CN101659757A - Method for preparing medium-viscosity PET slice by recycled low-viscosity polyester yarn - Google Patents
Method for preparing medium-viscosity PET slice by recycled low-viscosity polyester yarn Download PDFInfo
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- CN101659757A CN101659757A CN200910196653A CN200910196653A CN101659757A CN 101659757 A CN101659757 A CN 101659757A CN 200910196653 A CN200910196653 A CN 200910196653A CN 200910196653 A CN200910196653 A CN 200910196653A CN 101659757 A CN101659757 A CN 101659757A
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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
- 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
Abstract
The invention provides a method for preparing a medium-viscosity PET slice through adding a viscosified chain extender during the process that a double-screw extruder smelts and extrudes recycled low-viscosity polyester fiber or polyester fabric fragments to carry out smelting, chain extension and extrusion reaction. The method enables the viscosity of PET to be enhanced through the following steps: taking the recycled low-viscosity terylene fiber or the polyester fabric fragments as a raw material, adding the viscosified chain extender, enabling the raw material and the chain extender to react in the extruder, and then extruding the reaction products to increase the viscosity of the PET. Through changing processing conditions and reaction proportion, the PET slices with different viscosity can be obtained. The products obtained by the invention can be used for industrial yarns, such as carpets, filature and the like and can serve as the raw materials of textile fabrics.
Description
Technical field
The present invention relates to process the method that obtains medium-viscosity PET section to reclaiming low viscosity polyster fibre or polyester piece good fragment, react the method for extruding its intrinsic viscosity of raising after specifically utilizing twin screw extruder that the low viscosity polyster fibre of handling through densification or pulverize the back is added the tackify chainextender, can be used for producing medium-high viscosity PET spinning chips.The densification processing of herein mentioning refers to and makes the surface thawing agglomerating in the heating through cleaning and certain temperature the PET after reclaiming, and forms the spheroid of 2~20mm, is convenient to accurately feed in raw material and improve output.
Background technology
PET (polyethylene terephthalate, be commonly called as terylene) since nineteen fifty-three is realized industrialization by E.I.Du Pont Company, because the cost that its good Physical Processing performance and big suitability for industrialized production are brought reduces the superiority of effectiveness that is embodied, other kind that has replaced many man-made fiber rapidly, the present gang that has become output maximum in the synthon.Since two thousand three, the production capacity of global PET is expanded with average annual about 9% speed, and 2005 annual capacities have reached about more than 4,000 ten thousand tons, and the production capacity of China in 2008 surpasses 2,000 ten thousand tons, has become PET world production, consumption first big country.
At present, the main use of PET is aspect fiber and beverage packets bottling in the world, particularly in the last few years, the PET bottle blows pull technology, PET hot filling, inferior hot filling technology, and the cold aseptic filling technology of the PET of current trend, all promoted the flourish of global PET bottled drink, the use proportion of PET on the bottle material rises rapidly.According to statistics, world PET goods output was 4091.7 ten thousand t in 2005, and wherein packing bottle for beverage resin 1106.3 ten thousand t account for 27.0%.And PET has the performance that can process repeatedly as thermoplastics, so a lot of research institution is devoted in the recycling of PET bottle always.
When PET uses (wherein major part is to use as the PET beverage bottle) as wrapping material, it is shorter to recycle the time, and too big variation can not take place its performance, and the PET bottle sheet intrinsic viscosity after general the recovery still can reach 0.7, therefore after cleaning is selected, can directly carry out secondary and use.
Because the good heat resistance of PET can use under up to 120 ℃ environment.When the PET melt-spinning used as fiber, it is high 3 times that its strength ratio wool is wanted, and elasticity is then better near wool and crease resistance, and wear resistance also is only second to polyamide fibre, is most widely used a kind of in the fiber.2007 China's polyster fibre cumulative productions reach 1,900 ten thousand tons (comprising the PET section of partially recycled back second stage employ), increase by 18.45% than 2006.But because PET uses as polyster fibre, grow (generally all being higher than 18 months) duration of service, is exposed to slowly oxidative degradation of quilt in the air, and molecular weight seriously reduces, and performance also reduces a lot, and the fiber through reclaiming is directly melt-spinning use usually.Therefore can only discard, or after modification, improve its intrinsic viscosity and reuse.
Current, the recovery method to PET mainly contains following several both at home and abroad:
1. " bottle to bottle " technology
The regeneration of bottle to bottle is meant the section that PET bottle sheet is converted to food grade, and this food grade section can substitute virgin material and direct and Food Contact.This method has realized the conversion between the Waste recovery high value material, has also realized the environmental protection of production and the comprehensive utilization of resource.
2. chemical recovery technology
The chemical recovery technology is that recovery PET is resolved into monomer, and resynthesis can be used for the process engineering for regenerating of beverage bottle.Chemical recycling mainly contains hydrolysis, alcoholysis and sugared solution etc.Alcoholysis and sugared solution are the degradation method of comparative maturity.But because chemical decomposition process needs big energy, energy consumption is bigger, and the three wastes are more to serious environment pollution, and this method can't be used on a large scale.
3. regeneration and granulation
Intrinsic viscosity after cleaning separation is higher than the PET pulverizing material of 0.6dL/g can make fiber as pillow, cotton-padded mattress, sleeping bag, felt etc. through melt-spinning after the forcing machine extruding pelletization is made section.Also can strengthen with glass, the regenerative PET material of manufacturing has better heat-resisting and mechanical strength, can be used to make automobile component and electrical apparatus insulation material.Perhaps the regenerative PET material can with other polymer blendings, make various modifying material, be with a wide range of applications.
4. tackify chain extension granulation
General polyster fibre or the polyester piece good fragment intrinsic viscosity that reclaims all is lower than 0.5, can't be used as melt-spun material, can only use through behind the tackify chain extension.The intrinsic viscosity of PET section can reach 0.65 even higher behind the tackify chain extension, can directly be used in the melt-spinning aspect or uses as common plastics with the other materials blend.
The most frequently used in the above method is the regeneration and granulation method, and the intensity of the POLYESTER YARNS after second melting processing obviously reduces, and can't directly utilize once more after the recovery.For example, limiting viscosity be the raw material of 0.6~0.7dL/g after melt-processed again, intrinsic viscosity can be reduced to 0.4-0.5dL/g.The PET intrinsic viscosity that reclaims often is reduced between the 0.3-0.6dL/g, can't directly be used as spinning, must carry out just can using behind the tackify again.The tackify method mainly contains following two kinds:
The simple blend method
The simple blend method is the PET melt blending with low viscous PET and middle and high viscosity, to improve the overall characteristic viscosity number of processing PET, reaches service requirements.
Chemistry tackify method
Chemistry tackify method is that low viscous PET is made the polymer molecule chainpropagation behind chemical reaction, reaches the purpose that improves intrinsic viscosity.Chemical method is divided into condensed type and add-on type two classes.Condensed type is meant that adding certain catalyzer under high temperature fused state makes the molecular chain end group that dehydration condensation take place again; Because the end group of PET includes carboxyl and hydroxyl, add-on type adds the tackify chainextender that contains polynary (binary or more than) active group exactly, and the PET molecular chain is coupled together by chemical reaction, reaches the purpose that increases the PET molecular weight.
At present the many tackify chainextenders of research have types such as epoxies, anhydrides, isocyanates, bisoxazoline class and two kinds and the coupling of above tackify chainextender.Wherein the chemical molecular formula of isocyanates, bisoxazoline class tackify chainextender and epoxies tackify chainextender is as follows:
Diisocyanates: O=C=N-R-N=C=O
PET fiber recovery amount is huge in the existing market, but because lower, the intensity difference of viscosity, can not be directly as normal spinning material, use after can only mixing High Viscosity PET.But this method has reduced the marketable value of High Viscosity PET.Melt extrude material through promptly can be used as behind the adding chainextender tackify chain extension, improved the value of PET.Therefore the polyster fibre or the polyester piece good fragment that reclaim, centre are mingled with other impurity can not be used as food grade materials, but still has been widely used.As following purposes is arranged at field of textiles:
The regenerative PET non-woven fabrics, industrialized at present product is mainly spunbond PET non-woven fabrics, PET melt spraying non-woven fabrics etc.It can be used for filtering, and makes absorption agent and campsite facility etc.
The length POLYESTER YARNS is sprayed silk with the PET section that processes through the high temperature extruding, can be made into long and short different fiber, is used for clothes manufacturing, packing material, carpet weaving etc.Bundling belt can also be extruded,, steel band can be replaced because of having very high toughness.
Also after fillers such as glass fibre strengthen, its injection member can be used for automobile, household electrical appliance, electric switch etc. in addition.Can also obtain engineering materials with the other materials blend.
Summary of the invention
The objective of the invention is that lower (0.3~0.5dL/g) polyster fibre that can't directly use or polyester piece good fragment carry out the tackify chain extension to reclaiming the back intrinsic viscosity, the intrinsic viscosity that the PET of different viscosity can be extruded the PET section that makes after the processing is increased to 0.6-1.0dL/g, to reach the processing request that can carry out melt-spinning.
The present invention mentions low viscosity polyster fibre or the polyester piece good fragment that PET is mainly recovery, but also can be used for reclaiming other PET materials such as PET bottle sheet.Working method is handled for earlier the PET that reclaims being carried out densification in special processing unit (plant), manufactures behind particulate state or the dusty raw materials oven dry back that dewaters and uses.The tackify chainextender is mainly polyfunctional group class materials such as bisoxazoline class, epoxy resin and diisocyanates, wherein diisocyanates can with hydroxyl reaction , bisoxazoline class among the PET can with the end carboxyl reaction among the PET.In order to adapt to the conditional request of PET extrusion reaction, also can change the wherein chemically reactive of some tackify chainextender with the method for the tackify chainextender being carried out modification, improve the mechanical property of extruding the PET section simultaneously.Can reach 1.2dL/g by the intrinsic viscosity of extruding PET section behind the chain extension tackify.
The implementation process of aforesaid method is specific as follows: low intrinsic viscosity polyster fibre that will reclaim or polyester piece good fragment clean through sorting and carry out pulverizing granulating, powdery with pulverizer after densification is handled, and also can only directly enter next step through the sorting cleaning step.Reclaim raw material through after the first step again under 110 ℃ of-160 ℃ of conditions drying dewater.Then exsiccant PET raw material and tackify chainextender are joined and carry out melting mixing in the twin screw extruder and extrude pelletizing, make the PET section of medium viscosity.In melt extruding process, can respectively distinguish temperature acquisition different qualities viscosity number PET section by setting the PET and the ratio of tackify chainextender, the screw speed of regulating forcing machine, the adjustment forcing machine that drop into forcing machine.
Wherein twin screw extruder is respectively distinguished temperature between 100 ℃-300 ℃, and the extruder screw rotating speed is between 70-250 changes.The intrinsic viscosity that melt extrudes back PET can be increased to predetermined value, and by the water-bath cooling, the PET section of melting spinning is made in pelletizing.
The present invention has the following advantages:
The polyester piece good fragment of low intrinsic viscosity can be processed into the PET spinning chips of higher intrinsic viscosity, can be as required by regulating feed ratio, extruding the PET section that processing conditions (screw speed, barrel temperature etc.) promptly can be made into the different qualities viscosity number.And working method does not simply need to process repeatedly, and this method also can be continuously produced, and section performance virgin material is close.
Embodiment
Now in conjunction with specific embodiments content of the present invention is described in detail.
Embodiment 1
To reclaim low viscosity polyster fibre or polyester piece good fragment PET material and be positioned over 160 ℃ of convection oven inner dryings after 4 hours, and wait in the adding forcing machine hopper and extruding through classification, cleaning.Modification MDI (containing the 28wt% isocyano) and dried PET added in the forcing machine with 1: 100 mass ratio melt extrude.The tackify chainextender utilizes the volume pump accurate measurement to add.Each section of barrel temperature is in the extrusion:
PET after the chain extension tackify is extruded cools off in cooling trough after the dicing machine pelletizing obtains the sample of cutting into slices.Test back result is: intrinsic viscosity is increased to 0.65dL/g by the 0.4dL/g of raw material.
Embodiment 2
In MDI, add polyoxyethylene glycol-500, still be the tackify chainextender of isocyano for the polyoxyethylene glycol two ends in the middle of making.The back processes according to embodiment 1 condition, and the intrinsic viscosity of PET section is increased to 0.6dL/g by 0.4dL/g behind the acquisition tackify chain extension.
Embodiment 3
To reclaim low viscosity polyster fibre or polyester piece good fragment PET material and obtain PET raw material particle after densification is handled through cleaning, put into 130 ℃ of convection oven after dry 12 hours, the modification MDI that will contain the 18wt% isocyano adds in the forcing machine with 1.2% of PET feeding quantity through volume pump.Each section of barrel temperature is in the extrusion:
Extrude after pelletizing after the water cooling, after tested, intrinsic viscosity is increased to 0.85dL/g by the 0.64dL/g of raw material, and testing other performances has
Embodiment 4
To reclaim the low viscosity polyster fibre is positioned over 160 ℃ of convection oven inner dryings and puts into hopper after 4 hours and wait to extrude through classification, after cleaning.Melt extrude working method and extrude according to the described method of embodiment 2 methods, the ingredient proportion that only changes tackify chainextender MDI (18wt% isocyanate group) and PET is 3: 100.Record the PET intrinsic viscosity after the cooling and dicing and be increased to 1.12dL/g by 0.64dL/g.Other performance and raw material contrast have following table:
Embodiment 5
To reclaim low viscosity polyster fibre or polyester piece good fragment is positioned over 130 ℃ of convection oven inner dryings and puts into 40 ℃ of vacuum drying ovens after 12 hours and vacuumize and make its cooling through classification, after cleaning.Bisoxazoline and dried PET added in the forcing machine with 0.8: 100 mass ratio melt extrude.Extrusion condition such as following table:
After the cooling tank cooling, pelletizing obtains section.PET is increased to 0.6dL/g by 0.4dL/g after measuring.
Embodiment 6
To reclaim low viscosity polyster fibre or polyester piece good fragment PET material and obtain PET raw material particle after densification is handled, put into 130 ℃ of convection oven dry 12 hours through cleaning.1,3 benzene ,-bisoxazolines and dried PET added in the forcing machine with 1: 100 mass ratio melt extrude.Extrusion condition is identical with embodiment 4, obtains the PET section through the cooling tank cooling and dicing.Measure back PET and be increased to 0.75dL/g behind the tackify chain extension by the 0.4dL/g of raw material.
Embodiment 7
To reclaim low viscosity polyster fibre or polyester piece good fragment PET material and obtain PET raw material particle after densification is handled, put into 130 ℃ of convection oven dry 12 hours through cleaning.Dried PET add-on: bisoxazoline add-on: the pyromellitic dianhydride add-on is 100: 0.4: 0.5, and wherein two kinds of chainextender bisoxazolines and pyromellitic dianhydride add in the forcing machine respectively.Other conditions are identical with example 5, obtain the PET section through cooling and dicing.Test has the PET intrinsic viscosity to be increased to 0.65dL/g by 0.4dL/g.
Embodiment 8
To reclaim low viscosity polyster fibre or polyester piece good fragment PET material and obtain PET raw material particle after densification is handled, put into 130 ℃ of convection oven dry 12 hours through cleaning.Resins, epoxy and dried PET added in the forcing machine with 2: 100 mass ratio melt extrude.Extrusion condition is identical with embodiment 4, obtains the PET section through the cooling tank cooling and dicing.After tested, intrinsic viscosity is increased to 0.66dL/g by 0.4dL/g, and the breaking tenacity of measuring fiber behind the melt-spinning is increased to more than the 2.0cN/dtex by 1.0cN/dtex, after measured the performance such as the following table of PET section behind the tackify chain extension:
Claims (10)
- It is 1, a kind of that (intrinsic viscosity is a raw material from 0.35~0.5dl/g) with reclaiming polyster fibre or reclaiming the polyester piece good fragment, be metered into the tackify chainextender and become the section that can be used for spinning through the twin screw extruder melting mixing, after extruding, cool off slivering, pelletizing, the intrinsic viscosity of this section can be increased to 0.6-1.0dl/g from 0.35~0.5dl/g, can be used as raw materials such as carpet, rope, line, garment material.The weight ratio of wherein extruding PET and tackify chainextender is 100: 0.5~10.
- 2, according to claim 1, raw material is mainly the recovery polyster fibre of handling through densification after the recovery or reclaims the polyester piece good fragment.
- 3, according to claim 1, raw material can be higher than 2.0cN/dtex through the tackify chain extension fibre breakage intensity that obtains that obtains cutting into slices behind melt-spinning.
- 4, as described in the claim 1,2, the intrinsic viscosity of the polyster fibre of recovery or polyester piece good fragment is lower, even can not be directly used in and melt extrude spinning.
- 5, according to claim 1, the tackify chainextender of adding has types such as epoxies, anhydrides, diisocyanates, bisoxazoline class and two kinds and the coupling of above tackify chainextender.Wherein diisocyanates tackify chainextender main with PET in hydroxyl reaction chain extension tackify, the raising molecular weight; The bisoxazoline class then with PET in carboxyl reaction, improve molecular weight.
- 6, as described in the claim 1,4, can carry out modification, change the chemically reactive of tackify chainextender, thereby better control and regulate prepared section performance, and can adjust the extrusion process required time the tackify chainextender
- 7, as described in the claim 1,4, can regulate PET residence time in extruder barrel by screw speed, generally setting the residence time is 1~5min.
- 8, according to claim 1, the tackify chainextender adds forcing machine by measuring apparatus, and fully fusion, mixing, reaction in forcing machine.
- 9, according to claim 1, the extruder barrel temperature controlling range is between 190 ℃-290 ℃.
- 10, according to claim 1, extrude the PET section that obtains behind the chain extension tackify and be mainly used in the extruding spinning material, as carpet silk, non-woven fabrics, rope, line, garment material, also can carry out melt blending and be used for injection moulding processing, make automobile, household electrical appliance, electric switch etc. with other materials.
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CN102120868A (en) * | 2011-04-08 | 2011-07-13 | 扬州三星塑胶有限公司 | Toughening process for high-tensile-strength recycled polyester sheet |
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