CN101935393A - Recycling process of dacron wastes on continuous polymerization production line and device thereof - Google Patents
Recycling process of dacron wastes on continuous polymerization production line and device thereof Download PDFInfo
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- CN101935393A CN101935393A CN2009101813361A CN200910181336A CN101935393A CN 101935393 A CN101935393 A CN 101935393A CN 2009101813361 A CN2009101813361 A CN 2009101813361A CN 200910181336 A CN200910181336 A CN 200910181336A CN 101935393 A CN101935393 A CN 101935393A
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Abstract
The invention discloses a recycling process of dacron wastes on a continuous polymerization production line and a device thereof. The recycling process of the dacron wastes comprises the following steps of: (a) mixing purified terephthalic acid with glycol for stirring; (b) carrying out esterification reaction on uniformly mixed materials; (c) carrying out polymerization reaction on sufficiently esterified materials; (d) sucking polymers by using a material sucking pump, filtering, and then spinning or slicing and pelletizing; and (e) grinding, melting and alcoholizing wastes generated from the step (d), and then recycling to the step (c) for mixing with fresh materials for polymerization. The device comprises a stirring system, an esterification system, a polymerization system and a dacron waste addition system, wherein the stirring system, the esterification system and the polymerization system are sequentially connected in series; one end of the dacron waste addition system is connected with a waste inlet, and the other end is connected with the polymerization system.
Description
Technical field
The present invention relates to technology and device that polyster fibre is produced, relate in particular to a kind of technology and device that utilizes terylene waste material on the successive polymerization production line, to utilize again.
Background technology
Polyester is extensively applied in the various application, thereby wherein many high molecular weight polyesters that needs obtain needed every performance.Thus, polyester can be used to make the moulded parts such as food and beverage container.The technology of present domestic production terylene is comparative maturity, for example four still continuous polymerization unit and the technical process that design by China Textiles Industry Designing Institute, and other five stills successive polymerization flow processs or one two tail successive polymerization flow path device, all have a wide range of applications industrial.Along with the development of domestic PET industry, in the production of polyester, also unavoidably can produce a large amount of industrial wastes.The waste material that produces in the present industrial production (comprising waste silk, useless piece), terylene factory generally all is sold to little factory and reclaims use in addition, generally can not directly reclaim use.This has reduced economic benefit of enterprises to a certain extent, has wasted resource.
Summary of the invention
Technical problem to be solved by this invention is how can directly utilize the terylene waste material that is produced in the technical process of successive polymerization, thereby save energy, resource improves economic benefit of enterprises.
For solving the problems of the technologies described above, the technology that technical scheme of the present invention provides a kind of terylene waste material to utilize on the successive polymerization production line again, this technology may further comprise the steps: (a) pure terephthalic acid is mixed stirring with ethylene glycol; (b) mixed uniformly material is carried out esterification; (c) material after the abundant esterification is carried out polyreaction; (d) with polymkeric substance with charging absorption pump sucking-off, filtration, reel off raw silk from cocoons then or cut into slices pelletizing; (e) by mixing with fresh material, carry out polymerization with being recycled in (c) after (d) middle waste material process pulverizing that produces, fusion, the alcoholysis.
A preferred embodiment of the present invention is: earlier mixed uniformly material is sent into first esterifying kettle in the described step (b) and carry out esterification, then material is sent into the further esterification of second esterifying kettle again; Earlier the material after the abundant esterification is sent into the first precondensation still in the described step (c) and carried out the prepolymerization reaction, and then reacted polymkeric substance is sent into whole polycondensation vessel carry out further polyreaction; Join after waste material pulverizing by will producing in (d) in the described step (e), fusion, the alcoholysis and mix with fresh material in first polycondensation vessel and waste material is recycled to step (c).
Terylene waste material of the present invention utilizes a kind of preferred version of technology to be on the successive polymerization production line again: the waste material in the described step (e) adds the screw extruder fusion after crushed, and in the 5th district and ethylene glycol mixing alcoholysis of screw rod, make its limiting viscosity from dropping to 0.30 η～0.25 η more than 0.60 η, and then be recycled to step (c).
Terylene waste material of the present invention utilizes a kind of preferred version of technology to be on the successive polymerization production line again: the ratio control of the add-on of ethylene glycol and waste material is between 5%～10% in the described step (e), screw rod the 5th district's temperature is controlled at 269 degrees centigrade to 271 degrees centigrade, and the ratio of mixture of waste material and fresh material is 1%～10% in the described step (e).
Terylene waste material of the present invention utilizes a kind of preferred version of technology to be on the successive polymerization production line again: the ratio of mixture of waste material and fresh material is 2%～3% in the described step (e).
Terylene waste material of the present invention utilizes a kind of preferred version of technology to be on the successive polymerization production line again: screw rod first district's temperature is controlled at 150 degrees centigrade to 200 degrees centigrade in the described step (e), two district's temperature are controlled at 265 degrees centigrade to 268 degrees centigrade, three district's temperature are controlled at 267 degrees centigrade to 270 degrees centigrade, and four district's temperature are controlled at 269 degrees centigrade to 271 degrees centigrade.
For implementing above-mentioned technology, technical scheme of the present invention also provides implements terylene waste material utilizes technology again on the successive polymerization production line device, this device comprises: stirring system, esterification system, paradigmatic system, it between three systems placed in-line successively relation, also comprise the terylene waste material add-on system, this system is connected with paradigmatic system, described terylene waste material add-on system adds system and screw extruder by ethylene glycol, temperature sensor, pressure transmitter, strainer, volume pump, jacket pipe, go out stub bar and form, wherein ethylene glycol adds system and screw extruder, temperature sensor, pressure transmitter, strainer, volume pump, going out stub bar is linked in sequence.
Enforcement terylene waste material of the present invention utilizes a kind of preferred version of the device of technology to be on the successive polymerization production line again: described screw extruder is divided into five districts, wherein the 5th district is for mixing the alcoholysis district, have the nail-shaped mixing head on this district's screw rod, and this section length is 3.5: 1 with the diameter ratio, on the screw sleeve at this melt inlet place, district, have an aperture at least, be provided with the ethylene glycol inlet nozzle.
Enforcement terylene waste material of the present invention utilizes a kind of preferred version of the device of technology to be on the successive polymerization production line again: described ethylene glycol adds system and is made up of ethylene glycol storage tank, nitrogen tube, accurate under meter, check valve, chuck cooling tube, ethylene glycol inlet nozzle.
Enforcement terylene waste material of the present invention utilizes a kind of preferred version of the device of technology to be on the successive polymerization production line again: described device has the heating agent heat-insulation system, material is carried out temperature control.
Technique effect of the present invention is: technology of the present invention and device thereof are by being recycled directly in the polyreaction after terylene waste material pulverizing, fusion, the alcoholysis, thereby general 2%～3% terylene waste material that produces in the general continuous polymerization unit can be recycled directly in the continuous polymerization unit utilize, thereby waste material has been become finished product, improve economic benefit, further improved the utility value of terylene waste material.
Description of drawings
The invention will be further described below in conjunction with accompanying drawing.
Fig. 1 is a process flow sheet of the present invention.
Fig. 2 is the technological process device synoptic diagram of a specific embodiment of the present invention.
Fig. 3 is existing five still continuous polymerization unit schematic flow sheets.
Fig. 4 is the process flow diagram of existing " one two tail " device.
Embodiment
Fig. 1 is a process flow sheet of the present invention.Fig. 2 is the concrete technological process device synoptic diagram of one embodiment of the invention, and wherein: pure terephthalic acid's feed bin 1, ethylene glycol storage tank 2, stirring tank 3, first esterifying kettle 4, second esterifying kettle 5, the first precondensation still 6, whole polycondensation vessel 7, ethylene glycol add system 8, accurate under meter 9, check valve 10, screw extruder 11, the preceding temperature sensor 12 of filter, thief hole 13, the preceding pressure transmitter 14 of filter, fondant filter 15, filter back pressure transmitter 16, volume pump 17, filter back temperature sensor 18, go out stub bar 19.
Concrete technical process is as follows: 1. the pure terephthalic acid delivers to pure terephthalic acid's feed bin through conveyor chain, continuously sends into the making beating still from pure terephthalic acid's feed bin through metering, and ethylene glycol is continuously sent into the making beating still from storage tank through metering simultaneously.2. pure terephthalic acid and ethylene glycol are uniformly mixed into slurry under the stirring action of making beating still agitator.Slurry is continuously sent into first esterifying kettle by spiral pump by certain amount again and is carried out esterification.3. first esterification.Around the esterifying kettle and in the still heating unit is arranged all, normal temps is controlled between 254 degrees centigrade～265 degrees centigrade.Esterification mainly is a thermo-negative reaction.A large amount of water and ethylene glycol steam of producing in the reaction process.Water enters process tower with ethylene glycol steam to be separated, and water is discharged from, and an ethylene glycol part be back to first esterifying kettle participate in again the reaction, a part is discharged into the ethylene glycol storage tank.Material stops in first esterifying kettle after 4～5 hours and to flow into second esterifying kettle and carry out further esterification.4. second esterification.Second esterification mainly is that the material esterification yield general requirement of sending after second esterification reaches 96～97% with the incomplete good further esterification of material of esterification after first esterification.Material the second esterifying kettle residence time about 2 hours.This still temperature generally is controlled between 256 degrees centigrade to 266 degrees centigrade.Material will flow into the first precondensation still and carry out the preshrunk polyreaction after abundant esterification.5. first precondensation.This still divides inside and outside two Room, and the temperature of two Room is different, and the negative pressure value of two Room is also different.Material is in this still, and under certain negative pressure and temperature condition, carboxylate (material) begins polymerization.After reaching certain polymerization degree, polymkeric substance flows into inner room from the mistress again, and material carries out further polymerization under the effect of agitator, vacuum box temperature, after polymkeric substance reaches certain viscosity, material is admitted to whole polycondensation vessel through strainer and carries out last polymerization by the charging absorption pump sucking-off.6. final minification is poly-.This still is a horizontal retort, and horizontal mixer all is equipped with at the two ends of still.The temperature of this still generally is controlled at 272 degrees centigrade～283 degrees centigrade.Polymkeric substance under the effect of high temperature, high negative pressure and agitator, polymerization fully and uniformly.When polymer viscosity reaches (the finished product index request) more than 0.66 η.Polymkeric substance, is sent to spinning and reels off raw silk from cocoons or send into dicing machine and be cut into the section particle, be i.e. the finished product of this continuous apparatus through strainer by the charging absorption pump sucking-off.
General this continuous apparatus can produce 2%～3% waste material, the waste material that comprises spinning, these waste materials are directly sent into the terylene waste material add-on system, waste material is through after cutting off, pulverizing in this system, add screw extruder, carry out fusion, alcoholysis, extrude by going out stub bar then, join in the precondensation still of continuous apparatus and fresh material uniform mixing under the stirring of agitator, and together carry out new polyreaction.Specific as follows:
A. waste silk adds screw extruder through after cutting off (scrap is through pulverizing, and useless section can directly add), and this screw rod is the particular design screw rod.Screw rod is provided with five districts, and the temperature in each district is controlled respectively, and it is different that each distinguishes function.One district is a material feeding region, is furnished with the desalination cooling system, and normal temps is controlled at 150 degrees centigrade to 200 degrees centigrade.Two districts are melting zone, and temperature is controlled at 265 degrees centigrade to 268 degrees centigrade.Three districts are crush zone, and temperature is controlled at 267 degrees centigrade to 270 degrees centigrade.Four districts are metering zone, and temperature is controlled at 269 degrees centigrade to 271 degrees centigrade.Five districts are for mixing the alcoholysis district, and this district also is the different places with other screw extrusion presss of particular design screw rod of the present invention.Difference is: have the nail-shaped mixing head on (1) this district's screw rod.And this section length is special design, and its length-to-diameter ratio (ratio of length and diameter) is 3.5: 1.The purpose that increases length is in order to improve mixed effect, to strengthen the alcoholysis effect.(2) on the screw sleeve at this melt inlet place, district, have an aperture, the ethylene glycol inlet nozzle is housed.Make ethylene glycol in this district and melt-mixing, and make polymkeric substance make its limiting viscosity from dropping to 0.30 η～0.25 η more than 0.60 η in this alcoholysis.The size of this limiting viscosity be directly connected to material the precondensation still whether can with the original material uniform mixing of precondensation still, and together reaction.The big or small key of this limiting viscosity depends on the adding proportion of ethylene glycol and the temperature setting and the control in screw rod four, five districts.The add-on of ethylene glycol normally is controlled between 5%～10%, and five district's temperature generally are controlled at 269 degrees centigrade to 271 degrees centigrade.If control badly, will cause the undue alcoholysis of polyester fondant, be unfavorable for that later process carries out, cause the polymer viscosity inequality when serious, directly influence end product quality.
Described ethylene glycol adds by following system: 1. ethylene glycol extrudes by nitrogen in storage tank.(the using and the reserved).The ethylene glycol nozzle that enters on the screw sleeve through nitrogen tube, accurate flow calorimeter, check valve, chuck cooling tube enters the screw mixes district.2. the flow of ethylene glycol.Automatic pressure regulator by accurate flow calorimeter control nitrogen pipeline guarantees the stable of ethylene glycol add-on.3. check valve is the refluence that prevents material in the Special Circumstances screw rod.Cooling jacket is not allow the heat passage vaporization that has prevented ethylene glycol to the ethylene glycol pipeline of screw rod.4. material is after screw rod is extruded, each operation of process all adopt the heating agent insulation.The open degree that temperature control is regulated the variable valve of heating agent pipeline by temperature regulator realizes temperature control.This temperature generally is controlled at 265 degrees centigrade to 268 degrees centigrade.
B. material is sent from screw extrusion press and is entered the chuck materail tube, (materail tube is provided with the material thief hole, is convenient to the material assay).Preceding after filtration pressure transmitter, strainer, pressure transmitter after filtering again.(pressure transmitter is all controlled interlocking with screw drive before and after filtering, and preceding pressure is a protector.When pressure surpasses set(ting)value.Screw rod will shut down automatically.Filter back pressure transmitter is the control steady state value.When fluctuation appearred in pressure, screw rod guaranteed the constant supply of storeroom with the automatic deceleration degree) thus the enough pressure of material before the volume pump guaranteed.
C. material is transported to volume pump through the chuck materail tube again by filter back pressure transmitter.Material is sent into out stub bar by pipeline again through accurate measurement.Material is extruded by going out on the stub bar tens apertures, joins in the precondensation still of continuous apparatus and fresh material, uniform mixing under the stirring of agitator, and together carry out new polyreaction.The load of volume pump depends on the mass mixing ratio of reclaimed materials and fresh material, and normally in 1%～10% scope, optimum value is between 2%～3% for this ratio of mixture.
Repeat embodiment 1 by described same steps as, but district's material feeding region temperature is controlled at 150 degrees centigrade, two district's melting zone temperature are controlled at 265 degrees centigrade, three districts are crush zone, and temperature is controlled at 267 degrees centigrade, and four districts are metering zone, temperature is controlled at 269 degrees centigrade, five districts are for mixing the alcoholysis district, and this section length is special design, and its length-to-diameter ratio (ratio of length and diameter) is 4: 1.And make the polymkeric substance alcoholysis make its limiting viscosity from dropping to 0.30 η more than 0.60 η.The add-on of ethylene glycol is controlled at 5%, five district's temperature and generally is controlled at 269 degrees centigrade.The waste material that reclaims and the ratio of mixture of fresh material are 2%.
Repeat embodiment 1 by described same steps as, but district's material feeding region temperature is controlled at 200 degrees centigrade, two district's melting zone temperature are controlled at 268 degrees centigrade, three districts are crush zone, and temperature is controlled at 270 degrees centigrade, and four districts are metering zone, temperature is controlled at 271 degrees centigrade, five districts are for mixing the alcoholysis district, and this section length is special design, and its length-to-diameter ratio (ratio of length and diameter) is 3.75: 1.And make the polymkeric substance alcoholysis make its limiting viscosity from dropping to 0.25 η more than 0.60 η.The add-on of ethylene glycol is controlled at 10%, five district's temperature and generally is controlled at 271 degrees centigrade.The waste material that reclaims and the mass mixing ratio of fresh material are 3%.
The present invention can summarize with other specific form without prejudice to spirit of the present invention or principal character.Therefore, no matter from which point, above-mentioned embodiment of the present invention is the description of this invention, and can not limit the present invention.Any change in implication that claims any and of the present invention are suitable and the scope all should be thought to be included in the scope of claims.
Claims (10)
1. a terylene waste material utilizes technology again on the successive polymerization production line, and this technology may further comprise the steps: (a) pure terephthalic acid is mixed stirring with ethylene glycol; (b) mixed uniformly material is carried out esterification; (c) material after the abundant esterification is carried out polyreaction; (d) with polymkeric substance charging absorption pump sucking-off, filtration, reel off raw silk from cocoons then or cut into slices pelletizing, it is characterized in that: also have step (e),, carry out polymerization by mixing with fresh material with being recycled in (c) after (d) middle waste material process pulverizing that produces, fusion, the alcoholysis.
2. terylene waste material according to claim 1 utilizes technology again on the successive polymerization production line, it is characterized in that: earlier mixed uniformly material is sent into first esterifying kettle in the described step (b) and carry out esterification, then material is sent into the further esterification of second esterifying kettle again; Earlier the material after the abundant esterification is sent into the first precondensation still in the described step (c) and carried out the prepolymerization reaction, and then reacted polymkeric substance is sent into whole polycondensation vessel carry out further polyreaction; Join after waste material pulverizing by will producing in (d) in the described step (e), fusion, the alcoholysis and mix with fresh material in first polycondensation vessel and waste material is recycled to step (c).
3. terylene waste material according to claim 1 utilizes technology again on the successive polymerization production line, it is characterized in that: the waste material in the described step (e) adds the screw extruder fusion after crushed, and in the 5th district and ethylene glycol mixing alcoholysis of screw rod, make its limiting viscosity from dropping to 0.30 η～0.25 η more than 0.60 η, and then be recycled to step (c).
4. terylene waste material according to claim 3 utilizes technology again on the successive polymerization production line, it is characterized in that: the add-on of ethylene glycol and the mass ratio of waste material are controlled between 5%～10% in the described step (e), screw rod the 5th district's temperature is controlled at 269 degrees centigrade to 271 degrees centigrade, and the mass mixing ratio of waste material and fresh material is 1%～10% in the described step (e).
5. terylene waste material according to claim 4 utilizes technology again on the successive polymerization production line, it is characterized in that: the ratio of mixture of waste material and fresh material is 2%～3% in the described step (e).
6. on the successive polymerization production line, utilize technology again according to claim 4 or 5 described terylene waste materials, it is characterized in that: screw rod first district's temperature is controlled at 150 degrees centigrade to 200 degrees centigrade in the described step (e), two district's temperature are controlled at 265 degrees centigrade to 268 degrees centigrade, three district's temperature are controlled at 267 degrees centigrade to 270 degrees centigrade, and four district's temperature are controlled at 269 degrees centigrade to 271 degrees centigrade.
7. implement terylene waste material as claimed in claim 1 utilizes technology again on the successive polymerization production line device for one kind, this device comprises: stirring system, esterification system, paradigmatic system, it between three systems placed in-line successively relation, it is characterized in that: also comprise the terylene waste material add-on system, this system's one end is connected with the waste material import, the other end is connected with paradigmatic system, described terylene waste material add-on system adds system and screw extruder by ethylene glycol, temperature sensor, pressure transmitter, strainer, volume pump, jacket pipe, go out stub bar and form, wherein ethylene glycol adds system and screw extruder, temperature sensor, pressure transmitter, strainer, volume pump, going out stub bar is linked in sequence.
8. device as claimed in claim 7, it is characterized in that: described screw extruder is divided into five districts, wherein the 5th district is for mixing the alcoholysis district, have the nail-shaped mixing head on this district's screw rod, and this section length is 3.5: 1 with the diameter ratio, on the screw sleeve at this melt inlet place, district, have an aperture at least, be provided with the ethylene glycol inlet nozzle.
9. device as claimed in claim 8 is characterized in that: described ethylene glycol adds system and is made up of ethylene glycol storage tank, nitrogen tube, accurate under meter, check valve, chuck cooling tube, ethylene glycol inlet nozzle.
10. according to the described device of arbitrary claim in the claim 7 to 9, it is characterized in that: described device has the heating agent heat-insulation system, material is carried out temperature control.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009101813361A CN101935393A (en) | 2009-07-01 | 2009-07-01 | Recycling process of dacron wastes on continuous polymerization production line and device thereof |
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| CN2009101813361A CN101935393A (en) | 2009-07-01 | 2009-07-01 | Recycling process of dacron wastes on continuous polymerization production line and device thereof |
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| CN101935393A true CN101935393A (en) | 2011-01-05 |
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| CN2009101813361A Pending CN101935393A (en) | 2009-07-01 | 2009-07-01 | Recycling process of dacron wastes on continuous polymerization production line and device thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106832397A (en) * | 2015-12-07 | 2017-06-13 | 中国石化仪征化纤有限责任公司 | The method of online reuse PET Polymerization Wastes |
| CN109575358A (en) * | 2018-12-18 | 2019-04-05 | 中国石油天然气集团有限公司 | Waste polyester film recyclable device and method |
-
2009
- 2009-07-01 CN CN2009101813361A patent/CN101935393A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106832397A (en) * | 2015-12-07 | 2017-06-13 | 中国石化仪征化纤有限责任公司 | The method of online reuse PET Polymerization Wastes |
| CN106832397B (en) * | 2015-12-07 | 2019-09-20 | 中国石化仪征化纤有限责任公司 | The method of online reuse PET Polymerization Waste |
| CN109575358A (en) * | 2018-12-18 | 2019-04-05 | 中国石油天然气集团有限公司 | Waste polyester film recyclable device and method |
| CN109575358B (en) * | 2018-12-18 | 2022-02-18 | 中国石油天然气集团有限公司 | Waste polyester film recovery device and method |
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Application publication date: 20110105 |