CN101805445B - Chemical treating method for melt polycondensation high polymer old material regeneration - Google Patents
Chemical treating method for melt polycondensation high polymer old material regeneration Download PDFInfo
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
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- Y02W30/62—Plastics recycling; Rubber recycling
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Abstract
The invention relates to a chemical treating method for melt polycondensation high polymer old material regeneration and belongs to the technical field of chemical fiber and plastic processing. According to the method, a molecular chain structure is changed substantially, and organic impurities of polyolefin such as a PVC, a PP, a PE and the like and polyolefin derivatives are removed from a recycled material by the following process procedures of alcoholysis or hydrolysis, homogenization, impurities removal, micromolecule removal and reaggregation in a homogenization reaggregation integrated horizontal reactor, so that the purity and the quality of a regenerative raw material are improved, and uniformity, impurity content and final quality of formed polyester melt are much higher than indexes; and the polyester melt is widely applied to occasions with higher requirements on the quality of the recycled materials, such as a POY filament yarn, a three-dimensional sandwich, an FDY, non-woven fabric, a moderately strong industrial filament, a reusable bottle and the like, the demand of the raw material and the consumption of petroleum resource are reduced, and the polyester melt is favorable for realizing recycling economy.
Description
Technical field
The present invention relates to a kind of chemical treatment method of melt polycondensation high polymer old material regeneration; In order to improve melt polycondensation high polymer old salvage material regenerated quality quality; The reprocessing cycle that is specifically related to high polymer old materials such as polyester, polymeric amide, polycarbonate is used, and belongs to chemical fibre, technical field of plastic.
Background technology
The reclaiming of existing high polymer old material realizes through the physics method or through chemical method.
The characteristics of chemical method be exactly whole process be core with the chemical reaction, reclaimed materials needs after chemical reaction further to improve some quality index or several quality index.Chemical method can improve some inner quality index of raw material from changing structure in essence; Chemical method not only can be removed the organic impurity that mechanical impurity can also be removed other non-PET classes, thereby improves the quality of product.
There are following some shortcomings in existing physics method: it is very high that (1) requires to reclaim material quality, " particular about food " phenomenon of originating highly stable; (2) even reached the quality requirements of raw material, also because reclaimed materials has always passed through processing, the downgrade that in the course of processing, causes cannot be repaired; (3) quality uniformity of raw material does not reach the high quality of industrialized unit, successional requirement.
Summary of the invention
The objective of the invention is above-mentioned deficiency to the existence of existing recovery raw material regenerated physics method; Provide and to change molecular chain structure; Polyolefine and derivatives class organic impuritys thereof such as the PVC in the removal recovery raw material, PP, PE, thereby the chemical treatment method of a kind of melt polycondensation high polymer old material regeneration of the purity of raising regenerative raw materials and quality.
The objective of the invention is to realize through following technical scheme; A kind of chemical treatment method of melt polycondensation high polymer old material regeneration; Comprise that waste and old material becomes melt through the fusion of common deep trouth list screw rod; The mechanical impurity and the solid impurity that filter out in the melt through strainer obtain comparatively purified melt again; It is characterized in that; Said method comprises that also the mass percent after the filtration is 100% melt adds 500-30000ppm alcoholysis agent, 10-120ppm catalyzer and the 0-50ppm whitening agent of the preparation of auxiliary material add-on system by mass percentage in being connected to the melt pipe of static mixer a mixed solution, and melt and mixed solution get into behind the uniform mixing in static mixer accomplishes alcoholysis or hydrolysis reaction in the integrated horizontal reactor of homogenizing reaggregation, regenerates in homogenizing, decon, removal small molecules technological process and reaggregation reaction back.
Terepthaloyl moietie is adopted in described alcoholysis agent, and catalyzer adopts the antimony series polyester catalyst.
Described alcoholysis or hydrolysis reaction are to get into behind melt and the mixed solution uniform mixing in the integrated horizontal reactor of homogenizing reaggregation; At temperature 230-300 ℃; Under the condition of absolute pressure 80-240Pa, the depolymerization reaction of beginning alcoholysis or hydrolysis, the about 2-15 of continuously stirring minute; Melt and terepthaloyl moietie are accomplished halfway local control alcoholysis reaction, obtain polymerization more evenly, the narrower polymer melt of MWD.
Described homogenizing process process is to stir the process that makes the alcoholysis reaction homogenizing through static mixer and reactor drum; Control alcoholysis agent content, the mixedness of static mixer and the relation between the stirring velocity; Let the alcoholysis agent fully contact the molecular melt chain, reach evenly in that statistical average is conceptive, form the suitable melt of molecular chain length; Reduce the kinetic viscosity of whole melt, realized the homogenizing process process.
Said decon process and homogenization process take place simultaneously, and polymer melt is at temperature 230-300 ℃, under the condition of absolute pressure 10-1000Pa; Polyolefins impurity generation decomposition reaction, the molecular weight of product of formation very low and can the part gasified, under lower kinetic viscosity; Low molecular weight impurities and gas thereof are diffused in the gas-phase space more easily; Through whisking appliance 1-10 rev/min speed control, the melt that is entrained with low molecular weight impurities and gas thereof has shortened the time from the melt internal divergence to gas phase gradually in the disk film forming of whisking appliance; Under the continuously pumping effect of vacuum system; Broken away from reactor drum, got into the impurity separation system, thereby reached the effect of decon.
Said removal small molecules technological process is that polymer melt is at temperature 230-300 ℃; Under the condition of absolute pressure 10-1000Pa; The degradation product that produces in residual moisture, screw rod melting process and the filtration procedure and carry out small molecules such as EG that reaggregation when reaction generate under the effect that rotation is stirred is taken away by vacuum system gradually.
Said reaggregation reaction process is that polymer melt is under the effect of antimony series polyester catalyst; At temperature 230-300 ℃; Under the condition of absolute pressure 10-1000Pa, and remove small molecules progressively condensation polymerization reaction takes place simultaneously, the even oligomer that alcoholysis or hydrolysis are formed regroups according to moulding the mechanism of gathering reaction; Molecular chain length progressively increases with the reduction of small molecules concentration in time, up to the molecular weight technical requirements that reaches the following process goods.
The integrated horizontal reactor of described homogenizing reaggregation is by cylindrical tube; The cylindrical shell two ends are through the bolted end cap of lip weldering tongued and grooved flanges; The oblique anti-blocking liquidometer mouth down that end cap is provided with near the bottom; The combination vacuum-sealing mechanism that tape spool that respective ends covers holds is passed at the stir shaft two ends that are provided with in the cylindrical shell, the stirring disc of fixed interval successively from front to back on the stir shaft, step-down gear and drive-motor that stir shaft one end connects; An end is fixed on the baffle plate that has opening on the cylinder inboard wall between the stirring disc; The heating agent chuck of the cylindrical shell outside and the welding of end cap outer face, cylindrical shell is near the opening for feed of the bottom solid welding of front end and the cylindrical shell discharge port near the bottom solid welding of rear end, the gas phase mouth formation of the cylindrical shell top solid welding of corresponding discharge port; Each baffle plate is connected on the cylinder inboard wall with bolt; The gas phase mouth of the integrated horizontal reactor of homogenizing reaggregation connects impurity separation system and vacuum system; The exit of the integrated horizontal reactor of homogenizing reaggregation connects melt vacuum self priming pump and in-line viscometer; Each heating agent chuck connects the heating agent heating system on the integrated horizontal reactor of homogenizing reaggregation; Bottom near the integrated horizontal reactor end cap of homogenizing reaggregation is provided with anti-blocking liquidometer mouth, inserts liquidometer in the anti-blocking liquidometer mouth.
The front and rear cover center slightly is provided with the stirring axis hole to the bottom eccentric part.
Stir the open-celled structure that adopts gradual change successively on the disc.
The present invention is through accomplishing alcoholysis or hydrolysis, homogenizing, decon, removal small molecules, the several technological processs of reaggregation in the integrated horizontal reactor of homogenizing reaggregation; From having changed molecular chain structure in essence; Polyolefine and derivatives class organic impuritys thereof such as the PVC that reclaims in the raw material, PP, PE have been removed; Thereby the purity and the quality of regenerative raw materials have been improved; The polyester fondant that forms thus just is higher than these indexs of raw material far away in homogeneity, foreign matter content and final quality; Thereby be widely used in POY long filament, three-dimensional hollow, FDY, non-woven fabrics, in strong industry silk, regeneration bottle etc. to reclaiming the occasion that raw materials quality is had relatively high expectations, reduce demand and consumption of petroleum resources to former raw material, realize recycling economy.The present invention has following beneficial effect:
(1) flexibility to waste and old raw material is strong, can use several extremely greatly markets to reclaim waste and old raw material and produce high quality raw product again;
(2) core of the present invention is homogenizing reaggregation process, has solved the quality problem of non-uniform between the raw material of different sources, and the raw material same with the physics method through this art breading, can be produced the product that quality is more stable, quality is higher;
(3) the present invention's macromolecule melt quality of producing can online adjustment quality index, and stably manufactured, satisfies the different industries specification of quality different to of a sort raw material;
(4) present technique is follow-up can use by supporting direct melt continuously, does not produce middle article (superpolymer particle) and need not regenerate, and reduces production process and energy consumption.
Description of drawings
Fig. 1 is the process flow sheet among the present invention;
Fig. 2 is the integrated horizontal reactor structural representation of homogenizing reaggregation among the present invention;
Among the figure, 1 common deep trouth list screw rod, 2 strainers, 3 auxiliary material add-on systems, the integrated horizontal reactor of 4 homogenizing reaggregations, 5 impurity separation systems; 6 vacuum systems, 7 heating agent heating systems, 8 melt vacuum self priming pumps, 9 in-line viscometers, 10 strainers, 11 heating agent chucks; 12 baffle plates, 13 stir disc, 14 cylindrical shells, 15 stir shafts, 16 discharge ports, 17 combination vacuum-sealings; 18 gas phase mouths, 19 anti-blocking liquidometer mouths, 20-end cap, 21 opening for feeds, 22 static mixers.
Embodiment
Further specify the present invention in conjunction with accompanying drawing and embodiment; As shown in Figure 1; Reclaimed materials of the present invention is becoming melt through the fusion of common deep trouth list screw rod, and the mechanical impurity and the solid impurity that filter out in the melt through strainer obtain comparatively purified melt again, in the integrated horizontal reactor of homogenizing reaggregation, carries out alcoholysis, homogenizing, decon, removal small molecules, these several technological processs of reaggregation again; Make the molecular structure of reclaimed materials readjust, satisfy the product requirement of different purposes.
1 fusion becomes melt through common deep trouth list screw rod to reclaim raw material, filters out mechanical impurity and solid impurity in the raw material through strainer 2 again, obtains comparatively purified melt.The melt of this moment is because the ununiformity of raw material and a small amount of hydrolysis that in screw rod 1 and strainer 2, takes place, thermal destruction and oxygen are degraded, and quality is bad.This moment in melt pipe according to ratio and the initial set value calculated; Adopt the addition successive of the control of regulating loop alcoholysis agent terepthaloyl moietie (EG), catalyzer (antimony series polyester catalyst) and whitening agent proportional mixing to add in the main melt pipe through auxiliary material add-on system 3; And, be fed through the integrated horizontal reactor 4 of homogenizing reaggregation through static mixer 22 uniform mixing.At integrated horizontal reactor 4 foremost; Local alcoholysis reaction takes place in alcoholysis agent terepthaloyl moietie EG and polyester fondant under 230-300 ℃, absolute pressure 80-240pa condition; Form the polyester oligomer; The MWD that under reversible balanced reaction, forms the oligomer of certain molecular chain length narrows down, and along with the reaction of stirring under disc 13 stirring actions in the reactor drum 4 is carried out, the homogeneity of melt has been enhanced; Meanwhile, organic impurity major parts such as PE, PP, PVC are by thermolysis; The kinetic viscosity of whole melt also is lowered thereupon, has reduced the diffusional resistance of vapour from the melt to the gas phase, helps removing small molecules and resolvent.Take up in the gas-phase space that is exposed to reactor drum being stirred disc 13 gradually subsequently; Most of impurity and small molecules that decomposes progressively is diffused in the gas-phase space; Reversible balanced reaction is carried out to direction of polymerization gradually; Under the suction function of vacuum system 6, impurity of separating and small molecules are condensed through impurity separation system 5 and collect.The melt that regroups is transported in the strainer 10 through melt vacuum self priming pump 8; Melt pressure and flow that melt vacuum self priming pump 8 provides spinning to need; In strainer 10, further filter the mechanical impurity residual in the raw material and the aggregated particle of degraded and the stylish generation of polycondensation, to guarantee the melt quality of spinning.Polycondensation is reversible balanced reaction; The small molecules concentration that the controlled polymerization degree can use control to generate realizes indirectly; Be equipped with the real-time quality of in-line viscometer 9 in order to the melt of monitoring output in the Melt Pump outlet, this monitoring data feeds back to vacuum system through automatic control system, with online adjusting vacuum tightness; Thereby control micromolecular concentration, guarantee that the melt quality of outlet is controlled in the very little deviation.Whole process heat energy is provided by heating agent heating system 7, adopts automation control system to realize fully automatic working.
The integrated horizontal reactor of homogenizing reaggregation among the present invention is as shown in Figure 2, and reactor drum 4 is horizontal cylindrical structural, and outside is a cylindrical shell 14; Two ends are front and rear cover 20; End cap 20 is oblique down near bottom direction, has anti-blocking liquidometer mouth 19, welds the tongued and grooved flanges bolt with lip between cylindrical shell 14 and the front and rear cover 20 and is connected; Cylindrical shell 14 and the end cap 20 outer one deck heating agent chucks 11 that all are provided with; Heating agent chuck 11 is welded on cylindrical shell 14 and the end cap 20, and near front end end cover 20 perforates welding opening for feed 21, the bottom is near rear end cap 20 perforates welding discharge port 16 in cylindrical shell 14 bottoms; Perforate is welded with gas phase mouth 18 near rear end cap at cylindrical shell 14 tops; End cap 20 centers slightly are provided with the stirring axis hole to the bottom eccentric part, and stir shaft 15 passes front and rear cover 20 and stirs axis holes, and the combination vacuum-sealing 17 of holding of the tape spool through two ends couples together stir shaft 15 and end cap 20 respectively.Be nested with the fixedly stirring disc 13 of different structure on the stir shaft 15 from front to back successively, stir shaft 15 1 ends connect motor-driven step-down gear, stir disc 13 and are fixed on the main shaft 15 through key and locating sleeve; And between several groups of stirring discs 13, be provided with polylith baffle plate 12; Have opening on the baffle plate 12, resistance difference and partition functionality zone before and after baffle plate 12 is used for increasing, baffle plate 12 usefulness bolts are connected on cylindrical shell 14 inwalls; And spot welding fixes, and also leaves the seam of 10-50mm with cylindrical shell 14 junctions.This inside reactor flows to and adopts zonal structure, also dividing plate can be set, stirs the open-celled structure that disc 13 adopts gradual change successively; Adapt to different viscosity and flow, axle system is eccentric installs, and integral body inclination angle slightly; Barrel does not have the dead angle; Form macromolecule melt mobile plug flow effect, accomplish alcoholysis (hydrolysis), homogenizing, decon smoothly, remove the integrated of low molecule, the several technological processs of reaggregation, and realize serialization production.
Anti-blocking liquidometer mouth 19 is open joints with well, along the sleeve pipe trend, is equipped with one on the top and stops up poker, and just often poker is pulled upwardly, and liquidometer is in normal operating conditions; When taking place to stop up, poker can move along interior pipe from top to bottom, the tamper in the cleaning sleeve pipe, and cleaning is withdrawn into original position again after finishing.
Mass percent after filtering among the present invention is that 100% melt is meant the melt flow of measuring with the vacuum self priming pump place.
Impurity separation system among the present invention, vacuum system, vacuum self priming pump, viscometer, heating agent heating system, motor and speed reducer adopt currently available products and prior art.
Claims (4)
1. the chemical treatment method of a melt polycondensation high polymer old material regeneration; Comprise that waste and old material becomes melt through the fusion of common deep trouth list screw rod; The mechanical impurity and the solid impurity that filter out in the melt through strainer obtain comparatively purified melt again; It is characterized in that; Said method comprises that also the mass percent after the filtration is 100% melt adds 500-30000ppm alcoholysis agent, 10-120ppm catalyzer and the 0-50ppm whitening agent of the preparation of auxiliary material add-on system by mass percentage in being connected to the melt pipe of static mixer a mixed solution; Melt and mixed solution get in the integrated horizontal reactor of homogenizing reaggregation behind the uniform mixing in static mixer and accomplish alcoholysis reaction, homogenizing, decon, removal small molecules technological process and reaggregation reaction back regeneration;
Terepthaloyl moietie is adopted in described alcoholysis agent, and catalyzer adopts the antimony series polyester catalyst;
Described alcoholysis reaction is to get into behind melt and the mixed solution uniform mixing in the integrated horizontal reactor of homogenizing reaggregation; At temperature 230-300 ℃; Under the condition of absolute pressure 80-240Pa, the depolymerization reaction of beginning alcoholysis, continuously stirring 2-15 minute; Melt and terepthaloyl moietie are accomplished halfway local control alcoholysis reaction, obtain polymerization more evenly, the narrower polymer melt of MWD;
Described homogenizing process process is to stir the process that makes the alcoholysis reaction homogenizing through static mixer and reactor drum; Control alcoholysis agent content, the mixedness of static mixer and the relation between the stirring velocity; Let the alcoholysis agent fully contact the molecular melt chain, reach evenly in that statistical average is conceptive, form the suitable melt of molecular chain length; Reduce the kinetic viscosity of whole melt, realized the homogenizing process process;
Said decon process and homogenization process take place simultaneously, and polymer melt is at temperature 230-300 ℃, under the condition of absolute pressure 10-1000Pa; Polyolefins impurity generation decomposition reaction, the molecular weight of product of formation very low and can the part gasified, under lower kinetic viscosity; Low molecular weight impurities and gas thereof are diffused in the gas-phase space more easily; Through whisking appliance 1-10 rev/min speed control, the melt that is entrained with low molecular weight impurities and gas thereof has shortened the time from the melt internal divergence to gas phase gradually in the disk film forming of whisking appliance; Under the continuously pumping effect of vacuum system; Broken away from reactor drum, got into the impurity separation system, thereby reached the effect of decon;
Said removal small molecules technological process is that polymer melt is at temperature 230-300 ℃; Under the condition of absolute pressure 10-1000Pa; The degradation product that produces in residual moisture, screw rod melting process and the filtration procedure and carry out EG small molecules that reaggregation when reaction generate under the effect that rotation is stirred is taken away by vacuum system gradually;
Said reaggregation reaction process is that polymer melt is under the effect of antimony series polyester catalyst; At temperature 230-300 ℃; Under the condition of absolute pressure 10-1000Pa, and remove small molecules progressively condensation polymerization reaction takes place simultaneously, the even oligomer that alcoholysis is formed regroups according to the mechanism of polycondensation; Molecular chain length progressively increases with the reduction of small molecules concentration in time, up to the molecular weight technical requirements that reaches the following process goods.
2. realize the integrated horizontal reactor of homogenizing reaggregation of the chemical treatment method employing of the described melt polycondensation high polymer old material reclaiming of claim 1; It is characterized in that; The integrated horizontal reactor of described homogenizing reaggregation is by cylindrical tube; The cylindrical shell two ends are through the bolted end cap of lip weldering tongued and grooved flanges, the oblique anti-blocking liquidometer mouth down that end cap is provided with near the bottom, and the combination vacuum-sealing mechanism that tape spool that respective ends covers holds is passed at the stir shaft two ends that are provided with in the cylindrical shell; The stirring disc of fixed interval successively from front to back on the stir shaft; Step-down gear and drive-motor that stir shaft one end connects, an end is fixed on the baffle plate that has opening on the cylinder inboard wall between the stirring disc, the heating agent chuck of the cylindrical shell outside and the welding of end cap outer face; Cylindrical shell is near the opening for feed of the bottom solid welding of front end and the cylindrical shell discharge port near the bottom solid welding of rear end, and the gas phase mouth of the cylindrical shell top solid welding of corresponding discharge port constitutes; Each baffle plate is connected on the cylinder inboard wall with bolt; The gas phase mouth of the integrated horizontal reactor of homogenizing reaggregation connects impurity separation system and vacuum system; The exit of the integrated horizontal reactor of homogenizing reaggregation connects melt vacuum self priming pump and in-line viscometer; Each heating agent chuck connects the heating agent heating system on the integrated horizontal reactor of homogenizing reaggregation; Bottom near the integrated horizontal reactor end cap of homogenizing reaggregation is provided with anti-blocking liquidometer mouth, inserts liquidometer in the anti-blocking liquidometer mouth.
3. the integrated horizontal reactor of homogenizing reaggregation according to claim 2 is characterized in that, the front and rear cover center slightly is provided with the stirring axis hole to the bottom eccentric part.
4. the integrated horizontal reactor of homogenizing reaggregation according to claim 3 is characterized in that, stirs the open-celled structure that adopts gradual change successively on the disc.
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| CN103146151B (en) * | 2011-12-06 | 2015-04-08 | 上海聚友化工有限公司 | Recycling method of waste polyester bottle |
| CN102532815B (en) * | 2011-12-06 | 2013-09-25 | 上海聚友化工有限公司 | Method for recycling waste polyester textiles |
| CN102731760B (en) * | 2012-07-17 | 2014-03-26 | 龙福环能科技股份有限公司 | Method for carrying out alcoholysis and then polymerization on recycled polyester bottle chip melts |
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| CN107698772B (en) * | 2017-10-17 | 2018-10-09 | 浙江中邦塑胶股份有限公司 | A kind of method of the branched enhancing regenerated plastics in original position |
| DE102018202547A1 (en) * | 2018-02-20 | 2019-10-02 | Thyssenkrupp Ag | Apparatus and method for mixing recycled material into a polyester melt |
| CN109345584A (en) * | 2018-09-20 | 2019-02-15 | 华北理工大学 | The method for calculating object area in high-temperature fusant is extracted based on hierarchical clustering algorithm |
| CN111253566B (en) * | 2020-02-14 | 2021-04-06 | 东华大学 | Polyamide 6 polycondensation reactor for efficient devolatilization and green recovery of polymerized monomers |
| CN111793832B (en) * | 2020-06-30 | 2022-03-01 | 浙江海利环保科技股份有限公司 | Method for removing oligomer in preparation process of regenerated polyester filament yarn melt |
| CN112225661B (en) * | 2020-10-16 | 2022-11-18 | 艾凡佳德(上海)环保科技有限公司 | Impurity removal method and equipment for alcoholysis product after continuous alcoholysis of waste polyester |
| CN113150375B (en) * | 2021-03-29 | 2022-12-27 | 中国科学院青岛生物能源与过程研究所 | Method for recycling polylactic acid material under catalysis of zinc catalyst |
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