CN106279758A - The method that 2,2'-ethylenedioxybis(ethanol). alcoholysis Waste Polyester textile preparation height joins quality melt - Google Patents
The method that 2,2'-ethylenedioxybis(ethanol). alcoholysis Waste Polyester textile preparation height joins quality melt Download PDFInfo
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- CN106279758A CN106279758A CN201610671823.6A CN201610671823A CN106279758A CN 106279758 A CN106279758 A CN 106279758A CN 201610671823 A CN201610671823 A CN 201610671823A CN 106279758 A CN106279758 A CN 106279758A
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- Prior art keywords
- ethylenedioxybis
- ethanol
- melt
- waste polyester
- polyester textile
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J11/00—Recovery or working-up of waste materials
- C08J11/04—Recovery or working-up of waste materials of polymers
- C08J11/10—Recovery or working-up of waste materials of polymers by chemically breaking down the molecular chains of polymers or breaking of crosslinks, e.g. devulcanisation
- C08J11/18—Recovery or working-up of waste materials of polymers by chemically breaking down the molecular chains of polymers or breaking of crosslinks, e.g. devulcanisation by treatment with organic material
- C08J11/22—Recovery or working-up of waste materials of polymers by chemically breaking down the molecular chains of polymers or breaking of crosslinks, e.g. devulcanisation by treatment with organic material by treatment with organic oxygen-containing compounds
- C08J11/24—Recovery or working-up of waste materials of polymers by chemically breaking down the molecular chains of polymers or breaking of crosslinks, e.g. devulcanisation by treatment with organic material by treatment with organic oxygen-containing compounds containing hydroxyl groups
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/25—Component parts, details or accessories; Auxiliary operations
- B29C48/92—Measuring, controlling or regulating
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C2948/00—Indexing scheme relating to extrusion moulding
- B29C2948/92—Measuring, controlling or regulating
- B29C2948/92504—Controlled parameter
- B29C2948/92704—Temperature
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2367/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
-
- 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/62—Plastics recycling; Rubber recycling
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Sustainable Development (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Polyesters Or Polycarbonates (AREA)
- Separation, Recovery Or Treatment Of Waste Materials Containing Plastics (AREA)
Abstract
The present invention relates to a kind of Waste Polyester high level cycling and reutilization technology, be specifically related to the method that a kind of 2,2'-ethylenedioxybis(ethanol). alcoholysis Waste Polyester textile preparation height joins quality melt.The method that 2,2'-ethylenedioxybis(ethanol). alcoholysis Waste Polyester textile preparation height joins quality melt, the method adds raw materials quality 1 ~ 8% 2,2'-ethylenedioxybis(ethanol). at raw material and enters screw extruder blended melting extrusion, the melt viscosity of screw extruder melt out is 0.40 ~ 0.50dl/g, then material enters that quenched tune is adhesive-assembly puts, and the melt viscosity of the adhesive-assembly melt putting out of quenched tune is 0.620dl/g~0.685dl/g.The present invention also efficiently solves, while improving melt viscosity, the problem that the filter cycle is short, vacuum system maintenance is big by adding appropriate 2,2'-ethylenedioxybis(ethanol). alcoholysis, can also improve value-added content of product while reducing production cost.
Description
Technical field
The present invention relates to a kind of Waste Polyester high level cycling and reutilization technology, be specifically related to a kind of 2,2'-ethylenedioxybis(ethanol). alcoholysis Waste Polyester and spin
The method that fabric preparation height joins quality melt.
Background technology
China is the textile production and consumption market that the whole world is maximum at present, and the textile processing total amount of China in 2015 surpasses
50000000 tons, the waste spinning fabric of generation is more than 20,000,000 tons, and Waste Polyester textile accounting therein is up to 70%, adds several years ago
Cumulative stock, the only storage of Waste Polyester textile the most up to more than 200,000,000 tons.But in view of, Waste Polyester textile source complexity,
Uneven and the existing production technology level of foam material quality of processing is limited, and large-scale application or high-value-use there is also bigger
Difficulty.Be mainly reflected in, the foam material impurity content of Waste Polyester textile processing is high, degradable containing more organic pigment, point
Pick the most thoroughly containing being mixed with natural fiber and other Waste Polyester fibers etc..Liquid-phase tackifying technology is used to run into increasing during producing fiber
Mould cyclone filter that agent, slurry, dyestuff and other low molecular weight volatiles cause, dust filter unit, vacuum pipe, tubular heat exchanger
Deng problems such as oligomer easily solidifications, causing vacuum system maintenance to increase, production cost increases.Further, since final melt
Viscosity is relatively low, and the quality of product is affected by certain, and the differentiation of product, the exploitation of high value added product also receive
Limit.
Current existing Waste Polyester textile thickening mainly by liquid-phase tackifying but because Waste Polyester textile source is multiple
Miscellaneous, be increased by the viscosity of the viscous rear polyester of the quenched tune of liquid phase, but thickening amplitude is relatively limited, the most key is molecular weight
Being distributed relatively wide, its main cause is the limited amount of the functional group of carboxyl and the hydroxyl opened in the polyester fondant after melting,
Limit the generation of polycondensation reaction in (≤500Pa), certain time (25min~65min) section under the conditions of certain vacuum.
The Chinese invention patent (application number: 201010574044.7, the applying date: 2010-12-01) of applicant's application is open
The quenched tune of a kind of waste plastics glues system, including vacuum separation tower;Described vacuum separation tower is arranged over feed(raw material)inlet and vacuum
Mouthful;It is provided with discharging opening below described vacuum separation tower;Described vacuum separation tower appearance is provided with heating agent coil pipe;Described vacuum separation tower
Internal vertical is arranged at intervals with porous plate on direction;Described discharging opening is also connected with that two grades of quenched tune are adhesive-assembly to be put.Owing to adding
One two grades of quenched tune are adhesive-assembly to be put, and is provided with screw rod, is possible not only to promote raw material, and can stir raw material and improve in this device
Viscosity;Singly add a vacuum pump, improve vacuum further, provide reaction environment for material viscosity, the above
Factor combines and facilitates significantly improving of High Viscosity PET plastic raw materials production efficiency.
Summary of the invention
Liquid-phase tackifying technology is used to produce polyester staple fiber with the foam material of Waste Polyester textile processing for raw material for existing
In the technical problem that intrinsic viscosity is low, molecular weight distribution is wide that runs into, the invention provides 2,2'-ethylenedioxybis(ethanol). alcoholysis Waste Polyester textile
The method that preparation height joins quality melt, the method uses the foam material of Waste Polyester textile processing to be raw material, through the appropriate alcohol of 2,2'-ethylenedioxybis(ethanol).
The method that after solution, liquid-phase tackifying prepares high-quality polyester fondant again, is improving the same of melt viscosity by adding appropriate 2,2'-ethylenedioxybis(ethanol).
Time also efficiently solve the problem that the filter cycle is short, vacuum system maintenance is big, can also carry reducing while production cost
The added value of high product.
For achieving the above object, present invention employs following technical scheme:
The method that 2,2'-ethylenedioxybis(ethanol). alcoholysis Waste Polyester textile preparation height joins quality melt, the method adds raw materials quality at raw material
1~8% 2,2'-ethylenedioxybis(ethanol). enter screw extruder blended melting extrusion, the melt viscosity of screw extruder melt out be 0.40~
0.50dl/g, then material enters that quenched tune is adhesive-assembly puts, and the melt viscosity of the adhesive-assembly melt putting out of quenched tune is 0.620dl/g
~0.685dl/g.
As improving further, the addition of described 2,2'-ethylenedioxybis(ethanol). is the 3~6% of raw materials quality.
The metering device of the addition of 2,2'-ethylenedioxybis(ethanol). is special 2,2'-ethylenedioxybis(ethanol). pump, and the 2,2'-ethylenedioxybis(ethanol). after metering is noted by pipe special
Enter the center of screw feed mouth, under screw rod and high temperature dual function, between foam material, be mutually mixed spreading to rapid of 2,2'-ethylenedioxybis(ethanol).,
Melt zone and mixed segment 2,2'-ethylenedioxybis(ethanol). in screw rod rotation are sufficiently mixed with melt under the effect of shearing force and frictional force and gradually open
Beginning alcoholysis.
As improving further, the temperature 280 of described screw extruder~300 DEG C, when the stop of screw extruder
Between be 10~20min.
As further improving, described screw extruder Luo mono-district to ten district's temperature be followed successively by 280 DEG C, 285 DEG C,
295℃、295℃、295℃、290℃、290℃、285℃、285℃、285℃。
As improving further, described screw extruder melt out first passes through filter, and to enter back into quenched tune adhesive-assembly
Put, the temperature 280 of filter~290 DEG C.
As improving further, adhesive-assembly the putting of described quenched tune includes interconnective vertical vacuum separating still and horizontal tune
Matter adjusts viscous still, is from top to bottom provided with multi-layer porous plate in vertical vacuum knockout tower, and the bottom that horizontal quenched tune glues still is provided with
It is 280~290 DEG C that augering screw, vertical vacuum knockout tower and horizontal quenched tune glue the temperature of still, vertical vacuum knockout tower true
Reciprocal of duty cycle is 250pa~150Pa, and it is 150Pa~50Pa that horizontal quenched tune glues the vacuum of still, quenched tune is adhesive-assembly put in stop time
Between be 30min~120min.As preferably, the vacuum of vertical vacuum knockout tower is 200pa~185Pa, and horizontal quenched tune glues
The vacuum of still is 100Pa~60Pa, quenched tune is adhesive-assembly put in the time of staying be 60min~90min.
As improving further, described raw material is become foam material by Waste Polyester textile.As further improving, method bag
Include following in step: Waste Polyester textile carries out sorting, enters after broken or cutting the foam material machine of high speed rotating, foam material machine
Temperature is 150~170 DEG C, through stirring, the mixing of 3min~6min, adds appropriate water and drastically lowers the temperature and make its molding, thus
Prepare foam material.
As preferably, described Waste Polyester textile selects polyester-containing textiles leftover pieces, Waste Polyester clothing, non-woven polyester system
The mixing of one or more in product.
For the viscosity differences of viscosity, aberration difference etc. between homogeneous raw material impurity content difference, batch as far as possible, raw material exists
Use in the demand needing to meet continuous and stable production through allotment.As improving further, described raw material≤-
Under the conditions of 0.96MPa vacuum and temperature 145 DEG C ± 5 DEG C, Rotary drying 8h~10h, the most aqueous≤120PPm put into Screw Extrusion
Machine.
The present invention is from screw extruder melt out because of 2,2'-ethylenedioxybis(ethanol). effect, and the viscosity of melt is compared with the direct melt viscosity of foam material
Having the viscosity drop of 0.05dl/g~0.15dl/g, the melt final viscosity after alcoholysis is less than 0.50dl/g.Foam material relatively is direct
The viscosity of melted more than the 0.54dl/g obtained, being greatly enhanced of the mobility of melt.When melt is through filter
Time filtered due to the mechanical admixture in preferable fluidity of molten melt, filter also acts as good immixture simultaneously,
While filtering, alcoholysis degree is further.During by the speed scalable melt stop in melt pipe that adjusts screw rod
Between, the time that generally changes is 10min~25min.
After the melt of alcoholysis, enter that quenched tune is adhesive-assembly to be put, under vacuum, low molecule position that alcoholysis produces,
The lower-molecular substances such as the dyestuff that contains in foam material self, slurry, oil preparation are waved the most together and are taken off, and the degree of purity of melt obtains into one
The raising of step.The appropriate functional group (hydroxyl, carboxyl) that alcoholysis stage produces simultaneously is also less than the vacuum condition of 500Pa in vacuum
Lower beginning polycondensation, by regulation quenched tune is adhesive-assembly put in vertical vacuum separation still and horizontal quenched tune glue still adjustable melt at this
The time of staying in stage, generally this process continue 30min~120min.By above-mentioned technique and flow process, finally obtain Gao Pin
The spinning melt of matter.
Due to the fact that and have employed above-mentioned technical scheme, the method is by mixing a small amount of 2,2'-ethylenedioxybis(ethanol). in the melt, real
The existing polyester quick micro-alcoholysis under high temperature, high pressure, opens moieties chain in polyester fondant, discharges the functional group of part,
For in the adhesive-assembly functional group putting lower realization polycondensation again offer necessity of the quenched tune of liquid phase.By melt under the same conditions after micro-alcoholysis
Intrinsic viscosity have the raising of 0.05~0.12, reach or close to polyester slice intrinsic viscosity after melted.
The profitable effect of the present invention is the following aspects:
1) energy-saving and cost-reducing: the method is by adding 2,2'-ethylenedioxybis(ethanol)., and after the viscosity of melt reduces, melt flowability obtains very
Big improvement, mechanical admixture in melt filter more thoroughly, filter use cycle stretch-out more than 1.5 times, the adding of screw rod
Thermal power and power of motor reduce more than 15%, have saved substantial amounts of energy consumption.
2) lower-molecular substance evaporated during the quenched tune of liquid phase is viscous and the 2,2'-ethylenedioxybis(ethanol). of a small amount of residual have well
Mobility, solves pipeline between cyclone separator pipeline and the reactor that conventional foam material occurs during quenched tune is viscous and easily blocks up
Plug and the problem of the easy coking of steam jet pump condenser.
3) primary quality measure of the melt obtained: intrinsic viscosity 0.635dl/g~0.685dl/g, viscosity reaches fiber
The level of grade pet chip.
4) the method the most effectively eliminates in melt the impurity such as the part pigment of residual, slurry, plasticizer to the most in addition
The impact of whole melt quality.
Detailed description of the invention:
Below by the 2,2'-ethylenedioxybis(ethanol). alcoholysis Waste Polyester textile profit to the present invention of the specific embodiment under different technology conditions
The method preparing high-quality fusant by micro-alcoholysis technology is further described.In following example, quenched tune is adhesive-assembly is set to vertical crouching
United reactor device.
Embodiment 1:
In certain vacuum (≤-0.96MPa) and temperature after foam material is compounded well according to impurity content, color, viscosity differences etc.
Under the conditions of degree (145 DEG C ± 5 DEG C), Rotary drying 9h, final aqueous 90PPm put into spinning feed bin.The speed of regulation 2,2'-ethylenedioxybis(ethanol). pump makes
Mass fraction is foam material the 4% of its 2,2'-ethylenedioxybis(ethanol). measured, screw feed amount 1t/h, spiral shell one district is followed successively by ten district's temperature
280 DEG C, 285 DEG C, 295 DEG C, 295 DEG C, 295 DEG C, 290 DEG C, 290 DEG C, 285 DEG C, 285 DEG C, 285 DEG C, filter temperature 285 DEG C,
The melt time of staying in screw rod, filter and pipeline is 16min.Enter the quenched tune of liquid phase and glue setup time 75min altogether, vertical
The vacuum of formula still and horizontal retort is respectively 200pa~185Pa and 100Pa~60Pa, and still temperature is 285 DEG C.Close at raw material
In the case of continuous service 48 hours, conclusion such as table 1 below:
Conventional and the micro-alcoholysis Data Comparison of table 1 is relatively
Embodiment 2:
In certain vacuum (≤-0.96MPa) and temperature after foam material is compounded well according to impurity content, color, viscosity differences etc.
Under the conditions of degree (145 DEG C ± 5 DEG C), Rotary drying 8.5h, 105PPm put into spinning feed bin.The speed of regulation 2,2'-ethylenedioxybis(ethanol). pump makes it count
The mass fraction of the 2,2'-ethylenedioxybis(ethanol). measured is the 5% of foam material, screw feed amount 0.8t/h, and spiral shell one district is followed successively by 280 to ten district's temperature
DEG C, 285 DEG C, 295 DEG C, 295 DEG C, 295 DEG C, 290 DEG C, 290 DEG C, 285 DEG C, 280 DEG C, 280 DEG C, filter temperature 285 DEG C, melt
The time of staying in screw rod, filter and pipeline is 20min.Enter the quenched tune of liquid phase and glue setup time 90min, vertical retort altogether
Being respectively 200pa~185Pa and 100Pa~60Pa with the vacuum of horizontal retort, still temperature is 280 DEG C.In the situation that raw material is close
Lower continuous service 48 hours, conclusion such as table 2 below:
Conventional and the micro-alcoholysis Data Comparison of table 2 is relatively
Claims (10)
1. the method that 2,2'-ethylenedioxybis(ethanol). alcoholysis Waste Polyester textile preparation height joins quality melt, it is characterised in that: the method adds at raw material
Enter raw materials quality 1 ~ 8% 2,2'-ethylenedioxybis(ethanol). and enter screw extruder blended melting extrusion, the melt viscosity of screw extruder melt out
Being 0.40 ~ 0.50dl/g, then material enters that quenched tune is adhesive-assembly puts, and the melt viscosity of the adhesive-assembly melt putting out of quenched tune is
0.620dl/g~0.685dl/g.
The method that 2,2'-ethylenedioxybis(ethanol). alcoholysis Waste Polyester textile the most according to claim 1 preparation height joins quality melt, its feature
It is: the addition of 2,2'-ethylenedioxybis(ethanol). is the 3 ~ 6% of raw materials quality.
The method that 2,2'-ethylenedioxybis(ethanol). alcoholysis Waste Polyester textile the most according to claim 1 and 2 preparation height joins quality melt, it is special
Levy and be: the temperature of screw extruder 280 ~ 300 DEG C, be 10 ~ 20min in the time of staying of screw extruder.
The method that 2,2'-ethylenedioxybis(ethanol). alcoholysis Waste Polyester textile the most according to claim 3 preparation height joins quality melt, its feature
Be: screw extruder Luo mono-district to ten district's temperature be followed successively by 280 DEG C, 285 DEG C, 295 DEG C, 295 DEG C, 295 DEG C, 290 DEG C,
290℃、285℃、285℃、285℃。
The method that 2,2'-ethylenedioxybis(ethanol). alcoholysis Waste Polyester textile the most according to claim 1 preparation height joins quality melt, its feature
It is: screw extruder melt out first passes through filter and enters back into that quenched tune is adhesive-assembly to be put, the temperature 280 ~ 290 of filter
℃。
The method that 2,2'-ethylenedioxybis(ethanol). alcoholysis Waste Polyester textile the most according to claim 1 and 2 preparation height joins quality melt, it is special
Levy and be: adhesive-assembly the putting of quenched tune includes that interconnective vertical vacuum separating still and horizontal quenched tune glue still, and vertical vacuum separates
From top to bottom being provided with multi-layer porous plate in tower, the bottom that horizontal quenched tune glues still is provided with augering screw, and vertical vacuum separates
It is 280 ~ 290 DEG C that tower and horizontal quenched tune glue the temperature of still, and the vacuum of vertical vacuum knockout tower is 250pa~150Pa, horizontal
It is 150Pa~50Pa that quenched tune glues the vacuum of still, quenched tune is adhesive-assembly put in the time of staying be 30min ~ 120min;As excellent
Choosing, the vacuum of vertical vacuum knockout tower is 200pa~185Pa, and it is 100Pa~60Pa that horizontal quenched tune glues the vacuum of still,
Quenched tune is adhesive-assembly put in the time of staying be 60min~90min.
The method that 2,2'-ethylenedioxybis(ethanol). alcoholysis Waste Polyester textile the most according to claim 1 preparation height joins quality melt, its feature
It is: one or more in polyester-containing textiles leftover pieces, Waste Polyester clothing, non-woven polyester goods selected by Waste Polyester textile
Mixing.
8. prepare, according to the 2,2'-ethylenedioxybis(ethanol). alcoholysis Waste Polyester textile described in claim 1 or 2 or 7, the method that height joins quality melt,
It is characterized in that: raw material is become foam material by Waste Polyester textile.
The method that 2,2'-ethylenedioxybis(ethanol). alcoholysis Waste Polyester textile the most according to claim 8 preparation height joins quality melt, its feature
It being: Waste Polyester textile carries out sorting, enters after broken or cutting the foam material machine of high speed rotating, foam material machine temperature is 150 ~
170 DEG C, through stirring, the mixing of 3min~6min, add appropriate water and drastically lower the temperature and make its molding, thus prepare foam material.
The method that 2,2'-ethylenedioxybis(ethanol). alcoholysis Waste Polyester textile the most according to claim 8 preparation height joins quality melt, its feature
It is: Rotary drying 8h~10h under the conditions of≤-0.96MPa vacuum and temperature 145 DEG C ± 5 DEG C made after foam material by raw material, finally
Aqueous≤120PPm puts into screw extruder.
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Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102093590A (en) * | 2010-12-01 | 2011-06-15 | 宁波大发化纤有限公司 | Waste plastic conditioning and viscosity modifying system |
CN102532815A (en) * | 2011-12-06 | 2012-07-04 | 上海聚友化工有限公司 | Method for recycling waste polyester textiles |
-
2016
- 2016-08-15 CN CN201610671823.6A patent/CN106279758A/en active Pending
Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102093590A (en) * | 2010-12-01 | 2011-06-15 | 宁波大发化纤有限公司 | Waste plastic conditioning and viscosity modifying system |
CN102532815A (en) * | 2011-12-06 | 2012-07-04 | 上海聚友化工有限公司 | Method for recycling waste polyester textiles |
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