery pump 423, and this delivery pump 423 also connects first esterifier 41 and second esterifier 51.
Said second stage esterification unit 5 bag connects successively draws together second esterifier 51 and second wastewater treatment equipment 52; Said second wastewater treatment equipment 52 is said first wastewater treatment equipment 41.
The said first prepolymerization reaction unit 6 comprises successively first Prepolycondensating reactor 61, first gas phase thing treating apparatus 62 and the liquid-ring vacuum pump 63 that connects; The said first gas phase thing treating apparatus 62 comprises the first scraper plate condenser 621 that is connected in successively between said first Prepolycondensating reactor 61 and the liquid-ring vacuum pump 63, first liquid seal trough 622, the first glycol circulation pump 623 and the first glycol-cooled device 623.
The said second prepolymerization reaction unit 7 comprises successively second Prepolycondensating reactor 71 that connects, the second gas phase thing treating apparatus 72, ethylene glycol steam jet pump 73 and liquid rotary pump 74; The said second gas phase thing treating apparatus 72 comprises the second scraper plate condenser 721 that is connected in successively between said second Prepolycondensating reactor 71 and the said ethylene glycol steam jet pump 73, second liquid seal trough 722, the second glycol circulation pump 723 and the second glycol-cooled device 724.
Said prepolymer is carried and filter element 8 comprises pre-polymer melt discharging pump 81, the pre-polymer melt filter 82 that connects successively.
Said final minification gathers reaction member 9 and comprises successively the 91 and the 3rd gas phase thing treating apparatus 92 that connects, said ethylene glycol steam jet pump 93; Said the 3rd gas phase thing treating apparatus 93 comprises the second scraper plate condenser 921 that is connected in successively between said final polycondensation reactor 91 and the said glycol steam jet pump 73 of second, second liquid seal trough 922, the second glycol circulation pump 923 and the second glycol-cooled device 924.
Wherein, said overhead condenser 422, liquid-ring vacuum pump 63, liquid rotary pump 74 all connect a waste water stripping system 200.
Said whole polymers is carried with filter element 10 and is comprised the whole polymers melt discharging pump 101 and fondant filter 102 that is connected successively;
Said spinning melt is carried and allocation units 11 comprise the booster pump 112 that connects successively through spinning threadling melt pipe 111, melt cooler 113, first static mixer 114, distributing valve 115, the second static mixers 116;
As shown in Figure 5; Said spinning unit 12 comprises a plurality of spinning manifolds 121; Each spinning manifold 121 connects a up-coiler 122, and is provided with filament spinning component in the spinning manifold 121, and these a plurality of up-coilers 122 are through a hauling machine 123 and a feeding-wheel 124; The below of feeding-wheel is provided with barrel machine 125, and barrel machine 125 that falls is provided with fiber barrel 126;
As shown in Figure 6, said drafting unit 13 comprises that successively the wire feeder 131 that connects, soaker 132, preheating machine, first drawing machine 133, water-bath drawing-off groove 134, second drawing machine 135, Steam Heating case 136, tension-setting machine 137, oil spout cooler 138, the 4th elongator 139, tow are through a folded silk machine 140, steam preheating case 141, crimping machine 142, a shop silk machine 143, drying machine 144, cutting machine 145 and baling press 146;
Said slurry preparation groove 33, slurry screw pump 34, first esterifier 41, second esterifier 51, first Prepolycondensating reactor 61, second Prepolycondensating reactor 71, pre-polymer melt discharging pump 81, pre-polymer melt filter 82, final polycondensation reactor 91, whole polymers melt discharging pump 101 and fondant filter 102 connect successively, and fondant filter 102 connects downstream again and directly spins the short fiber device; First charging pump 18 of said fire retardant preparation unit 1 connects said second esterifier 51; Second charging pump 24 of said catalyst & auxiliary agent mixed solution preparation unit 2 connects said slurry preparation groove 33.
Said first esterifier 41 and second esterifier 51 are the esterifier that vertical band stirs, and second esterifier, 51 inside are provided with inner sleeve.
Said pre-polymer melt filter 82 be can online switching twin pre-polymer melt filter; The gear pump that said pre-polymer melt discharging pump 81 is two jacketed moves simultaneously, adopts frequency control.
Said final polycondensation reactor 91 is horizontal band combination collar plate shape reactor; The employing twin shaft drives; Frequency control; And final polycondensation reactor 91 inlet sides and outlet side respectively are provided with a radioactivity level-sensing device, all are provided with temperature-detecting device at the inlet side of final polycondensation reactor 91, cylindrical shell middle part and outlet side.
Said whole polymers melt discharging pump 101 is the gear pump that two jacketed are also moved simultaneously, and this gear pump adopts frequency control; Said fondant filter 102 is duplex and fondant filter that can online switching, i.e. two filter chamber the using and the reserved.
Said whole polymers is carried and also is connected a pelletizing system 300 with the fondant filter 102 of filter element 10.
Below the operation principle of explanation device systems of the present invention is promptly explained the technology of utilizing the present device system to make flame-retardant polyester fiber, comprises the steps:
CEPPA+EG
90kPa, 175 ℃, 60min
CEPPA-EG esterifying liquid+H
2O ↑.
Wherein fire retardant is prepared main technologic parameters:
| EG(L) | CEPPA(kg) | Reaction temperature (° C) | Reaction pressure (kPa) | Reaction time (min) |
| 6500 | 5000 | 175 | 90 | 60 |
Because pure fire retardant CEPPA heat decomposition temperature is lower, adopt the test of thermal weight loss detection method to disclose, pure CEPPA begins to decompose about 188 ℃, has decomposed 50% about 267 ℃.And the reaction temperature of flame retardant polyester is higher than the heat decomposition temperature of pure CEPPA between 260 ~ 280 ℃, so the present invention adopts CEPPA and polyester raw material EG to carry out esterification earlier, synthetic heat resistance is the CEPPA-EG esterifying liquid preferably.Adopt the test of thermal weight loss detection method to disclose, the CEPPA-EG esterifying liquid begins to decompose about 263 ℃, decomposes about 380 ℃ to reach 50%.CEPPA-EG esterification fluid power effectively suppresses the thermal decomposition of fire retardant.
The water that produces during said synthetic CEPPA-EG esterifying liquid is collected through still 141 fractionation, first cooler, 142 lime set feeders 143; Judge reaction end through the collected water yield; Esterifying kettle 13 filled nitrogen pressurization discharging after reaction was accomplished; The CEPPA-EG esterifying liquid that makes is put into medial launder through 15 coolings of second cooler; Sample analysis is qualified puts into feeder channel 17 after filter 16 filters, be added in proportion continuously in said second esterifier, 51 inner rooms by first charging pump 18 and (see step 3).Wherein, also can connect a medial launder 19 between second cooler 15 and the filter 16.
Step 2, catalyst & auxiliary agent mixed solution are prepared: as shown in Figure 3; A batch allotment operation is adopted in the allotment of catalyst & auxiliary agent mixed solution; In preparing tank 21, add the ethylene glycol EG that measured earlier; Under stirring, drop into load weighted antimony acetate SbAC3, trimethyl phosphate TMP, anti-oxidant 2215 respectively; At 165 ℃ of following stirring and dissolving 3HR of design temperature, sample analysis is qualified puts into after second filter 22 filters that qualified seasoning liquid is added in the preparing tank 21 with special ratios with second charging pump 24 continuously in second feeder channel, 23, the second feeder channels 23.This catalyst & auxiliary agent mixed solution allotment main technologic parameters is:
| EG(L) | SbAC3(kg) | TMP（kg） | 2215（kg） | SbAC3 concentration (%wt.) | TMP concentration (%wt.) | 2215 concentration (%wt.) | Thermostat temperature (° C) | Constant temperature time (h) |
| 6265 | 150 | 35 | 375 | 2.0% | 0.47% | 5.0% | 165 | 3 |
| PTA(kg/h) | EG(L/h) | Catalyst & auxiliary agent mixed solution (L/h) | TiO2 slurries 20%wt. (L/h) |
| 10128 | 2955 | 320 | 545 |
| Temperature ℃ | Pressure kg/cm2 | Liquid level % | Esterification time hr | The quantity of reflux kg/h of ethylene glycol |
| 260~265 | 0.6~0.7 | 50~55 | 5.3 | 1900~2100 |
Step 5, second stage esterification: slurry is accomplished the phase I esterification in first esterifier 41 after, flow into certainly and continue the second stage esterification in second esterifier 51.Wherein, higher from the temperature of charge that first esterification is come, continue reaction the mistress, overflow is advanced behind the inner room and is lowered the temperature because of the CEPPA-EG esterifying liquid that adds.Second esterifier is the esterifier that vertical band stirs; And the second esterifier inside is provided with inner sleeve; Be separated into inner room and mistress to reactor; The mistress that material is introduced into reactor reacts, and the overflow inner room that gets into reactor further reacts then, at last from the tube end discharging of inner room.So just be equivalent to the series connection of two vertical reactors, make material reach the state that is similar to laminar flow, make discharging more even in the complete mixing flow process.The quantity of reflux of temperature, pressure, liquid level and ethylene glycol through regulating esterification; The control esterification yield reaches 98%; Simultaneously; Reactor inner room at second esterifier 51 adds fire retardant CEPPA-EG esterifying liquid, and the monomers B HET that generates with esterification fully mixes, and the preliminary polymerization reaction generation degree of polymerization is at 2 ~ 5 oligomer; The fire retardant preparation is that the EG (ethylene glycol) that purchases one of next CEPPA powder and polyester main material is processed better CEPPA-EG esterifying liquid (saying in essence that from technology the CEPPA-EG esterifying liquid is exactly the polyester modification monomer) of heat resistance, stability through esterification.Planning adds from second esterification on the technology; Be to let it and PTA-EG carboxylate BHET (polyester monocase, polycondensation monomer, ethylene glycol terephthalate) fully mix earlier; " be total to (contracting) and gather reaction " again in polycondensation reaction stage and BHET then, make that modified monomer CEPPA-EG can " evenly chain is gone into " polyester macromolecule.The second esterification system main technologic parameters:
| CEPPA-EG esterifying liquid addition (L/h) | Temperature ℃ | Pressure kg/cm2 | Liquid level % | Esterification time hr | The quantity of reflux kg/h of ethylene glycol |
| 1160 | 240~245 | |
40~45 | 1.8 | 380~420 |
；
In addition; Water that phase I esterification and second stage esterification generate and ethylene glycol evaporation back get into process tower 421 and carry out rectifying separation; Heavy ends ethylene glycol wherein is from the discharging of tower still, adopts delivery pump 423 to send back in first esterifier 41, second esterifier 51; Light component water send waste water stripping system 200 to carry out stripping through the 422 condensation extraction of air-cooled type overhead condenser and handles; And ethylene glycol content is less than 0.5% in the control process tower 421 overhead condensation liquid, and the ethylene glycol water content is less than 1.5% in the tower still.
Moreover, be the molten condition that guarantees reaction mass, the continuation that the CEPPA-EG esterifying liquid fully mixes and keep reaction, can control the interior room temperature of second esterifier is 240 ℃.
| Temperature ℃ | Vacuum mbar | Liquid level % | Time of staying hr | Esterification yield % | Degree of polymerization Pn |
| 268~270 | 90~110 | 30~35 | 1.43 | 98 | 20 |
The first scraper plate condenser 621 is set between first Prepolycondensating reactor 61 and the liquid-ring vacuum pump 62; The gas phase thing that reaction generates gets into the said first scraper plate condenser 621; With reverse contact of ethylene glycol of spray, capture the entrainment in the gas phase, form the ethylene glycol lime set and be collected in first liquid seal trough 622; Adopt the first glycol circulation pump 623 to carry again, after the first glycol-cooled device 624 adopts the recirculated cooling water cooling to reduce temperature, recycle; Said ethylene glycol lime set main component is the accessory substance of ethylene glycol, water, oligomer and reacted; Wherein water content is higher from the gas phase that first Prepolycondensating reactor 61 is drawn out of, its lime set need be sent to process tower separate after reuse again.
| Temperature ℃ | Vacuum mbar | Liquid level % | Time of staying hr | Esterification yield % | Degree of polymerization Pn |
| 275~280 | 23~27 | 35~36 | 1.40 | 99.5 | 80 |
；
The second scraper plate condenser 721 is set between second Prepolycondensating reactor 71 and the liquid rotary pump 73; The gas phase thing that reaction generates gets into the said second scraper plate condenser 721; With reverse contact of ethylene glycol of spray, capture the entrainment in the gas phase, form the ethylene glycol lime set and be collected in second liquid seal trough 722; Adopt the second glycol circulation pump 723 to carry again, after the second glycol-cooled device 724 adopts the recirculated cooling water cooling to reduce temperature, recycle; Said ethylene glycol lime set main component is the accessory substance of ethylene glycol, water, oligomer and reacted.
| Temperature ℃ | Vacuum mbar | Liquid level % | Time of staying hr | The online detection of inherent viscosity η |
| 280~282 | 1.5~3 | 32~35 | 3.40 | 0.715±0.005 |
；
The 3rd scraper plate condenser 921 is set between final polycondensation reactor 91 and the ethylene glycol steam jet pump 72; The gas phase thing that reaction generates gets into said the 3rd scraper plate condenser 921; With reverse contact of ethylene glycol of spray, capture the entrainment in the gas phase, form the ethylene glycol lime set and be collected in the 3rd liquid seal trough 922; Adopt triethylene glycol circulating pump 923 to carry again, after triethylene glycol cooler 924 adopts the recirculated cooling water cooling to reduce temperature, recycle; Said ethylene glycol lime set main component is the accessory substance of ethylene glycol, water, oligomer and reacted.
Fire-retardant polyester melt main quality index wherein:
| Inherent viscosity (dl/g) | Fusing point (℃) | Content of carboxyl end group (mol/t) | The B value | The L value | DEG(%) | TiO2 content (%) | P content (ppm) |
| 0.710±0.005 | 240~245 | 25~30 | ≤7 | ≥70 | 2.50±0.05 | 1.20±0.05 | ≥6500 |
；
| Pipe temperature (℃) | Heating agent outlet pressure kg/cm 2 | Press kg/cm behind the booster pump 2 |
| 275~280 | 2.5 | 100 |
；
| Spinning speed m/min | Spinning body temperature (℃) | The quenching wind-warm syndrome (℃) | Quenching wind speed m/s | Oil concentration % |
| 1300~1400 | 280~285 | 18~20 | 2.8~3.0 | 0.30~0.40 |
；
Step 13, drawing-off: as shown in Figure 5; Tow is drawn from fiber barrel 125, boundling, oil, preheating; Tow afterwards gets into first drawing machine 133, water-bath drawing-off groove 134, second drawing machine 135; And in water bath 134, accomplish drawing-off for the first time, tow gets into tension-setting machine 137 after 136 preheatings of Steam Heating case then, between second drawing machine 135 and tension-setting machine 137; In Steam Heating case 136, accomplish drawing-off for the second time, and in tension-setting machine 137, accomplish HEAT SETTING; The tow that comes out from tension-setting machine 137 cools off through oil spout; Qualitative cooled tow is through folded silk machine; Through tension adjustment machine, Tension Control roller, behind the adjustment tension force and after the preheating of steam preheating case, send into crimping machine 142 and curl, the tow after curling is layered on the drying machine 144 after the atomizer spraying oils through shop silk machine 143 equably; Through drying machine 144 dry with laxation shaping after tow feed cutting machine 145 through silk guide frame, tension regulator adjustment of tonicity after evenly; Tow after the cut-out falls in baling press 146 casings by gravity, behind weighing, is pressed into fibre bag, through putting in storage after the assay was approved.Drafting process main technologic parameters wherein:
| Speed of a motor vehicle M/MIN | Ratio of elongation | The dense % of oil | Finish discharge rate L/H | The crimping machine master presses kg/cm 2 | Crimping machine back pressure kg/cm 2 |
| 255~275 | 3.060*1.115 | 2.40 | 300~320 | 5.0 | 2.0 |
Fire-retardant polyester short fiber main quality index through equipment of the present invention and above-mentioned preparation process gained is:
| Fiber number dtex | Intensity cN/dtex | Degree of stretching % | Fault mg/100g | Crispation number No./2.5cm | Xeothermic % | Compare resistance |
| 1.56 | 4.50 | 40.0 | 25.0 | 10.8 | 11.0 | 2.5* 10 6 |
We are according to " GB/T 5454-1997 textile combustion performance test oxygen index method "; Select the automatic limiting oxygen index determination appearance of LFY-605 for use; The limited oxygen index that carries out conventional polyester fiber and fabric and flame-retardant polyester fiber and fabric detects; Record conventional polyester fiber LOI=22.45, its fabric LOI=24.26; According to the flame-retardant polyester fiber LOI=32.56 that present device system and above-mentioned technology make, its fabric LOI=34.53.
Limited oxygen index (LOI) is meant that under defined terms material carries out the required minimum oxygen concentration of flaming combustion in oxygen-nitrogen mixture stream.Numerical value with the shared percentage by volume of oxygen is represented, is a kind of method for expressing of evaluating material relative combustion property, the complexity of burning when judging that with this material contacts with flame in air.It is generally acknowledged LOI<27 genus combustible material, 27≤LOI<32 genus combustible material, the genus nonflammable material of LOI>=32.
Though more than described the specific embodiment of the present invention; But the technical staff who is familiar with the present technique field is to be understood that; We described concrete embodiment is illustrative; Rather than being used for qualification to scope of the present invention, those of ordinary skill in the art are in the modification and the variation of the equivalence of doing according to spirit of the present invention, all should be encompassed in the scope that claim of the present invention protects.
Claims (9)
1. the equipment systems of a flame-retardant polyester fiber is characterized in that: comprise that fire retardant preparation unit, catalyst auxiliary agent mixed solution preparation unit, slurry preparation unit, phase I esterification unit, second stage esterification unit, the first prepolymerization reaction unit, the second prepolymerization reaction unit, prepolymer conveying and filter element, final minification gather reaction member, whole polymers conveying and filter element, spinning melt conveying and allocation units, spinning unit and drafting unit;
Said slurry preparation unit, phase I esterification unit, second stage esterification unit, the first prepolymerization reaction unit, the second prepolymerization reaction unit, prepolymer conveying and filter element, final minification gather reaction member, whole polymers conveying and filter element, spinning melt conveying and allocation units, spinning unit and drafting unit and are connected successively;
Said fire retardant preparation unit is a second stage esterification unit continuous feeding; Said catalyst & auxiliary agent mixed solution preparation unit is a slurry preparation unit continuous feeding.
2. the equipment systems of flame-retardant polyester fiber as claimed in claim 1 is characterized in that:
Said fire retardant preparation unit comprises making beating jar, screw pump, esterifying kettle, still, first cooler, the lime set feeder that connects successively; Said esterifying kettle also connects second cooler, first filter, first feeder channel and first charging pump successively;
Preparing tank, second filter, second feeder channel and second charging pump that connects successively drawn together in said catalyst & auxiliary agent mixed solution preparation unit;
Said slurry preparation unit comprises PTA continuous feeding device, weighing apparatus, slurry preparation groove and the slurry screw pump that connects successively;
Said phase I esterification unit comprises first esterifier and first wastewater treatment equipment that connects successively;
Said second stage esterification unit bag connects successively draws together second esterifier and second wastewater treatment equipment;
The said first prepolymerization reaction unit comprises first Prepolycondensating reactor, first gas phase thing treating apparatus and the liquid-ring vacuum pump that connects successively;
The said second prepolymerization reaction unit comprises second Prepolycondensating reactor, the second gas phase thing treating apparatus, ethylene glycol steam jet pump and the liquid rotary pump that connects successively;
Said prepolymer is carried and filter element comprises pre-polymer melt discharging pump, the pre-polymer melt filter that connects successively;
Said final minification gathers reaction member and comprises successively the final polycondensation reactor that connects and the 3rd gas phase thing treating apparatus, said ethylene glycol steam jet pump;
Said whole polymers is carried and is comprised whole polymers melt discharging pump and the fondant filter that is connected successively with filter element;
Said spinning melt is carried and allocation units comprise booster pump, melt cooler, first static mixer, distributing valve and second static mixer that connects successively through the spinning threadling melt pipe;
Said spinning unit comprises a plurality of spinning manifolds; Each spinning manifold connects a up-coiler, and is provided with filament spinning component in the spinning manifold, and these a plurality of up-coilers are through a hauling machine and a feeding-wheel; The below of feeding-wheel is provided with a barrel machine, and barrel machine that falls is provided with fiber barrel;
Said drafting unit comprises wire feeder, soaker, preheating machine, first drawing machine, water-bath drawing-off groove, second drawing machine, Steam Heating case, tension-setting machine, oil spout cooler, the 4th elongator, the folded silk of a tow warp machine, steam preheating case, crimping machine, shop silk machine, drying machine, cutting machine and the baling press that connects successively;
Wherein, said slurry preparation groove, slurry screw pump, first esterifier, second esterifier, first Prepolycondensating reactor, second Prepolycondensating reactor, pre-polymer melt discharging pump, pre-polymer melt filter, final polycondensation reactor, whole polymers melt discharging pump and fondant filter connect successively;
First charging pump of said fire retardant preparation unit connects said second esterifier; Second charging pump of said catalyst & auxiliary agent mixed solution preparation unit connects said slurry preparation groove.
3. the equipment systems of flame-retardant polyester fiber as claimed in claim 2 is characterized in that:
Said first wastewater treatment equipment comprises process tower, the overhead condenser that connects successively; The bottom of said process tower also connects a delivery pump, and this delivery pump also connects first esterifier and second esterifier;
Said second wastewater treatment equipment is said first wastewater treatment equipment;
The said first gas phase thing treating apparatus comprises the first scraper plate condenser, first liquid seal trough, the first glycol circulation pump and the first glycol-cooled device that is connected in successively between said first Prepolycondensating reactor and the liquid-ring vacuum pump;
The said second gas phase thing treating apparatus comprises the second scraper plate condenser, second liquid seal trough, the second glycol circulation pump and the second glycol-cooled device that is connected in successively between said second Prepolycondensating reactor and the said ethylene glycol steam jet pump;
Said the 3rd gas phase thing treating apparatus comprise be connected in successively said end second Prepolycondensating reactor and the said glycol steam jet pump of second between the second scraper plate condenser, second liquid seal trough, the second glycol circulation pump and the second glycol-cooled device;
Wherein, said overhead condenser, liquid-ring vacuum pump, liquid rotary pump all connect a waste water stripping system.
4. the equipment systems of flame-retardant polyester fiber as claimed in claim 1 is characterized in that: said first esterifier and second esterifier are the esterifier that vertical band stirs, and the second esterifier inside is provided with inner sleeve.
5. the equipment systems of flame-retardant polyester fiber as claimed in claim 2 is characterized in that: said pre-polymer melt filter is twin pre-polymer melt filter that can online switching; The gear pump that said pre-polymer melt discharging pump is two jacketed moves simultaneously, adopts frequency control.
6. the equipment systems of flame-retardant polyester fiber as claimed in claim 2; It is characterized in that: said final polycondensation reactor is horizontal band combination collar plate shape reactor; The employing twin shaft drives; Frequency control, and final polycondensation reactor inlet side and outlet side respectively be provided with a radioactivity level-sensing device all is provided with temperature-detecting device at inlet side, cylindrical shell middle part and the outlet side of final polycondensation reactor.
7. the equipment systems of flame-retardant polyester fiber as claimed in claim 2 is characterized in that: said whole polymers melt discharging pump is two jacketed and the gear pump of operation simultaneously, and this gear pump adopts frequency control; Said fondant filter is duplex and fondant filter that can online switching, i.e. two filter chamber the using and the reserved.
8. the equipment systems of flame-retardant polyester fiber as claimed in claim 2 is characterized in that: said whole polymers is carried and also is connected a pelletizing system with the fondant filter of filter element.
9. the equipment systems of flame-retardant polyester fiber as claimed in claim 2; It is characterized in that: the PTA continuous feeding device of said slurry preparation unit further comprise one feed intake cucurbit, deliver to feed hopper, pipe carrier bar induction system and feed storehouse, said weighing apparatus is connected the exit of bottom, feed storehouse.
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| CN201210203013XA CN102691131A (en) | 2012-06-19 | 2012-06-19 | Manufacturing equipment system of flame-retardant polyester fiber |
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| CN201210203013XA CN102691131A (en) | 2012-06-19 | 2012-06-19 | Manufacturing equipment system of flame-retardant polyester fiber |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103290507A (en) * | 2013-05-07 | 2013-09-11 | 桐乡市中辰化纤有限公司 | Preparation method of polymerized micro-amount modified super bright polyester fibers |
| CN104262598A (en) * | 2014-10-14 | 2015-01-07 | 浙江万凯新材料有限公司 | Online polyester production conversion equipment and production conversion method adopting same |
| CN104403091A (en) * | 2014-11-18 | 2015-03-11 | 浙江古纤道新材料股份有限公司 | Polyester production equipment and technology |
| CN110724253A (en) * | 2019-11-14 | 2020-01-24 | 扬州普立特科技发展有限公司 | Full-continuous PBAT production equipment and process flow |
| CN110790907A (en) * | 2019-11-18 | 2020-02-14 | 扬州普立特科技发展有限公司 | Production equipment and process flow of full-continuous PETG |
| CN110818888A (en) * | 2019-12-17 | 2020-02-21 | 扬州普立特科技发展有限公司 | Production equipment and process flow of fully-continuous PBS (Poly Butylene succinate) |
| CN110835407A (en) * | 2018-08-16 | 2020-02-25 | 远东新世纪股份有限公司 | Polyester polyol, method for producing same, and polyurethane foam material |
| CN111850721A (en) * | 2020-08-11 | 2020-10-30 | 江苏华西村股份有限公司 | Special short fiber production line for high-cleanness spunlace non-woven fabric |
| CN111910265A (en) * | 2020-07-17 | 2020-11-10 | 湖南工程学院 | Electrostatic spinning injection device with liquid preparation function |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5515422A (en) * | 1978-07-18 | 1980-02-02 | Nippon Ester Co Ltd | Continuous esterification of terephthalic acid |
| CN1085685C (en) * | 1995-12-14 | 2002-05-29 | 纳幕尔杜邦公司 | Process of making polyester prepolymer |
| CN2592645Y (en) * | 2002-12-17 | 2003-12-17 | 中国石化仪征化纤股份有限公司 | Apparatus for continuous production from crude terephthalic acid to polythylene glycol terephthalate |
| US20040024241A1 (en) * | 2000-12-18 | 2004-02-05 | Friedrich-Georg Martin | Method for producing higher (meth)acrylic acid esters |
| CN101186689A (en) * | 2006-11-22 | 2008-05-28 | 株式会社晓星 | Manufacturing method of flame retardant polyester polymer, polyester polymer and fiber therefrom |
| US20090240007A1 (en) * | 2004-11-04 | 2009-09-24 | Fritz Wilhelm | Method of producing polyesters |
| CN201809482U (en) * | 2010-08-16 | 2011-04-27 | 扬州普立特科技发展有限公司 | Device for producing fusant with regenerated polyester |
| CN202626370U (en) * | 2012-06-19 | 2012-12-26 | 福建经纬新纤科技实业有限公司 | Manufacture equipment system for fire-resistant polyester fiber |
-
2012
- 2012-06-19 CN CN201210203013XA patent/CN102691131A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5515422A (en) * | 1978-07-18 | 1980-02-02 | Nippon Ester Co Ltd | Continuous esterification of terephthalic acid |
| CN1085685C (en) * | 1995-12-14 | 2002-05-29 | 纳幕尔杜邦公司 | Process of making polyester prepolymer |
| US20040024241A1 (en) * | 2000-12-18 | 2004-02-05 | Friedrich-Georg Martin | Method for producing higher (meth)acrylic acid esters |
| CN2592645Y (en) * | 2002-12-17 | 2003-12-17 | 中国石化仪征化纤股份有限公司 | Apparatus for continuous production from crude terephthalic acid to polythylene glycol terephthalate |
| US20090240007A1 (en) * | 2004-11-04 | 2009-09-24 | Fritz Wilhelm | Method of producing polyesters |
| CN101186689A (en) * | 2006-11-22 | 2008-05-28 | 株式会社晓星 | Manufacturing method of flame retardant polyester polymer, polyester polymer and fiber therefrom |
| CN201809482U (en) * | 2010-08-16 | 2011-04-27 | 扬州普立特科技发展有限公司 | Device for producing fusant with regenerated polyester |
| CN202626370U (en) * | 2012-06-19 | 2012-12-26 | 福建经纬新纤科技实业有限公司 | Manufacture equipment system for fire-resistant polyester fiber |
Non-Patent Citations (1)
| Title |
|---|
| 蔡秀卿: "《合成纤维生产工艺学 第二版 （下册）》", 30 June 1994, 中国纺织出版社 * |
Cited By (11)
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|---|---|---|---|---|
| CN103290507A (en) * | 2013-05-07 | 2013-09-11 | 桐乡市中辰化纤有限公司 | Preparation method of polymerized micro-amount modified super bright polyester fibers |
| CN103290507B (en) * | 2013-05-07 | 2016-03-02 | 桐乡市中辰化纤有限公司 | A kind of preparation method being polymerized micro-modification lustrous polyester fiber |
| CN104262598A (en) * | 2014-10-14 | 2015-01-07 | 浙江万凯新材料有限公司 | Online polyester production conversion equipment and production conversion method adopting same |
| CN104403091A (en) * | 2014-11-18 | 2015-03-11 | 浙江古纤道新材料股份有限公司 | Polyester production equipment and technology |
| CN104403091B (en) * | 2014-11-18 | 2017-02-22 | 浙江古纤道新材料股份有限公司 | Polyester production equipment and technology |
| CN110835407A (en) * | 2018-08-16 | 2020-02-25 | 远东新世纪股份有限公司 | Polyester polyol, method for producing same, and polyurethane foam material |
| CN110724253A (en) * | 2019-11-14 | 2020-01-24 | 扬州普立特科技发展有限公司 | Full-continuous PBAT production equipment and process flow |
| CN110790907A (en) * | 2019-11-18 | 2020-02-14 | 扬州普立特科技发展有限公司 | Production equipment and process flow of full-continuous PETG |
| CN110818888A (en) * | 2019-12-17 | 2020-02-21 | 扬州普立特科技发展有限公司 | Production equipment and process flow of fully-continuous PBS (Poly Butylene succinate) |
| CN111910265A (en) * | 2020-07-17 | 2020-11-10 | 湖南工程学院 | Electrostatic spinning injection device with liquid preparation function |
| CN111850721A (en) * | 2020-08-11 | 2020-10-30 | 江苏华西村股份有限公司 | Special short fiber production line for high-cleanness spunlace non-woven fabric |
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