CN101280095A - Glass fiber reinforced polyethylene glycol terephthalate composite material and preparation thereof - Google Patents

Glass fiber reinforced polyethylene glycol terephthalate composite material and preparation thereof Download PDF

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Publication number
CN101280095A
CN101280095A CNA200810037696XA CN200810037696A CN101280095A CN 101280095 A CN101280095 A CN 101280095A CN A200810037696X A CNA200810037696X A CN A200810037696XA CN 200810037696 A CN200810037696 A CN 200810037696A CN 101280095 A CN101280095 A CN 101280095A
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China
Prior art keywords
matrix
fiberglass reinforced
ester
nano
mah
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CNA200810037696XA
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Chinese (zh)
Inventor
施利毅
丁鹏
葛春华
杨慧
陈德杰
胡秀兰
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Jujie High Molecular Material Co., Ltd., Shanghai
Shanghai Univer
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University of Shanghai for Science and Technology
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Priority to CNA200810037696XA priority Critical patent/CN101280095A/en
Publication of CN101280095A publication Critical patent/CN101280095A/en
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Classifications

    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29CSHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/25Component parts, details or accessories; Auxiliary operations
    • B29C48/36Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die
    • B29C48/395Means 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
    • B29C48/40Means 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
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29CSHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/25Component parts, details or accessories; Auxiliary operations
    • B29C48/92Measuring, controlling or regulating
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29CSHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C2948/00Indexing scheme relating to extrusion moulding
    • B29C2948/92Measuring, controlling or regulating
    • B29C2948/92504Controlled parameter
    • B29C2948/9258Velocity
    • B29C2948/9259Angular velocity
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29CSHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C2948/00Indexing scheme relating to extrusion moulding
    • B29C2948/92Measuring, controlling or regulating
    • B29C2948/92504Controlled parameter
    • B29C2948/92704Temperature
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29CSHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C2948/00Indexing scheme relating to extrusion moulding
    • B29C2948/92Measuring, controlling or regulating
    • B29C2948/92819Location or phase of control
    • B29C2948/92857Extrusion unit
    • B29C2948/92876Feeding, melting, plasticising or pumping zones, e.g. the melt itself
    • B29C2948/92885Screw or gear
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29CSHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C2948/00Indexing scheme relating to extrusion moulding
    • B29C2948/92Measuring, controlling or regulating
    • B29C2948/92819Location or phase of control
    • B29C2948/92857Extrusion unit
    • B29C2948/92876Feeding, melting, plasticising or pumping zones, e.g. the melt itself
    • B29C2948/92895Barrel or housing
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29CSHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C2948/00Indexing scheme relating to extrusion moulding
    • B29C2948/92Measuring, controlling or regulating
    • B29C2948/92819Location or phase of control
    • B29C2948/92857Extrusion unit
    • B29C2948/92904Die; Nozzle zone

Abstract

The invention relates to a PET glass fiber reinforced composite material, which has the following components based on weight proportion: 100 portions of PET, 10-45 portions of alkali-free glass fibers, 5.0-25 portions of toughener, 0.1-10 portions of crystallization promoter, 0.1-1.0 portion of chain extender, 0.5-5.0 portions of nucleating agent, 0.1-0.5 portion of antioxidant and 0.3-0.5 portion of lubricant. The preparation method is that the components are evenly mixed on a high-speed mixer and melted and blended by a twin-screw extruder to prepare the composite material. The composite material has the advantages of good mobility, high tensile strength and high impact strength, which aims to realize low-cost and high-quality PET engineering plastic scale production to effectively substitute for high-grade plastics and expensive imported special materials.

Description

Fiberglass reinforced polyethyleneterephthalate matrix material and preparation method thereof
Technical field
The present invention relates to the engineering plastic modification technical field, be specifically related to a kind of fiberglass reinforced polyethyleneterephthalate (PET) matrix material and preparation method thereof.
Background technology
Polyethylene terephthalate (PET) is a kind of thermoplastic engineering plastic, has excellent mechanical property, electrical insulating property, thermotolerance and chemical reagent resistance, thereby is widely used in fiber, film and beverage bottle field.At present, with regard to world wide, the PET production capacity surplus, price drops, and product is expanded to non-polyester (bottle sheet, film, engineering plastics) field with polyester by fibre just gradually.And one of research and development focus in the engineering plastics non-fine field that is PET.China has become world PET production, consumption first big country, but there are many problems in the polyester industrial of China, and its outstanding behaviours exists: PET is fine with production of polyester ability surplus, and it is narrow to produce variety range, non-polyester ratio is obviously on the low side, a little less than the new product development ability.Because PET crystallization technology fails to be resolved, the machine-shaping of goods is met difficulty, and China becomes engineering plastics importer the biggest in the world for years.Therefore research and develop high performance PE T engineering plastics; the blockade on new techniques of breaks through foreign; solution PET fibre production of polyester ability surplus, the present situation that PET engineering plastics throughput is low; realize low-cost, the large-scale production of high quality PET engineering plastics; effectively substitute high-grade plastics and expensive import PP Pipe Compound, have crucial meaning.
Want to make the PET through engineering approaches, will improve the crystallization rate of PET resin, shorten injection cycle, corresponding raising PET shock resistance and physical strength.Glass is because remarkable, the addition of reinforced effects big (can reach 45%) and can improve the impact of material simultaneously and heat-drawn wire and generally be subjected to people's favor; but use its impelling strength of thermoplastic polyester of glass modification relatively poor merely; glossiness is low; regular meeting causes glass emergence on the surface when being injection molded into goods, influences product properties and outward appearance.In order to improve PET impelling strength, improve the surface smoothness of PET/ glass fiber composite material, common method of modifying is to add thermoplastic elastomer toughening, and glass is carried out organic process.As making the fiberglass reinforced polyethyleneterephthalate matrix material with the nylon-type polymkeric substance as nucleator among the patent CN1136577A, but its notched Izod impact strength deficiency is difficult to as the engineering structure part; Fung.K.L. wait and reported with MA-g-SEBS triblock copolymer toughened PET (Polym.Test.2005 No.24, p863-872), its notched Izod impact strength is greatly improved, and makes tensile strength of material and tensile modulus descend the loss material rigidity but then again.
Summary of the invention
The object of the present invention is to provide a kind of fiberglass reinforced polyethyleneterephthalate matrix material.
Another object of the present invention is to provide a kind of preparation method of fiberglass reinforced polyethyleneterephthalate matrix material.Improving the strength of materials, flexible simultaneously, improve its surface gloss, thermotolerance.
For achieving the above object, the present invention adopts following technical proposals:
A kind of fiberglass reinforced polyethyleneterephthalate matrix material is characterized in that its composition counts by weight:
(1) polyethylene terephthalate is 100 parts
(2) alkali free glass fibre (GF) is 10~45 parts
(3) toughner is 5.0~25 parts
(4) crystallization promoter is 0.1~10 part
(5) chainextender is 0.1~1.0 part
(6) nucleator is 0.5~5.0 part
(7) oxidation inhibitor is 0.1~0.5 part
(8) lubricant is 0.3~0.5 part
Described toughner is maleic anhydride grafted polyethylene multipolymer (PE-g-MAH), maleic anhydride inoculated polypropylene multipolymer (PP-g-MAH), maleic anhydride grafted ethene-octene copolymer (P0E-g-MAH), maleic anhydride graft polyphenylene ether copolymer (PPO-g-MAH), maleic anhydride graft styrene-butadiene-styrene multipolymer (MAH-g-SBS), maleic anhydride graft styrene-ethylene-butylene-styrene multipolymer (MAH-g-SEBS), glycidyl methacrylate-polyethylene graft copolymer (GMA-g-PE), glycidyl methacrylate-polypropylene graft copolymer (GMA-g-PP), polyethylene acrylic acid grafts (PE-g-AA), a kind of in the polypropylene grafted thing of vinylformic acid (PP-g-AA) or the compound of forming by above several toughner.
Described crystallization promoter is a low molecular compound, as ketone (benzophenone), ester class (season pentanediol benzhydryl ester, triphenyl, phthalic ester, carboxylic acid amide esters, imines ester); Or be macromolecular compound, as polyester (polycaprolactone and end-caps thereof), polyoxyethylene glycol (PEG1000, polypropylene glycol and end-caps thereof).
Described chainextender is the organism of two above hydroxyls or carboxyl, comprises equal benzene dianhydride (PMDA), Pyrogentisinic Acid's dihydroxyl ether (HQEE), 1, and the 4-butyleneglycol (1,4-BD), 3,3 '-two chloro-4,4 '-diamino-ditan (MOCA).
Described nucleator is for being of a size of nano level inorganic powder at least on the one dimension direction, its median size is 1~200nm, as nano imvite, nano mica, nanoclay, nano barite, nano-calcium carbonate, nano silicon, nano aluminium oxide, or its two or more compound; Perhaps nucleator is an organic nucleating agent, as monocarboxylic acid or multi-carboxylate, montanin wax or montanate salt, pentanoic, tetrachloroethane, acetone, Nitromethane 99Min., benzene, toluene, tetraline, aromatic alcohols and amine, basic metal aromatic alkyl sulfonate, epoxy compounds.
Described oxidation inhibitor is phenolic antioxidant, as four (β-(3, the 5-di-tert-butyl-hydroxy phenyl) propionic acid) pentaerythritol ester (antioxidant 1010), β-(4-hydroxy phenyl-3, the 5-di-t-butyl) the positive octadecanol ester of propionic acid (antioxidant 1076),, triglycol two [3-(3-tertiary butyl-4-hydroxy-5-aminomethyl phenyl) propionic ester] (oxidation inhibitor 245); Or for containing the thioesters kind antioxidant, as Tyox B (DLTP); Or be that phosphite ester kind antioxidant is as three (2, the 4-di-tert-butyl-phenyl) phosphorous acid esters (oxidation inhibitor 168), triphenyl phosphite (TPP); Or the mixture of the above oxidation inhibitor composition of serving as reasons.
Described lubricant is a kind of in estersil, organosilane, whiteruss, the five tetrahydroxybutane tetrastearates (PETS), or is the two fatty amide series lubricant agents of ethylene, or the mixture formed of the above lubricant of serving as reasons.
A kind of preparation method who is used for the fiberglass reinforced polyethyleneterephthalate matrix material, it is characterized in that this method has following technological process: after exsiccant polyethylene terephthalate and toughner, chainextender, nucleator, crystallization promoter, oxidation inhibitor, lubricant are stirred in homogenizer, add the twin screw extruder from charging opening, forcing machine melt extrudes temperature and is set in 220~290 ℃ of scopes, vacuum tightness-0.08Pa, engine speed 80~280r/min; Glass fibre needs to add at the downstream charging opening in advance through the silane coupling agent surface treatment; Extruded material after the drying, promptly gets the fiberglass reinforced polyethyleneterephthalate matrix material through cooling, air-dry, pelletizing.
The present invention is by multinomial new technology integrating, secondary innovation, with the high tensile of glass, high tensile modulus and thermoplastic elastomer toughening, the inorganic nano rigidity particle coordination plasticizing, the PET toughness that has compensated after glass adds descends, and other property retentions of material are constant or few the reduction, make the fiberglass reinforced polyethyleneterephthalate matrix material of high gloss, high-modulus, high impact-resistant, low warpage, dimensional stabilizing high comprehensive performance.
Embodiment
Below in conjunction with embodiment the present invention is elaborated.
Embodiment 1~6 gets the raw materials ready by the prescription of table 1; After exsiccant polyethylene terephthalate and toughner, chainextender, nucleator, crystallization promoter, oxidation inhibitor, lubricant stirred in homogenizer, add the twin screw extruder from charging opening, forcing machine melt extrudes temperature and is set in 220~290 ℃ of scopes, vacuum tightness one 0.08Pa, engine speed 80~280r/min; Glass fibre needs to add at the downstream charging opening in advance through the silane coupling agent surface treatment; Extruded material after the drying, promptly gets the fiberglass reinforced polyethyleneterephthalate matrix material through cooling, air-dry, pelletizing.
The prescription of embodiment such as following table:
Table 1 Example formulations
Table 2 embodiment performance of composites test result
Project Testing method Embodiment 1 Embodiment 2 Embodiment 3
Tensile strength (MPa) ??ASTMD638 ??122 ??157 ??170
Flexural strength (Mpa) ??ASTMD790 ??193 ??235 ??249
Modulus in flexure (Mpa) ??ASTMD790 ??8200 ??9150 ??11000
Notched Izod impact strength (cantilever) (J/m) ??ASTMD256 ??101 ??103 ??108
0.45Mpa following heat-drawn wire ℃ ??ASTMD648 ??240 ??246 ??250
The foregoing description for explanation technical conceive of the present invention and characteristics, is not in order to limit claim of the present invention only.All equivalences that spirit is done according to the present invention change or improve, and all should be included within protection scope of the present invention.

Claims (8)

1. fiberglass reinforced polyethyleneterephthalate matrix material is characterized in that its composition counts by weight:
(1) polyethylene terephthalate is 100 parts
(2) alkali free glass fibre is 10~45 parts
(3) toughner is 5.0~25 parts
(4) crystallization promoter is 0.1~10 part
(5) chainextender is 0.1~1.0 part
(6) nucleator is 0.5~5.0 part
(7) oxidation inhibitor is 0.1~0.5 part
(8) lubricant is 0.3~0.5 part.
2. fiberglass reinforced polyethyleneterephthalate matrix material according to claim 1 is characterized in that described toughner is maleic anhydride grafted polyethylene multipolymer (PE-g-MAH), maleic anhydride inoculated polypropylene multipolymer (PP-g-MAH), maleic anhydride grafted ethene-octene copolymer (P0E-g-MAH), maleic anhydride graft polyphenylene ether copolymer (PPO-g-MAH), maleic anhydride graft styrene-butadiene-styrene multipolymer (MAH-g-SBS), maleic anhydride graft styrene-ethylene-butylene-styrene multipolymer (MAH-g-SEBS), glycidyl methacrylate-polyethylene graft copolymer (GMA-g-PE), glycidyl methacrylate-polypropylene graft copolymer (GMA-g-PP), polyethylene acrylic acid grafts (PE-g-AA), a kind of in the polypropylene grafted thing of vinylformic acid (PP-g-AA) or the compound of forming by above several toughner.
3. fiberglass reinforced polyethyleneterephthalate matrix material according to claim 1, it is characterized in that described crystallization promoter is a low molecular compound, as ketone (benzophenone), ester class (season pentanediol benzhydryl ester, triphenyl, phthalic ester, carboxylic acid amide esters, imines ester); Or be macromolecular compound, as polyester (polycaprolactone and end-caps thereof), polyoxyethylene glycol (PEG1000, polypropylene glycol and end-caps thereof).
4. fiberglass reinforced polyethyleneterephthalate matrix material according to claim 1, it is characterized in that described chainextender is the organism of two above hydroxyls or carboxyl, comprise equal benzene dianhydride (PMDA), Pyrogentisinic Acid's dihydroxyl ether (HQEE), 1,4-butyleneglycol (1,4-BD), 3,3 '-two chloro-4,4 '-diamino-ditan (MOCA).
5. fiberglass reinforced polyethyleneterephthalate matrix material according to claim 1, it is characterized in that described nucleator is for being of a size of nano level inorganic powder at least on the one dimension direction, its median size is 1~200nm, as nano imvite, nano mica, nanoclay, nano barite, nano-calcium carbonate, nano silicon, nano aluminium oxide, or its two or more compound; Perhaps nucleator is an organic nucleating agent, as monocarboxylic acid or multi-carboxylate, montanin wax or montanate salt, pentanoic, tetrachloroethane, acetone, Nitromethane 99Min., benzene, toluene, tetraline, aromatic alcohols and amine, basic metal aromatic alkyl sulfonate, epoxy compounds.
6. according to claim 1 fiberglass reinforced polyethyleneterephthalate matrix material, it is characterized in that described oxidation inhibitor is phenolic antioxidant, as four (β-(3, the 5-di-tert-butyl-hydroxy phenyl) propionic acid) pentaerythritol ester (antioxidant 1010), β-(4-hydroxy phenyl-3, the 5-di-t-butyl) the positive octadecanol ester of propionic acid (antioxidant 1076),, triglycol two [3-(3-tertiary butyl-4-hydroxy-5-aminomethyl phenyl) propionic ester] (oxidation inhibitor 245); Or for containing the thioesters kind antioxidant, as Tyox B (DLTP); Or be that phosphite ester kind antioxidant is as three (2, the 4-di-tert-butyl-phenyl) phosphorous acid esters (oxidation inhibitor 168), triphenyl phosphite (TPP); Or the mixture of the above oxidation inhibitor composition of serving as reasons.
7. fiberglass reinforced polyethyleneterephthalate matrix material according to claim 1, it is characterized in that described lubricant is a kind of in estersil, organosilane, whiteruss, the five tetrahydroxybutane tetrastearates (PETS), or be 1,2-ethylenebis fatty amide series lubricant agent, or the mixture of the above lubricant composition of serving as reasons.
8. preparation method who is used for fiberglass reinforced polyethyleneterephthalate matrix material according to claim 1, it is characterized in that this method has following technological process: after exsiccant polyethylene terephthalate and toughner, chainextender, nucleator, crystallization promoter, oxidation inhibitor, lubricant are stirred in homogenizer, add the twin screw extruder from charging opening, forcing machine melt extrudes temperature and is set in 220~290 ℃ of scopes, vacuum tightness-0.08Pa, engine speed 80~280r/min; Glass fibre needs to add at the downstream charging opening in advance through the silane coupling agent surface treatment; Extruded material after the drying, promptly gets the fiberglass reinforced polyethyleneterephthalate matrix material through cooling, air-dry, pelletizing.
CNA200810037696XA 2008-05-20 2008-05-20 Glass fiber reinforced polyethylene glycol terephthalate composite material and preparation thereof Pending CN101280095A (en)

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Cited By (48)

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CN101875759A (en) * 2010-03-31 2010-11-03 深圳市科聚新材料有限公司 Reinforced polyethylene glycol terephthalate-modified material and preparation method thereof
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CN108948687A (en) * 2018-07-27 2018-12-07 长春智享优创科技咨询有限公司 Efficiently barrier polyethylene terephthalate composite material and preparation method
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CN111592667A (en) * 2020-06-01 2020-08-28 广西科学院 Reinforced antibacterial artificial granite waste residue-based plastic master batch and preparation method thereof

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