CN1887959A - Process of preparing engineering plastics with recovered polyethylene terephthalate - Google Patents
Process of preparing engineering plastics with recovered polyethylene terephthalate Download PDFInfo
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- CN1887959A CN1887959A CN 200610029694 CN200610029694A CN1887959A CN 1887959 A CN1887959 A CN 1887959A CN 200610029694 CN200610029694 CN 200610029694 CN 200610029694 A CN200610029694 A CN 200610029694A CN 1887959 A CN1887959 A CN 1887959A
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Abstract
The present invention is process of preparing engineering plastic with recovered polyethylene terephthalate (PET). The present invention prepares engineering plastic with recovered PET, polyamide 66 (PA66) with smelting point and viscosity near that of PET, reaction compatilizer for improving the compatibility, glass fiber for high rigidity of the composite material, antioxidant and lubricant. The composite PET/PA66/glass fiber material with the performance of engineering plastic is prepared through mixing all the materials except glass fiber in a high speed stirrer to obtain mixture, blending the mixture with glass fiber at certain temperature and rotation speed and pelletizing in a double screw extruder. The composite PET/PA66/glass fiber material has toughness and strength obviously higher that of composite PA66/glass fiber material and may be used to latter.
Description
Technical field
The present invention relates to a kind of with the method that reclaims polyethylene terephthalate (PET) preparation engineering plastics, relate in particular to and a kind ofly will reclaim polyethylene terephthalate, polyamide 66, reaction compatilizer, oxidation inhibitor, lubricant and glass fibre with twin screw extruder and carry out reactive blending, and obtain having the novel method of engineering plastics performance matrix material.The invention belongs to technical field of polymer processing.
Background technology
Polyethylene terephthalate (PET) is used for the bottle material of soft drink such as Coca-Cola in a large number, and the use of a large amount of bottles can bring pollution to environment as not recycling.At present, China's soft drink output increases progressively to surpass 20% average growth rate per annum, and the demand of its packaging PET bottle is also with 18% speed increment.According to statistics, had 1,400,000 tons of PET bottles to be dropped approximately in 2005, the pollution problem that causes thus is serious day by day, has caused extensive concern.In the face of a large amount of depleted PET bottles, how to realize that it reclaims and recycle becomes a social concern that needs to be resolved hurrily.Therefore, develop advanced recovery technology, increase substantially the ratio of " upgrading utilizes ", help comprehensive utilization, the pollution abatement of resource, solve the trouble and worry that packaging industry develops, open up new growth engines.
Exist problems such as intrinsic viscosity is low, stability of flow is poor, demoulding difficulty, moulding product impact difference owing to reclaim pet resin (PET), generally can not direct injection and extrusion moulding, be difficult to become a useful person, especially be difficult to prepare high-end product.People come to realise PET and reclaim significant, so people begin to do the recycling work of some PET, assume personal Synthesis of Polyester Waste with Benzene-Based Unsaturated Polyester Resin (CN200410084327.8) as Qian Jianhua and Liu, adopt the method for chemical reaction to utilize polyester waste material, but method is more loaded down with trivial details, and want large-scale recovery that certain difficulty is arranged, required expense and equipment is more complicated all, the cost height; People such as Guo Weihong (CN200510023658.5 and CN200510030325.5) adopt and reclaim blowing polyethylene terephthalate, polycarbonate and styrene/ethylene/butadiene/styrene copolymers is raw material, obtained the material of good-toughness, also prepare polyethylene terephtalate/nylon PA/ hydrogenation three block styrene-butadiene-styrene copolymer and obtained the engineering plastics of better performances, but the rigidity deficiency is used shortcoming to some extent as engineering plastics.
Summary of the invention
The objective of the invention is at the deficiencies in the prior art; provide a kind of with the method that reclaims polyethylene terephthalate preparation engineering plastics; utilize waste resource; prepare high strength, high performance matrix material with lower cost; actual user demand can be satisfied, environment can be well protected again.
For realizing such purpose, the present invention utilizes the close characteristics close with viscosity with polyamide 66 (PA66) fusing point of PET, and improves its consistency by adding compatilizer, utilizes glass fibre to improve the rigidity of matrix material simultaneously.The present invention is in twin screw extruder, be added in the mixture of the PET, polyamide 66, reaction compatilizer, oxidation inhibitor and the lubricant that mix on the homogenizer, under certain temperature and rotating speed, carry out reactively blending with glass fibre, extruding pelletization prepares the PET/PA66/ glass fiber compound material with engineering plastics performance.This material is compared with pure PA66 glass fibre enhanced material, and toughness and intensity all are improved significantly, and can substitute the PA66 engineering plastics.
In the method for the present invention, feed composition is by weight: reclaiming polyethylene terephthalate (PET) is that 30-60 part, PA66 are 20-50 part, reaction compatilizer 0.1-20 part, oxidation inhibitor 0.1-10 part, lubricant 0.1-10 part, 10-40 part glass fibre.
Earlier in PET; add PA66, reaction compatilizer, oxidation inhibitor and lubricant; on homogenizer, mix; the rotating speed of homogenizer is 3000-10000 rev/min; in common twin screw extruder, extrude then and make pellet with glass fibre; extruder temperature is 80-300 ℃; rotating speed is 120-600 rev/min; the residence time of material in screw rod is 1-8 minute; after the material cooling of extruding,, obtain pellet through the dicing machine pelletizing; in vacuum drying oven 80-160 ℃ dry 5-35 hour, obtain the PET/PA66/ glass fiber compound material.
Polyamide 66 of the present invention (PA66) is the polycondensate of hexanodioic acid and hexanediamine.
Polyethylene terephthalate of the present invention is the polycondensate of terephthalic acid and ethylene glycol.
Reaction compatilizer of the present invention is that a class can and can have the material of better avidity with glass fibre with polyethylene terephthalate and polyamide 66 generation chemical reaction, be silane coupling agent, titanate coupling agent, isocyanic ester, p-Hydroxybenzoate, lauryl amine, hexadecylamine, octadecylamine, 4,4 '-isopropylidene two (phenol salicylate), the salicylic acid phenyl ester, Resins, epoxy, the epoxidation vinyl benzene multipolymer, the epoxidized ethylene multipolymer, vinylbenzene-alkylmethacrylate polymer, styrene-maleic anhydride copolymer (SMA), PAUR, polyoxyethylene glycol (PEO), polythene-ethenol multipolymer (EVOH), ethylene-vinyl acetate copolymer (EVA), maleic anhydride grafted polyethylene multipolymer (PE-g-MAH), maleic anhydride inoculated polypropylene multipolymer (PP-g-MAH), polyethylene acrylic acid grafts (PE-g-AA), the polypropylene grafted thing of vinylformic acid (PP-g-AA), glycidyl methacrylate-polyethylene graft copolymer (PE-g-GMA), glycidyl methacrylate-polypropylene graft copolymer (PP-g-GMA), maleic anhydride graft styrene-butadiene-styrene multipolymer (SBS-g-MAH) or maleic anhydride graft acrylonitrile-butadiene-styrene copolymer (ABS-g-MAH), ethylene-acrylic acid copolymer (EAA), ethylene-acrylate copolymer (EMA) and 1,3-phenylene bisoxazoline (PBO) is got wherein two kinds of components or the mixture formed of two or more component.
Oxidation inhibitor of the present invention can be triphenyl phosphite, N, [3-(3 for N '-two, the 5-di-tert-butyl-hydroxy phenyl) propionyl] hydrazine (oxidation inhibitor 1098), three (2, the 4-di-tert-butyl-phenyl) phosphorous acid ester (oxidation inhibitor 168), 2,6-di-tert-butyl-4-methy phenol (antioxidant 264), four [β-(3 ', 5 '-di-t-butyl-4 '-hydroxy phenyl) propionic acid] pentaerythritol ester (antioxidant 1010), Tyox B (anti-oxidant DLTP) or 4,4 '-(β, β '-dihydroxyl dipropyl oxygen phenyl) 2,2-propane (dihydroxyphenyl propane), or the mixture of forming by them.
Lubricant of the present invention can be the two fatty amides of ethylene, silicone oil, silicone, organosilane, polymer organosilane, ethylene bis-fatty acid amine, erucicamide, amine hydroxybenzene, whiteruss, estersil, Chinese wax oil, Zinic stearas, calcium stearate or barium stearate, or the mixture of being made up of them.
Glass fibre of the present invention is long glass fibres or short glass fiber.
The inventive method is simple, prepared PET/PA66/ glass fiber compound material has excellent comprehensive performances such as good heat endurance, high strength, high tenacity, not only make recovery PET be used for high-end material, also reduced the cost of PA66 simultaneously, all significant to solving white pollution problems and industrial application.
Embodiment
Below in conjunction with embodiment technical scheme of the present invention is further described.
Following examples are to further specify of the present invention, rather than limit the scope of the invention.
Testing method among the embodiment: tensile strength is pressed GB1040, and notched Izod impact strength is pressed GB1843, and heat-drawn wire is tested by GB1633.
Embodiment 1
Feed composition is by weight: 30 parts of PET, 50 parts of PA66,0.05 part of PBO, 0.05 part of isocyanide ester, 0.2 part of antioxidant 1010,0.4 part of antioxidant 264,1.3 parts of silicone oil, 3 parts of Zinic stearass, 15 parts of short glass fibers.
Earlier with PET; PA66; PBO; isocyanide ester; antioxidant 1010; antioxidant 264; silicone oil; Zinic stearas mixes on homogenizer; the rotating speed of homogenizer is 10000 rev/mins; then mixture being put into twin screw extruder with long glass fibres extrudes and makes pellet; extruder temperature is 80/200/240/300/300/300 ℃; rotating speed is 120 rev/mins; the residence time of material in screw rod is 8 minutes; after the material cooling of extruding; through the dicing machine pelletizing; obtain pellet; 80 ℃ of dryings are 35 hours in vacuum drying oven, obtain PET/PA66/ glass fibre high performance composite.
Pure PA66 glass fiber reinforced materials and above-mentioned gained matrix material are carried out performance test, and the result who obtains is: pure PA66 glass fiber reinforced materials tensile strength is 86MPa, and shock strength is 8.1KJ/m
2, Vicat softening point is 245 ℃, smooth finish is general, and glass emergence on the surface is arranged; PET/PA66/ glass fibre high performance composite tensile strength is 112MPa, and shock strength is 10.1KJ/m
2, Vicat softening point is 246 ℃, smooth finish is fine, no glass emergence on the surface phenomenon.
Embodiment 2
Feed composition is by weight: 60 parts of PET, 20 parts of PA66,1.5 parts of EAA, 2 parts of SMA, 1098,1.3 parts of antioxidant 264s of 1.5 parts of oxidation inhibitor, 3.7 parts of erucicamides, 10 parts of short glass fibers.
Earlier with PET; PA66; PBO; EAA; SMA; oxidation inhibitor 1098; antioxidant 264; erucicamide mixes on homogenizer; the rotating speed of homogenizer is 5000 rev/mins; then mixture being put into twin screw extruder with short glass fiber extrudes and makes pellet; extruder temperature is 150/200/230/280/280/280 ℃; rotating speed is 240 rev/mins; the residence time of material in screw rod is 3 minutes; after the material cooling of extruding; through the dicing machine pelletizing; obtain pellet; 160 ℃ of dryings are 5 hours in vacuum drying oven, obtain PET/PA66/ glass fibre high performance composite.
Pure PA66 glass fiber reinforced materials and above-mentioned gained matrix material are carried out performance test, and the result who obtains is: pure PA66 glass fiber reinforced materials tensile strength is 86MPa, and shock strength is 8.1KJ/m
2, Vicat softening point is 245 ℃, smooth finish is general, and glass emergence on the surface is arranged; PET/PA66/ glass fibre high performance composite tensile strength is 123MPa, and shock strength is 9.4KJ/m
2, Vicat softening point is 245 ℃, smooth finish is fine, no glass emergence on the surface phenomenon.
Embodiment 3
Feed composition is by weight: 30 parts of PET, 20 parts of PA66,2 parts of SBS-g-MAH, 3 parts of EVOH, 2 parts of antioxidant 1010s, the two fatty amides of 168,2 parts of ethylenes of 1 part of oxidation inhibitor, 40 parts of long glass fibress.
Earlier with PET; PA66; SBS-g-MAH; EVOH; antioxidant 1010; oxidation inhibitor 168; the two fatty amides of ethylene mix on homogenizer; the rotating speed of homogenizer is 7500 rev/mins; then mixture being put into twin screw extruder with short glass fiber extrudes and makes pellet; extruder temperature is 100/200/220/270/270/270 ℃; rotating speed is 600 rev/mins; the residence time of material in screw rod is 1 minute; after the material cooling of extruding; through the dicing machine pelletizing; obtain pellet; 120 ℃ of dryings are 24 hours in vacuum drying oven, obtain PET/PA66/ glass fibre high performance composite.
Pure PA66 glass fiber reinforced materials and above-mentioned gained matrix material are carried out performance test, and the result who obtains is: pure PA66 glass fiber reinforced materials tensile strength is 86MPa, and shock strength is 8.1KJ/m
2, Vicat softening point is 245 ℃, smooth finish is general, and glass emergence on the surface is arranged; PET/PA66/ glass fibre high performance composite tensile strength is 135MPa, and shock strength is 11.3KJ/m
2, Vicat softening point is 247 ℃, smooth finish is fine, no glass emergence on the surface phenomenon.
From the result of embodiment as can be seen, what the present invention obtained the PET/PA66/ glass fiber compound material has a good comprehensive performance, toughness and intensity etc. obviously are better than the PA66/ glass fiber compound material, not only reclaimed PET, and can substitute the PA66 engineering plastics, also reduced simultaneously the cost of PA66, prepared the engineering plastics of excellent performance, wide application and industrial prospect have been arranged.
Claims (7)
1, a kind of with the method that reclaims polyethylene terephthalate preparation engineering plastics, it is characterized in that feed composition is by weight: reclaiming polyethylene terephtalate is that 30-60 part, PA66 are 20-50 part, reaction compatilizer 0.1-20 part, oxidation inhibitor 0.1-10 part, lubricant 0.1-10 part, 10-40 part glass fibre; Earlier in PET; add PA66, reaction compatilizer, oxidation inhibitor and lubricant; on homogenizer, mix; the rotating speed of homogenizer is 3000-10000 rev/min; in common twin screw extruder, extrude then and make pellet with glass fibre; extruder temperature is 80-300 ℃; rotating speed is 120-600 rev/min; the residence time of material in screw rod is 1-8 minute; after the material cooling of extruding,, obtain pellet through the dicing machine pelletizing; in vacuum drying oven 80-160 ℃ dry 5-35 hour, obtain the PET/PA66/ glass fiber compound material.
2, according to the method with recovery polyethylene terephthalate preparation engineering plastics of claim 1, it is characterized in that described PA66 is the polycondensate of hexanodioic acid and hexanediamine.
3, according to the method with recovery polyethylene terephthalate preparation engineering plastics of claim 1, it is characterized in that described polyethylene terephthalate is the polycondensate of terephthalic acid and ethylene glycol.
4, method according to claim 1 with recovery polyethylene terephthalate preparation engineering plastics, it is characterized in that described reaction compatilizer is a silane coupling agent, titanate coupling agent, vulcabond, p-Hydroxybenzoate, lauryl amine, hexadecylamine, octadecylamine, 4,4 '-isopropylidene is two, the salicylic acid phenyl ester, Resins, epoxy, the epoxidation vinyl benzene multipolymer, the epoxidized ethylene multipolymer, vinylbenzene-alkylmethacrylate polymer, vinylbenzene-copolymer-maleic anhydride, PAUR, polyoxyethylene glycol, polyethylene-vinyl alcohol copolymer, ethene-vinyl acetate copolymer, the maleic anhydride grafted polyethylene multipolymer, the maleic anhydride inoculated polypropylene multipolymer, the polyethylene acrylic acid grafts, the polypropylene grafted thing of vinylformic acid, glycidyl methacrylate-polyethylene graft copolymer, glycidyl methacrylate-polypropylene graft copolymer, maleic anhydride graft vinylbenzene-divinyl-styrol copolymer or maleic anhydride graft Acrylonitrile-butadiene-styrene Copolymer, ethene-acrylic copolymer, ethene-acrylate copolymer and 1,3-phenylene bisoxazoline is got the wherein mixture of two or more component composition.
5, method according to claim 1 with recovery polyethylene terephthalate preparation engineering plastics, it is characterized in that described oxidation inhibitor is triphenyl phosphite, N, [3-(3 for N '-two, the 5-di-tert-butyl-hydroxy phenyl) propionyl] hydrazine, three (2, the 4-di-tert-butyl-phenyl) phosphorous acid ester, 2, the 6-di-tert-butyl-4-methy phenol, four [β-(3 ', 5 '-di-t-butyl-4 '-hydroxy phenyl) propionic acid] pentaerythritol ester, Tyox B or 4,4 '-(β, β '-dihydroxyl dipropyl oxygen phenyl) 2,2-propane (dihydroxyphenyl propane), or the mixture of forming by them.
6, reclaim the method for polyethylene terephthalate preparation engineering plastics according to the usefulness of claim 1, it is characterized in that described lubricant is the two fatty amides of ethylene, silicone oil, silicone, organosilane, polymer organosilane, ethylene bis-fatty acid amine, erucicamide, amine hydroxybenzene, whiteruss, estersil, Chinese wax oil, Zinic stearas, calcium stearate or barium stearate, or the mixture of forming by them.
7, according to the method with recovery polyethylene terephthalate preparation engineering plastics of claim 1, it is characterized in that described glass fibre is long glass fibres or short glass fiber.
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