CN101402784A - Glass fiber reinforced polyethylene terephthalate composite material and method of producing the same - Google Patents
Glass fiber reinforced polyethylene terephthalate composite material and method of producing the same Download PDFInfo
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- CN101402784A CN101402784A CNA2008102025027A CN200810202502A CN101402784A CN 101402784 A CN101402784 A CN 101402784A CN A2008102025027 A CNA2008102025027 A CN A2008102025027A CN 200810202502 A CN200810202502 A CN 200810202502A CN 101402784 A CN101402784 A CN 101402784A
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- polyethylene terephthalate
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- 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
- B29C48/36—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die
- B29C48/395—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die using screws surrounded by a cooperating barrel, e.g. single screw extruders
- B29C48/40—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die using screws surrounded by a cooperating barrel, e.g. single screw extruders using two or more parallel screws or at least two parallel non-intermeshing screws, e.g. twin screw extruders
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- 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
- B29C48/03—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor characterised by the shape of the extruded material at extrusion
- B29C48/04—Particle-shaped
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- 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
-
- 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
- B29C2948/92819—Location or phase of control
- B29C2948/92857—Extrusion unit
- B29C2948/92876—Feeding, melting, plasticising or pumping zones, e.g. the melt itself
- B29C2948/92895—Barrel or housing
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Abstract
The invention relates to a polyethylene glycol terephthalate composite material strengthened by fiberglass, which is characterized by being composed of the following materials with the following parts by weight: 100 portions of PET, 5 portions to 20 portions of composite elastomer compatibilizer and flexibilizer, 1 portion to 3 portions of composite nucleator, 3 portions to 8 portions of crystal accelerator, 0 portion to 3 portions of ester exchange inhibitor, 1 portion to 2 portions of antioxidant, 2 portions to 9 portions of modifying auxiliary agent, 0.2 portion to 0.5 portion of silicon oil and 30 portions of fiberglass. The preparation method of the composite material consists of the following steps: firstly, the PET, the composite elastomer compatibilizer and flexibilizer and the silicon oil are mixed in a high speed mixer, and then the nucleator, the crystal accelerator, the ester exchange inhibitor, the antioxidant and the modifying auxiliary agent are added and mixed up; and secondly, the mixture is melted with the fiberglass in a combined twin-screw extruder to extrude particles. The composite material has the advantages that the prepared PET/fiberglass composite material can be shaped at the temperature of 70 DEG C mold temperature and the shrinkage and warpage degree in anaphase are small.
Description
Technical field
The present invention relates to a kind of glass reinforced polyethylene terephthalate and preparation method thereof, belong to the engineering plastics technical field.
Background technology
Polyethylene terephthalate (PET) is because of having good resistance to fatigue, rub resistance, ageing resistance and electrical insulating property, thereby is widely used in fields such as synthon, film and polyester bottles, but also very limited in the engineering plastics Application for Field.Because the rigid structure of PET molecular chain makes its crystallization velocity slower, its cold crystallization temperature generally reaches about 130 ℃, need adopt the gentle long shaping cycle of higher mould during injection moulding.Crystallization is slow under common molding processing temperature, the poor toughness of material, and the product warpage is serious, and poor dimensional stability is so limited its application in engineering plastics.
At present the gordian technique of commercialization PET is mainly grasped by external major companies such as Dupont, General Electric Apparatus Co.(U.S.A.) and German BTE companies, and price is high.China starts late PET as the research of engineering plastics development and use; and what go in for the study exploitation mainly is some universities and colleges or scientific research institutions; therefore the research about fast crystalline PET rests on theory or laboratory study stage mostly, and this is the deadly defect in the domestic PET engineering plastics research.In addition, in order to improve crystallization rate, be cost often with loss mechanical property or heat-drawn wire.Therefore, the domestic market need be developed the PET THE ENGINEERING PLASTICS INDUSTRY product of high comprehensive performance in a hurry, to satisfy the ever-increasing market requirement.
Summary of the invention
The purpose of this invention is to provide glass reinforced polyethylene terephthalate of a kind of low-shrinkage and low warpage and preparation method thereof.
In order to achieve the above object, technical scheme of the present invention provides a kind of glass reinforced polyethylene terephthalate, it is characterized in that, is made up of following raw material in weight part:
100 parts of polyethylene terephthalates;
Composite elastic body compatibilization and toughening agent 5-20 part;
Composite nucleating agent 1-3 part;
Crystallization promoter 3-8 part;
Ester exchange inhibitor 0-3 part;
Antioxidant 1-2 part;
Modified additive 2-9 part;
Silicone oil 0.2-0.5 part;
30 parts in glass fibre.
Further, the agent of described composite elastic body compatibilization and toughening preferably is made up of among maleic anhydride graft linear low density polyethylene, maleic anhydride graft styrene-ethylene-butylene-styrene segmented copolymer, ethylene-vinyl acetate copolymer, polybutylene terephthalate, ethene-n-butyl acrylate-glycidyl methacrylate copolymer and the PT862 two or more.
Described composite nucleating agent is preferably the A+B type, and wherein, A is made up of among NA-11, NaV101,295A, Surlyn8920 and the PET-C two or more; B is superfine talcum powder, stearic acid, organobentonite or Sodium Benzoate.
Described crystallization promoter is preferably butanols atactic polyether, polyoxyethylene glycol or polyether polyester copolymer.
Described ester exchange inhibitor preferably is made up of Stearinsaeure polyoxyethylene glycol phosphoric acid ester and SODIUM PHOSPHATE, MONOBASIC, uses when adding ethylene-vinyl acetate copolymer or polybutylene terephthalate.
Described modified additive preferably is made up of in modified barium sulphate, modified micaceous powder, glass microballon, calcium sulfate crystal whiskers, the outer distillate medicinal water of anti-fiber and the dispersion agent one or more.
The outer distillate medicinal water of described anti-fiber is preferably TAF.
Described dispersion agent is preferably glycolube-P or ethylene bis stearic acid amide.
The present invention also provides the preparation method of above-mentioned glass reinforced polyethylene terephthalate, it is characterized in that, concrete steps are: earlier with polyethylene terephthalate, the agent of composite elastic body compatibilization and toughening and silicone oil in high-speed mixer and mixing, and then adding nucleator, crystallization promoter, ester exchange inhibitor, antioxidant and modified additive, mix, melt extrude granulation with glass fibre again in the twin screw extruder of combination, extrusion temperature is 220～260 ℃.
PET of the present invention and glass fibre interfacial adhesion are strong, the mechanical property excellence; Composite nucleating agent can improve the crystallization rate of PET greatly, and crystallization promoter reduces the second-order transition temperature of polyester effectively, makes the PET can machine-shaping under lower mould temperature, and the shrinking percentage in later stage and buckling deformation are little.
Embodiment
The invention will be further described below in conjunction with embodiment.
Embodiment 1
A kind of glass reinforced polyethylene terephthalate is made up of following raw material in weight part: the polyethylene terephthalate (trade mark: the light section is arranged; Producer: the fine company limited in one-tenth Xinghua, Zhangjiagang) 100 parts; 5 parts of composite elastic body compatibilization and toughening agent; 1 part of composite nucleating agent; 3 parts of crystallization promoters; 1 part of antioxidant; 2 parts of modified additives; 0.2 part of silicone oil; 30 parts in glass fibre.
The agent of described composite elastic body compatibilization and toughening is made up of maleic anhydride graft linear low density polyethylene 2.5 weight parts and ethene-n-butyl acrylate-glycidyl methacrylate copolymer 2.5 weight parts.Described composite nucleating agent is the A+B type, and wherein, A is made up of NA-11 (Ciba company limited) 0.25 weight part and NaV101 (German Clariant company) 0.25 weight part; B is 0.5 part of a superfine talcum powder.Described crystallization promoter is the butanols atactic polyether.Described modified additive is made up of modified barium sulphate.Glass fibre is the ER13-2000-988A YF11 of megalith group.Described antioxidant is antioxidant 168 (a Switzerland vapour Bagong department).
The preparation method of above-mentioned glass reinforced polyethylene terephthalate, concrete steps are: earlier with polyethylene terephthalate, agent of composite elastic body compatibilization and toughening and silicone oil are in high-speed mixer and mixing, and then adding nucleator, crystallization promoter, antioxidant and modified additive, mix, in the twin screw extruder of combination, melt extrude granulation again with glass fibre, the engine speed of forcing machine is 244rpm, feeding rotating speed 44rpm, melt extruding temperature is 220～260 ℃, each section temperature is followed successively by: 220 ℃, 230 ℃, 240 ℃, 240 ℃, 240 ℃, 240 ℃, 240 ℃, 240 ℃, 230 ℃, 230 ℃, promptly obtain the glass REINFORCED PET matrix material of low-shrinkage and low warpage.
Embodiment 2
A kind of glass reinforced polyethylene terephthalate is made up of following raw material in weight part: the polyethylene terephthalate (trade mark: the light section is arranged; Producer: the fine company limited in one-tenth Xinghua, Zhangjiagang) 100 parts; 20 parts of composite elastic body compatibilization and toughening agent; 3 parts of composite nucleating agents; 8 parts of crystallization promoters; 3 parts of ester exchange inhibitor; 2 parts of antioxidants; 9 parts of modified additives; 0.5 part of silicone oil; 30 parts in glass fibre.
The agent of described composite elastic body compatibilization and toughening is made up of ethylene-vinyl acetate copolymer 10 weight parts and polybutylene terephthalate 10 weight parts.Described composite nucleating agent is the A+B type, and wherein, A is made up of 295A (U.S. Honeywell Inc.) 0.5 weight part, Surlyn8920 (du pont company) 0.5 weight part and PET-C (Beijing Beiqing Lianke Nano P﹠R Co., Ltd.) 0.5 weight part; B is stearic acid 1.5 weight parts.Described crystallization promoter is a polyoxyethylene glycol.
Described ester exchange inhibitor is made up of Stearinsaeure polyoxyethylene glycol phosphoric acid ester 1.5 weight parts and SODIUM PHOSPHATE, MONOBASIC 1.5 weight parts.Described modified additive is made up of modified micaceous powder 2 weight parts, glass microballon 2 weight parts, calcium sulfate crystal whiskers 2 weight parts, outer distillate medicinal water 2 weight parts of anti-fiber and dispersion agent 1 weight part.The outer distillate medicinal water of described anti-fiber is TAF (a Suzhou Xingtai state photochemistry auxiliary agent company limited).Described dispersion agent is glycolube-P (du pont company).Glass fibre is the ER13-2000-988A YF11 of megalith group.Described antioxidant is antioxidant 1010 (a Switzerland vapour Bagong department).
The preparation method of above-mentioned glass reinforced polyethylene terephthalate, concrete steps are: earlier with polyethylene terephthalate, agent of composite elastic body compatibilization and toughening and silicone oil are in high-speed mixer and mixing, and then adding nucleator, crystallization promoter, ester exchange inhibitor, antioxidant and modified additive, mix, in the twin screw extruder of combination, melt extrude granulation again with glass fibre, the engine speed of forcing machine is 244rpm, feeding rotating speed 44rpm, each section temperature is followed successively by: 240 ℃, and 250 ℃, 260 ℃, 260 ℃, 260 ℃, 260 ℃, 260 ℃, 260 ℃, 250 ℃, 250 ℃, promptly obtain the glass REINFORCED PET matrix material of low-shrinkage and low warpage.
Embodiment 3
A kind of glass reinforced polyethylene terephthalate is made up of following raw material in weight part: the polyethylene terephthalate (trade mark: the light section is arranged; Producer: the fine company limited in one-tenth Xinghua, Zhangjiagang) 100 parts; 10 parts of composite elastic body compatibilization and toughening agent; 2 parts of composite nucleating agents; 5 parts of crystallization promoters; 1.5 parts of ester exchange inhibitor; 1.5 parts of antioxidants; 5 parts of modified additives; 0.35 part of silicone oil; 30 parts in glass fibre.
The agent of described composite elastic body compatibilization and toughening is made up of maleic anhydride graft linear low density polyethylene 5 weight parts, ethylene-vinyl acetate copolymer 5 weight parts.Described composite nucleating agent is the A+B type, and wherein, A is made up of NA-11 (Ciba company limited) 0.5 weight part, 295A (U.S. Honeywell Inc.) 0.5 weight part; B is an organobentonite.Described crystallization promoter is a polyether polyester copolymer.Described ester exchange inhibitor is made up of Stearinsaeure polyoxyethylene glycol phosphoesterase 30 .5 weight part and SODIUM PHOSPHATE, MONOBASIC 1 weight part.Described modified additive is made up of modified micaceous powder 1 weight part, glass microballon 1 weight part, calcium sulfate crystal whiskers 1 weight part, outer distillate medicinal water 1 weight part of anti-fiber and dispersion agent 1 weight part.The outer distillate medicinal water of described anti-fiber is TAF (a Suzhou Xingtai state photochemistry auxiliary agent company limited).Described dispersion agent is an ethylene bis stearic acid amide.Glass fibre is the ER13-2000-988A YF11 of megalith group.Antioxidant is antioxidant 1010 (a Switzerland vapour Bagong department).
The preparation method of above-mentioned glass reinforced polyethylene terephthalate, concrete steps are: earlier with polyethylene terephthalate, agent of composite elastic body compatibilization and toughening and silicone oil are in high-speed mixer and mixing, and then adding nucleator, crystallization promoter, ester exchange inhibitor, antioxidant and modified additive, mix, in the twin screw extruder of combination, melt extrude granulation again with glass fibre, the engine speed of forcing machine is 244rpm, feeding rotating speed 44rpm, each section temperature is followed successively by: 230 ℃, and 240 ℃, 250 ℃, 250 ℃, 250 ℃, 250 ℃, 250 ℃, 250 ℃, 240 ℃, 240 ℃, promptly obtain the glass REINFORCED PET matrix material of low-shrinkage and low warpage.
Embodiment 4
A kind of glass reinforced polyethylene terephthalate is made up of following raw material in weight part: the polyethylene terephthalate (trade mark: the light section is arranged; Producer: the fine company limited in one-tenth Xinghua, Zhangjiagang) 100 parts; 10 parts of composite elastic body compatibilization and toughening agent; 2 parts of composite nucleating agents; 5 parts of crystallization promoters; 1.5 parts of ester exchange inhibitor; 1.5 parts of antioxidants; 5 parts of modified additives; 0.35 part of silicone oil; 30 parts in glass fibre.
The agent of described composite elastic body compatibilization and toughening is made up of maleic anhydride graft linear low density polyethylene 5 weight parts, ethylene-vinyl acetate copolymer 5 weight parts.Described composite nucleating agent is the A+B type, and wherein, A is made up of NA-11 (Ciba company limited) 0.5 weight part, 295A (U.S. Honeywell Inc.) 0.5 weight part; B is a Sodium Benzoate.Described crystallization promoter is a polyether polyester copolymer.Described ester exchange inhibitor is made up of Stearinsaeure polyoxyethylene glycol phosphoesterase 30 .5 weight part and SODIUM PHOSPHATE, MONOBASIC 1 weight part.Described modified additive is made up of modified micaceous powder 1 weight part, glass microballon 1 weight part, calcium sulfate crystal whiskers 1 weight part, outer distillate medicinal water 1 weight part of anti-fiber and dispersion agent 1 weight part.The outer distillate medicinal water of described anti-fiber is TAF (a Suzhou Xingtai state photochemistry auxiliary agent company limited).Described dispersion agent is an ethylene bis stearic acid amide.Glass fibre is the ER13-2000-988A YF11 of megalith group.Antioxidant is antioxidant 1010 (a Switzerland vapour Bagong department).
The preparation method of above-mentioned glass reinforced polyethylene terephthalate, concrete steps are: earlier with polyethylene terephthalate, agent of composite elastic body compatibilization and toughening and silicone oil are in high-speed mixer and mixing, and then adding nucleator, crystallization promoter, ester exchange inhibitor, antioxidant and modified additive, mix, in the twin screw extruder of combination, melt extrude granulation again with glass fibre, the engine speed of forcing machine is 244rpm, feeding rotating speed 44rpm, each section temperature is followed successively by: 230 ℃, and 240 ℃, 250 ℃, 250 ℃, 250 ℃, 250 ℃, 250 ℃, 250 ℃, 240 ℃, 240 ℃, promptly obtain the glass REINFORCED PET matrix material of low-shrinkage and low warpage.
The Mechanics Performance Testing of embodiment 1-4 products obtained therefrom is as follows:
Above-mentioned product is drawn a design at injection moulding machine, and the injection mold temperature is 70 ℃.Batten is tested, its result such as table 1, wherein molding shrinkage records sample behind 130 ℃ of annealing 35h.The purpose that adds nucleator is to reduce cold crystallization peak temperature, improves fusion-crystallization peak temperature, and the difference of cold crystallization peak temperature and fusion-crystallization peak temperature is a crystallization range.Crystallization range is big more, shows that crystallization nucleation speed is fast more, helps injection moulding under low mould temperature more.
The detected result of table 1 shows, every performance index of described a kind of low-shrinkage and low warp glass fiber REINFORCED PET matrix material all meet or exceed pre-provisioning request, make material have good mechanical performance and processing characteristics, and the shrinking percentage of goods and buckling deformation are less.
The mechanical property of table 1 PET/GF and crystal property
Claims (10)
1. a glass reinforced polyethylene terephthalate is characterized in that, is made up of following raw material in weight part:
100 parts of polyethylene terephthalates;
Composite elastic body compatibilization and toughening agent 5-20 part;
Composite nucleating agent 1-3 part;
Crystallization promoter 3-8 part;
Ester exchange inhibitor 0-3 part;
Antioxidant 1-2 part;
Modified additive 2-9 part;
Silicone oil 0.2-0.5 part;
30 parts in glass fibre.
2. a kind of glass reinforced polyethylene terephthalate as claimed in claim 1, it is characterized in that the agent of described composite elastic body compatibilization and toughening is made up of among maleic anhydride graft linear low density polyethylene, maleic anhydride graft styrene-ethylene-butylene-styrene segmented copolymer, ethylene-vinyl acetate copolymer, polybutylene terephthalate, ethene-n-butyl acrylate-glycidyl methacrylate copolymer and the PT862 two or more.
3. a kind of glass reinforced polyethylene terephthalate as claimed in claim 1, it is characterized in that, described composite nucleating agent is the A+B type, and wherein, A is made up of among NA-11, NaV101,295A, Surlyn8920 and the PET-C two or more; B is superfine talcum powder, stearic acid, organobentonite or Sodium Benzoate.
4. a kind of glass reinforced polyethylene terephthalate as claimed in claim 1 is characterized in that described crystallization promoter is butanols atactic polyether, polyoxyethylene glycol or polyether polyester copolymer.
5. a kind of glass reinforced polyethylene terephthalate as claimed in claim 1, it is characterized in that, described ester exchange inhibitor is made up of Stearinsaeure polyoxyethylene glycol phosphoric acid ester and SODIUM PHOSPHATE, MONOBASIC, uses when adding ethylene-vinyl acetate copolymer or polybutylene terephthalate.
6. a kind of glass reinforced polyethylene terephthalate as claimed in claim 1 is characterized in that described antioxidant is antioxidant 168 or antioxidant 1010.
7. a kind of glass reinforced polyethylene terephthalate as claimed in claim 1, it is characterized in that described modified additive is made up of in modified barium sulphate, modified micaceous powder, glass microballon, calcium sulfate crystal whiskers, the outer distillate medicinal water of anti-fiber and the dispersion agent one or more.
8. a kind of glass reinforced polyethylene terephthalate as claimed in claim 7 is characterized in that, the outer distillate medicinal water of described anti-fiber is TAF.
9. a kind of glass reinforced polyethylene terephthalate as claimed in claim 7 is characterized in that described dispersion agent is glycolube-P or ethylene bis stearic acid amide.
10. the preparation method of a kind of glass reinforced polyethylene terephthalate as claimed in claim 1, it is characterized in that, concrete steps are: earlier with polyethylene terephthalate, the agent of composite elastic body compatibilization and toughening and silicone oil in high-speed mixer and mixing, and then adding nucleator, crystallization promoter, ester exchange inhibitor, antioxidant and modified additive, mix, melt extrude granulation with glass fibre again in the twin screw extruder of combination, extrusion temperature is 220～260 ℃.
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| CNA2008102025027A CN101402784A (en) | 2008-11-10 | 2008-11-10 | Glass fiber reinforced polyethylene terephthalate composite material and method of producing the same |
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| CNA2008102025027A CN101402784A (en) | 2008-11-10 | 2008-11-10 | Glass fiber reinforced polyethylene terephthalate composite material and method of producing the same |
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2008
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