CN1324084C - PA/PET high molecule alloy material - Google Patents
PA/PET high molecule alloy material Download PDFInfo
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- CN1324084C CN1324084C CNB2005100303255A CN200510030325A CN1324084C CN 1324084 C CN1324084 C CN 1324084C CN B2005100303255 A CNB2005100303255 A CN B2005100303255A CN 200510030325 A CN200510030325 A CN 200510030325A CN 1324084 C CN1324084 C CN 1324084C
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- 239000000956 alloy Substances 0.000 title claims abstract description 18
- 239000000463 material Substances 0.000 claims abstract description 17
- 239000004677 Nylon Substances 0.000 claims abstract description 7
- 229920001778 nylon Polymers 0.000 claims abstract description 7
- 229920000139 polyethylene terephthalate Polymers 0.000 claims description 54
- 239000003112 inhibitor Substances 0.000 claims description 13
- 230000003647 oxidation Effects 0.000 claims description 13
- 238000007254 oxidation reaction Methods 0.000 claims description 13
- 239000004970 Chain extender Substances 0.000 claims description 9
- 239000012752 auxiliary agent Substances 0.000 claims description 9
- 235000013361 beverage Nutrition 0.000 claims description 8
- 238000011084 recovery Methods 0.000 claims description 7
- GHKOFFNLGXMVNJ-UHFFFAOYSA-N Didodecyl thiobispropanoate Chemical compound CCCCCCCCCCCCOC(=O)CCSCCC(=O)OCCCCCCCCCCCC GHKOFFNLGXMVNJ-UHFFFAOYSA-N 0.000 claims description 4
- 238000005984 hydrogenation reaction Methods 0.000 claims description 4
- ZUOUZKKEUPVFJK-UHFFFAOYSA-N phenylbenzene Natural products C1=CC=CC=C1C1=CC=CC=C1 ZUOUZKKEUPVFJK-UHFFFAOYSA-N 0.000 claims description 3
- 235000010290 biphenyl Nutrition 0.000 claims description 2
- 150000002148 esters Chemical class 0.000 claims description 2
- HZVOZRGWRWCICA-UHFFFAOYSA-N methanediyl Chemical compound [CH2] HZVOZRGWRWCICA-UHFFFAOYSA-N 0.000 claims description 2
- FACXGONDLDSNOE-UHFFFAOYSA-N buta-1,3-diene;styrene Chemical compound C=CC=C.C=CC1=CC=CC=C1.C=CC1=CC=CC=C1 FACXGONDLDSNOE-UHFFFAOYSA-N 0.000 claims 2
- 229920000468 styrene butadiene styrene block copolymer Polymers 0.000 claims 2
- 125000006267 biphenyl group Chemical group 0.000 claims 1
- 229920001935 styrene-ethylene-butadiene-styrene Polymers 0.000 claims 1
- 229920006351 engineering plastic Polymers 0.000 abstract description 14
- 238000012545 processing Methods 0.000 abstract description 8
- 238000005516 engineering process Methods 0.000 abstract description 5
- 239000002994 raw material Substances 0.000 abstract description 5
- 229920003023 plastic Polymers 0.000 abstract description 4
- 239000004033 plastic Substances 0.000 abstract description 4
- 229920000642 polymer Polymers 0.000 abstract description 4
- 229910045601 alloy Inorganic materials 0.000 abstract description 3
- 238000001125 extrusion Methods 0.000 abstract description 3
- 239000002184 metal Substances 0.000 abstract description 3
- 230000003014 reinforcing effect Effects 0.000 abstract description 3
- 230000001105 regulatory effect Effects 0.000 abstract description 2
- 239000012634 fragment Substances 0.000 abstract 1
- 239000005020 polyethylene terephthalate Substances 0.000 description 44
- 238000000034 method Methods 0.000 description 12
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 5
- 238000001035 drying Methods 0.000 description 5
- 238000001746 injection moulding Methods 0.000 description 5
- 238000001291 vacuum drying Methods 0.000 description 5
- 238000002347 injection Methods 0.000 description 4
- 239000007924 injection Substances 0.000 description 4
- 230000035939 shock Effects 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 239000002699 waste material Substances 0.000 description 4
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 230000018109 developmental process Effects 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- KAKZBPTYRLMSJV-UHFFFAOYSA-N Butadiene Chemical compound C=CC=C KAKZBPTYRLMSJV-UHFFFAOYSA-N 0.000 description 2
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 description 2
- 239000002250 absorbent Substances 0.000 description 2
- 238000005452 bending Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000005336 cracking Methods 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 238000005469 granulation Methods 0.000 description 2
- 230000003179 granulation Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000005453 pelletization Methods 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 230000008929 regeneration Effects 0.000 description 2
- 238000011069 regeneration method Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000009987 spinning Methods 0.000 description 2
- 230000006641 stabilisation Effects 0.000 description 2
- 238000011105 stabilization Methods 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
- 239000005977 Ethylene Substances 0.000 description 1
- 239000004831 Hot glue Substances 0.000 description 1
- 229910001125 Pa alloy Inorganic materials 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- -1 Polyethylene terephthalate Polymers 0.000 description 1
- 208000037656 Respiratory Sounds Diseases 0.000 description 1
- 208000013201 Stress fracture Diseases 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000004378 air conditioning Methods 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 150000004982 aromatic amines Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- ZZVUWRFHKOJYTH-UHFFFAOYSA-N diphenhydramine Chemical group C=1C=CC=CC=1C(OCCN(C)C)C1=CC=CC=C1 ZZVUWRFHKOJYTH-UHFFFAOYSA-N 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 238000013467 fragmentation Methods 0.000 description 1
- 238000006062 fragmentation reaction Methods 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000008188 pellet Substances 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 238000004080 punching Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000001172 regenerating effect Effects 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 230000011218 segmentation Effects 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 230000003019 stabilising effect Effects 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 125000000383 tetramethylene group Chemical group [H]C([H])([*:1])C([H])([H])C([H])([H])C([H])([H])[*:2] 0.000 description 1
- 229920000428 triblock copolymer Polymers 0.000 description 1
- 229920006337 unsaturated polyester resin Polymers 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
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Abstract
The present invention discloses an engineering plastic which has super plasticity, super toughness, low cost and the characteristics of plastic strength, rubber extensibility, metal workability, etc. The present invention takes recovered PET bottle fragments and nylon plastics as main raw materials, and obtains polymer alloy which has excellent processing plasticity and the mechanical property of universal engineering plastics by particular extrusion processing technology. Simultaneously, the rigidity and the ductility of the present invention achieve balance in various states by regulating the component proportion of all reinforcing and plasticizing materials in order to satisfy various application requirements.
Description
Technical field
The present invention relates to a kind of super-toughness engineering plastic cheaply, relate in particular to a kind of to reclaim beverage bottle (main component: polyethylene terephtalate), PA (nylon), SEBS (styrene/ethylene/butadiene/styrene) multipolymer and other auxiliary agent etc. are toughness reinforcing and novel high polymer alloy material compatible components, belong to field of material preparation.
Background technology
At present, in world's pet container, have nearly 2/3 to be used in the drink pack aspect.Flourish along with drink industry, the application of PET bottle also more and more widely, consumption also increases sharply.What bring thus is the white pollution that a large amount of waste PET bottles bring, and from the angle of save energy and resource, protection environment, the recovery of waste PET bottle has crucial meaning.
Useless PET beverage bottle regeneration and utilization can reduce environmental pollution, and can turn waste into wealth, and create good economic benefit and social benefit.This problem has caused that countries in the world generally pay attention to, and has many scholars just being devoted to this research both at home and abroad.China PET beverage bottle consumption reaches 9.6 ten thousand tons/year at present, has only at present seldom partly to be utilized, and causes a large amount of wastes of resource and environmental pollution, and its reutilization technology has wide prospect.
PET beverage bottle recovery method has chemical recovery and physics to reclaim two kinds of methods.Chemical recycling is the depolymerization under certain reaction conditions of the useless bottle of PET to be generated the method that is worth chemical of utilizing is arranged.The physics absorption method is PET to be drunk section's bottle carry out process for granulating again through separation, fragmentation, washing and drying treatment.At present domesticly all be confined to behind the regeneration and granulation spinning or be cracked into low molecular compound for the research of reclaiming PET, as poly-and raw material or produce hot melt adhesive, coating and unsaturated polyester resin etc., wherein major part is used for spinning, as the lining of clothes etc.The high value utilization of a large amount of reclaimed materials is made slow progress, and for example the singulation or the like that becomes 3-tier architecture, reclaimed materials with new resin compounded all is difficult to apply owing to cost or technical reason.Therefore, the new relevant technologies of exploitation is imperative.
Polyethylene terephthalate (PET) is the polycondensate of terephthalic acid and ethylene glycol, is also referred to as polyester.Its averagemolecular wt amount is 20,000～30,000.It is a kind of high crystallinity polymer, and 260 ℃ of fusing points have excellent mechanical property, high impact and wearability, creep resistant, and the rigidity height, hardness is big, water-absorbent is little and dimensional stability is good.
Engineering plastics are one of research and development focuses that the non-fibre of PET enlivens with industry in the world today.PET has over-all propertieies such as high strength, high rigidity, good thermotolerance, good dimensional stability, chemical proofing as engineering plastics, is used widely in fields such as electronic and electric components, machinery, trolley parts.China's PET engineering plastics are new industries, almost are blank with PET production engineering plastics, and the main raw material of production engineering plastics still adopts PBT, however PBT engineering plastics cost height.Development along with Chinese national economy, domestic every profession and trade is very fast to the demand growth of engineering plastics, particularly automotive field has heavy demand to the excellent property engineering plastics, and China has abundant PET raw material, these development and use for the PET engineering plastics provide good development space.
Summary of the invention
The invention provides a kind of is main raw material(s) to reclaim PET bottle sheet, is aided with other toughness reinforcing and compatible components, extrudes the high polymer alloy of extraordinary toughness of having of preparation and plasticity by twin screw.
Design of the present invention is as follows:
PET is that crystallization velocity is too slow as the difficulty of plastic applications, can not adapt to general plastics forming technology, and shock strength also has much room for improvement.Nylon (PA) has the temperature use range of outstanding impelling strength, broadness, and product size is stable, is a kind of good comprehensive properties engineering plastics.But be easy to stress cracking, to the breach sensitivity, wear resistance is not good enough.Carry out blend with PET and PA, can improve the flowability of solvent resistance, stress cracking resistance and the improvement system of system, be convenient to the processing that is shaped.SEBS is that vinylbenzene (S)-ethene (E)/butylene (B)-vinylbenzene (S) constitutes segmented copolymer, and molecular configuration is the triblock copolymer of A-B-A type (-soft section-hard section of hard section), and its molecular formula is as follows:
SEBS is scattered between PET and the PA particle as the elastomerics particle, becomes the obstacle that microfracture increases, and can stop the tiny crack that forms under stress further to increase effectively, thereby the toughness of system improves greatly.Simultaneously, SEBS low melting point and low viscous characteristics can promote the cohesive action that PET and PC in the blend process two are alternate, thereby further improve the continuity in the extrusion process.
Technical scheme of the present invention is:
A kind of PA/PET high molecule alloy material, its spy is that its mass fraction proportioning of described high molecule alloy material is: PET: PA: SEBS=70～100: 22～50: 8～30; The add-on of chainextender MDI (benzhydryl vulcabond) is the 0-10% of total mass;
Above-mentioned SEBS is: hydrogenation degree＞80%, number-average molecular weight are 3-30 ten thousand, are provided by Japanese Kurary Co., Ltd., and commodity are called Septon8006;
Above-mentioned reactive chainextender is: its structural formula of MDI (phenylbenzene methylene radical isocyanic ester) is:
Hot procedure for nylon, the use of oxidation inhibitor is to its stabilization remarkable (add oxidation inhibitor whether DSC contrast experiment and see Fig. 1), but the stabilising effect that is used alone stablizer is not remarkable, and oxidation inhibitor (hindered phenol or aromatic amine) has stabilization preferably with the one package stabilizer of auxiliary antioxidant.
In the present invention, can add oxidation inhibitor and the antioxygen auxiliary agent of total mass 0-10%, the mass ratio of oxidation inhibitor and antioxygen auxiliary agent is: the mass ratio of oxidation inhibitor and antioxygen auxiliary agent is 10: 1,
Described oxidation inhibitor is AO-80 or DPN, and the antioxygen auxiliary agent is DLTP; Molecular formula is:
Described PET also can select for use recovery, be the sheet PET beverage bottle sheet of 2-8mm through crusher in crushing, its intrinsic viscosity η=0.65-1.10dl/g.
Described nylon (PA) is: PA6 or PA66, molecular weight are 2-6 ten thousand.
In addition, following material also can serve as the chainextender of PET, as:
O＝C＝N-(CH
2)
6-N＝C＝O
According to the characteristics of this system, the water-absorbent of nylon is strong, and the requirement to moisture content is high in the PET hot-work, so must be to all components is carried out sufficient drying.
Concrete complete processing is: reclaim PET bottle sheet and PA in drying plant 120 ℃ dry 4 hours down, extrude after drying, injection moulding after the water-cooled granulation after mixing by proportioning.Each section of forcing machine extrusion temperature is 60-240 ℃, and the injection moulding machine temperature is 260-280 ℃.Material preparation has made full use of the structure that PET bottle sheet forms in blowing processing, kept the rigidity and the intensity of engineering plastics, can realize big deformation after surrender again.Gordian technique wherein is to carry out the low temperature solid phase at 60-240 ℃ and extrude to handle and add chainextender and react reclaiming PET bottle sheet, allow to carry out the adjustment of the compound of component and prescription, these adjustment can be regulated the rigidity and the ductility of material, make material can satisfy the demand of different occasions.
Beneficial effect
This material can be bent to arbitrarily ± and 180 °, and keep distortion and do not rupture; Shock resistance is better, can at room temperature push, processing such as punching press, mold pressing.Its properties of materials is mainly reflected in:
(1) plasticity-is good: the forming process ratio is easier to, and the crystallization and the orientation form that can keep PET to form in the course of processing by common means such as injection moulding, hot pressing can be made complicated shape as requested.
(2) good mechanical performance such as shock-resistant can at room temperature be pushed, impact briquetting prepares products such as safety helmet, has simultaneously and low temperature ductility and cold plasticity like the metal species, can process with the metal method for processing.
(3) crooked ± 180 ° repeatedly foldingly do not rupture, hammering into nail does not have crackle, fastness is also suitable with timber.
(4) heat-drawn wire＞110 ℃, resistance to elevated temperatures is good.
The regenerative PET novel material can be widely used in automobile industry (safety lever, lamp socket, external decorative material and the interior bearing circle of car such as car door, parts such as panel board) respectively; Household electrical appliance (interior fittings of air conditioning machinery, electric fan, refrigerator, the housing of televisor, sound-track engraving apparatus and accessory); Office industry (shells of office equipment such as facsimile recorder, duplicating machine, computer, printer); Daily necessities industry (sanitary ware, toy, stationery) etc.
Description of drawings
Fig. 1 is the DSC spectrogram of PA/PET alloy.
Embodiment
Embodiment 1
Recovery PET beverage bottle cleans up after pulverizer is pulverized and is 2-8mm sheet size.Take by weighing and reclaim PET bottle sheet 9.500Kg, PA6:4.230Kg, SEBS:2.350Kg, PET and PA6 are in 100 ℃ of following removal moisture drying 4 hours, SEBS vacuum drying treatment.Dry back in high-speed mixer with specific order with above mixing of materials, addings MDI is a chainextender: 30 restrain, oxidation inhibitor (AO-80/DLTP=3/1): 25g.Material drops into the twin screw extruder feeding and carries out extruding pelletization after the high-speed mixer high speed is mixed 10 minutes.Each section of forcing machine temperature is set at:
| Hop count | 1 | 2 | 3 | 4 | 5 | 6 | 7 | |
| Temperature ℃ | ||||||||
| 100 | 100 | 100 | 100 | 200 | 240 | 240 | 240 |
The main-machine screw rotating speed is 200rpm, and the feeding rotating speed is 10rpm.Extrude pellet before injection in 100 ℃ of following vacuum-dryings 20 hours after injection molding.Injector segmentation temperature is set at:
| Hop count | 1 | 2 | 3 | 4 |
| Temperature ℃ | 230 | 220 | 220 | 210 |
Injection pressure is 9-15Mpa, 50 ℃ of mould temperature.Its The performance test results of injection moulding sample sees Table one.
Embodiment 2
Recovery PET beverage bottle cleans up after pulverizer is pulverized and is 2-8mm sheet size.Take by weighing and reclaim PET bottle sheet 7.200Kg, PA66:3.200Kg, SEBS:1.800Kg, PET and PA66 are in 100 ℃ of following vacuum-dryings 20 hours, SEBS vacuum drying treatment.Dry back with above mixing of materials, adds MDI chainextender 90 grams, oxidation inhibitor (DPN/DLTP=4/1): 20g in high-speed mixer.Material drops into the twin screw extruder feeding and carries out extruding pelletization after the high-speed mixer high speed is mixed 10 minutes.Each section of forcing machine temperature is set at
| Hop count | 1 | 2 | 3 | 4 | 5 | 6 | 7 | |
| Temperature ℃ | ||||||||
| 100 | 100 | 100 | 100 | 100 | 150 | 150 | 150 |
The main-machine screw rotating speed is 250rpm, and the feeding rotating speed is 12rpm.Extrude blend before injection in 100 ℃ of following vacuum-dryings 20 hours.Injecting each section temperature is
| Hop count | 1 | 2 | 3 | 4 |
| Temperature ℃ | 230 | 220 | 220 | 210 |
Injection pressure 9～15MPa, 40 ℃ of mould temperature.Its The performance test results sees Table one.
Table one PET/PA alloy mechanical property
| Mechanical property | System | PA6/PET | PA66/PET |
| Notch shock non-notch tensile impact intensity elongation at break stretch modulus bending strength bending modulus | (kJ/m 2) (kJ/m 2) (MPa) (％) (MPa) (MPa) (GPa) | 60 continuous 56 230 400 63 1.7 | 52 continuous 58 201 401 68 1.9 |
Claims (5)
1, a kind of PA/PET high molecule alloy material, it is characterized in that its mass fraction proportioning of described high molecule alloy material is: polyethylene terephtalate: nylon PA: hydrogenation three block styrene-butadiene-styrene copolymer SEBS=70～100: 22～50: 8～30;
The intrinsic viscosity η of above-mentioned PET=0.65-1.10dl/g,
Above-mentioned PA is: PA6 or PA66, molecular weight are 2-6 ten thousand,
Hydrogenation degree＞80% of above-mentioned hydrogenation three block styrene-butadiene-styrene copolymer, number-average molecular weight are 3-30 ten thousand.
2, PA/PET high molecule alloy material as claimed in claim 1 is characterized in that, described high molecule alloy material also contains and accounts for alloy material total mass 0-10% chainextender,
Described chainextender is a phenylbenzene methylene radical isocyanic ester, and its structural formula is:
3, PA/PET high molecule alloy material as claimed in claim 1 or 2, it is characterized in that, described high molecule alloy material also contains oxidation inhibitor and the antioxygen auxiliary agent that accounts for alloy material total mass 0-10%, and the mass ratio of oxidation inhibitor and antioxygen auxiliary agent is: the mass ratio of oxidation inhibitor and antioxygen auxiliary agent is 10: 1.
Described oxidation inhibitor is: AO-80 or DPN, antioxygen auxiliary agent: DLTP; Molecular formula is respectively:
4, PA/PET high molecule alloy material as claimed in claim 1 or 2 is characterized in that, described PET select for use recovery, be the sheet PET beverage bottle sheet of 2-8mm through crusher in crushing.
5, PA/PET high molecule alloy material as claimed in claim 2 is characterized in that, described chainextender is a kind of in following three kinds of materials:
O＝C＝N-(CH
2)
6-N＝C＝O
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100303255A CN1324084C (en) | 2005-10-09 | 2005-10-09 | PA/PET high molecule alloy material |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100303255A CN1324084C (en) | 2005-10-09 | 2005-10-09 | PA/PET high molecule alloy material |
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| CN1749314A CN1749314A (en) | 2006-03-22 |
| CN1324084C true CN1324084C (en) | 2007-07-04 |
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| CNB2005100303255A Expired - Fee Related CN1324084C (en) | 2005-10-09 | 2005-10-09 | PA/PET high molecule alloy material |
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| CN102229738B (en) * | 2011-05-17 | 2013-05-01 | 威海联桥新材料科技股份有限公司 | High glow-wire flame retardant reinforced PET/PA (polyethylene terephthalate/polyamide) alloy material and production method thereof |
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|---|---|---|---|---|
| US5238490A (en) * | 1992-09-04 | 1993-08-24 | Olin Corporation | Process for generating copper pyrithione in-situ in a paint formulation |
| CN1374346A (en) * | 2001-03-14 | 2002-10-16 | 中国科学院化学研究所 | Compound containing nano montmorillonoid and its prepn |
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