CN1472254A - Fibreglass reinforced polyester composite material and preparing method thereof - Google Patents
Fibreglass reinforced polyester composite material and preparing method thereof Download PDFInfo
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- CN1472254A CN1472254A CNA021362505A CN02136250A CN1472254A CN 1472254 A CN1472254 A CN 1472254A CN A021362505 A CNA021362505 A CN A021362505A CN 02136250 A CN02136250 A CN 02136250A CN 1472254 A CN1472254 A CN 1472254A
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Abstract
A glass fibres reinforced polyester material is prepared from polyester, nucleator, toughening and chain-enlarging agent, antioxidizing agent and glass fibres through proportional mixing, fusing, extruding out, and granulating. Its advantages are high impact strength and modulus, and easy machining.
Description
Technical field
The present invention relates to a kind of matrix material of glass-fiber-reinforced polyester, more specifically relate to a kind of matrix material that contains the glass-fiber-reinforced polyester of toughness reinforcing, chainextender.
The invention still further relates to the preparation method of this matrix material.
Background technology
Linear saturated polyester such as PET etc. have just obtained gyp application a long time ago as fiber, film.Because its excellent physics and chemical property in recent years, are applied to the engineering plastics field more and more.Along with increasing that polyester is used in engineering plastics, glass-fiber-reinforced polyester comes into one's own all the more.Compound by glass fibre and polyester both can have been improved mechanical property and other physicalies of material, greatly also can improve the thermal property of material.Yet, because some singularity of polyester self intrinsic, when use glass-fiber-reinforced polyester, not only to consider to overcome the singularity problem of polyester itself, the while also to take into account some non-enhancing systems the technical problem that can not occur.
It at the bottom of the crystallization rate institute of polyester inherent singularity problem own.The distinctive low crystallization rate of polyester can cause the shaping cycle of product to reduce, and dimensional stability was not good when production efficiency was difficult to raising and high temperature.The importing of glass fibre can promote crystallizing polyester, and part addresses this problem, but practice shows that this also is nowhere near.
Because the compound technical barrier that produces of glass fibre and polyester mainly shows following four aspects:
The firstth, because the importing of glass fibre and reduce the processability of system greatly.
The secondth, owing to the importing of glass fibre increases considerably the viscosity of material, thereby increase the difficulty of its application.
The 3rd is that a large amount of cloudings can appear in the surface of moulding.The appearance of clouding is relevant with employed low-viscosity polyester in the glass-fiber-reinforced polyester.
The 4th, the same with the glass fibre reinforcement of other types, need consider interface bonding situation between polyester and the glass fibre with glass fibre enhanced polyester.The interface bonding is all extremely important for any glass fibre reinforcement, because different polymkeric substance has different characteristics, therefore must take in respectively for different polymkeric substance.
In order to obtain to process the glass-fiber-reinforced polyester material of facility, excellent property, must address the above problem one by one.
The at present relevant low problem of crystallizing polyester speed has had the very technical solution of mature and reliable (English Patent No.1,249,252 (1971/10/13)).For with glass-fiber-reinforced polyester to the formation of forming materials performance, product surface clouding and the detrimentally affect that restriction caused of polyester viscosity, comparatively ideal solution (U.S. Patent No. 1,249,252 (1971/10/13)) has also been arranged at present
In all problems that the glass-fiber-reinforced polyester material must solve, study the improvement problem of maximum interface bonding situations.
U.S. Patent No. 4,487,797 and No.4,745, all introduced a kind of used water in 028 and done the surface treatment agent that the epoxy compounds of dispersion agent, emulsifying agent or solvent and a kind of glass fibre form with coupling agent and a kind of propylene oxide-ethylene oxide copolymer and come glass fibre is carried out surface treatment, and polyester has been strengthened with this.In the component of this surface treatment agent by a kind of coupling agent (U.S. Patent No. 4,745,028) that becomes epoxy Polyurethanes and one or more organic metal salts to form by isocyanate or the end capped water of ester crosslinked group.U.S. Patent No. 4,276,208 have introduced that a kind of usefulness contains the epoxy compounds of two epoxide groups at least such as the salt of bisphenol-A epoxy compounds or bisphenol-f epoxy compounds etc. and a kind of montanin wax comes glass fibre is carried out surface treatment as surface treatment agent, and with this to polyester enhanced method.This patent is also pointed out simultaneously, after the epoxy compounds that uses this kind to contain two epoxide groups at least comes as surface treatment agent glass fibre carried out surface treatment, if 5% of adding weight polyester percentage composition identical epoxy compounds in the glass-fiber-reinforced polyester system then will further significantly improve the various aspects of performance of gained material again.
That Japanese Patent No.53/144954, No.53/144955, No.53/143649, No.53/106750 and No.53/106749 have reported is two with containing-or the surface treatment agent of three-isocyanate or ester glass fibre is carried out the surface-treated method.Two in the above-mentioned patent-or three-isocyanate or ester all as the linking agent of polyester, rather than as the coupling agent of glass fibre.U.S. Patent No. 4,990,549 further proposed two-or three-isocyanate or ester role in the glass-fiber-reinforced polyester system be exactly a kind of effect of coupling agent.By two-or tensile strength, flexural strength, anti-non-notch that three-isocyanate or ester can significantly improve material impact and notch shock.
Improving aspect the interface bonding situation of glass-fiber-reinforced polyester storeroom, above-mentioned patent mainly all adopts directly from how increasing the functionality coating that one deck is fit to polyester to glass fibre, thus the interface agglutinating method between raising glass fibre and the polyester.An obvious deficiency of this method is the complicacy that has increased technology, thereby has caused the rising of production cost.
Summary of the invention
The purpose of this invention is to provide that a kind of preparation technology is simple, cost is low, the matrix material of the glass-fiber-reinforced polyester of excellent performance, improving the interface agglutinating complex process between glass fibre and the polyester, the shortcoming that cost is high to overcome prior art.
The present invention finds, a kind of commercially available ethylene copolymer that contains epoxy-functional can be used as the properties-correcting agent of glass-fiber-reinforced polyester material, by can distinguish on this modifier molecules chain can and the functional group of polyester and the glass fibre effect handled through silane coupling agent KH550, directly reach interface agglutinating purpose between raising glass fibre and the polyester.In addition, this properties-correcting agent can also play toughening effect efficiently to the glass-fiber-reinforced polyester material when addition reaches certain proportion, thereby produces high impact-resistant glass-fiber-reinforced polyester matrix material.
The composition (weight %) of the matrix material of the glass-fiber-reinforced polyester that the present invention proposes is as follows:
Polyester 45-87
Nucleator 1-3.5
Toughness reinforcing, chainextender 1.5-20
Oxidation inhibitor 0.1-1
Glass fibre 10-37
In the above-mentioned composite-material formula, nucleator is a relative density 1.14～1.15, nylon 6 that fusing point is 215～225 ℃ or relative density 1.10～1.15, nylon 66 that fusing point is 250～270 ℃ or relative density 2.7～2.8, the talcum powder of order several 1250～2500; Toughness reinforcing, chainextender produces for Dupont company, and trade names are the ethylene copolymer that contains epoxy-functional of Elvaloy PTW; Glass fibre is handled through silane coupling agent KH55, and diameter is the 6-17 micron, and wherein silane coupling agent KH550 is that Yaohua Glass-making Plant, Shanghai produces, and chemical name is a γ-An Bingjisanyiyangjiguiwan; Oxidation inhibitor produces for Ciba company, and trade names are Irganox 1010, and chemical name is four [β-(3,5-di-tert-butyl-4-hydroxy phenyl) propionic acid] pentaerythritol ester; Polyester is a relative density 1.30～1.38,255～260 ℃ of fusing points, the polyethylene terephthalate of melt viscosity 0.3～0.6 or relative density 1.31～1.55,220～230 ℃ of fusing points, the polybutylene terephthalate of melt viscosity 0.3～0.6.
Among the present invention, interfacial adhesion between polyester and the glass fibre is strong, simultaneously owing to the ethylene copolymer that contains epoxy-functional is effective to the polyester chain extension, and this properties-correcting agent has played toughening effect efficiently to the glass-fiber-reinforced polyester material when addition reaches certain proportion, it is fast that nucleator makes crystallizing polyester speed in addition, make the composite materials property excellence that makes, and cost is low, easily processing.
Embodiment
According to the prescription of above-mentioned matrix material pre-dry polyester, nucleator, toughness reinforcing, chainextender, oxidation inhibitor are done under room temperature state in super mixer in proportion and mixed, afterwards, in twin screw extruder, be that the glass fibre of 6-17 micron is with the suitable proportion blending again with diameter, through melt extrude, granulation, can be made into the matrix material that the present invention proposes.Wherein, each the heating region temperature setting of the screw rod of polyethylene terephthalate is respectively: 245～250 ℃ in a district, 250～255 ℃ in two districts, 250～255 ℃ in three districts, 245～250 ℃ in four districts; Each the heating region temperature setting of the screw rod of polybutylene terephthalate is respectively: 230～235 ℃ in a district, 235～240 ℃ in two districts, 235～240 ℃ in three districts, 230～235 ℃ in four districts.
Beneficial effect
1, the present invention uses toughness reinforcing, chainextender in the matrix material of glass-fiber-reinforced polyester, and prepared composite property excellence has characteristics such as easy processing, high impact strength and modulus height.
2, the present invention adopts cheap commercially available organism as nucleator, and component such as toughness reinforcing, chainextender and oxidation inhibitor has reduced production cost of products.
3, the preparation technology of the matrix material of the glass-fiber-reinforced polyester of the present invention's proposition is simple, cost is low.
Embodiment 1
With the PET weight ratio be 65.4%, talcum powder 2%, PTW (toughness reinforcing, chainextender) 2.5% and 1010 (oxidation inhibitor) 0.1% do under room temperature state in super mixer and mix, afterwards, glass fibre (diameter 6-17 micron) 30% blending of handling through coupling agent KH550 with the surface at twin screw extruder again, melt extrude through 260～280 ℃, matrix material is made in granulation.Wherein, each heating region temperature setting of screw rod is respectively: 245～250 ℃ in a district, 250～255 ℃ in two districts, 250～255 ℃ in three districts, 245～250 ℃ in four districts.
Embodiment 2
With the PET weight ratio be 62.9%, talcum powder 2%, PTW (toughness reinforcing, chain extension) 5% and 1010 (oxidation inhibitor) 0.1% do under room temperature state in super mixer and mix, afterwards, glass fibre (diameter 6-17 micron) 30% blending of handling through coupling agent KH550 with the surface at twin screw extruder again, through melt extruding, matrix material is made in granulation.Wherein, each heating region temperature setting of screw rod is respectively: 245～250 ℃ in a district, 250～255 ℃ in two districts, 250～255 ℃ in three districts, 245～250 ℃ in four districts.
Embodiment 3
With the PET weight ratio be 57.9%, talcum powder 2%, PTW (toughness reinforcing, chain extension) 10% and 1010 (oxidation inhibitor) 0.1% do under room temperature state in super mixer and mix, afterwards, glass fibre (diameter 6-17 micron) 30% blending of handling through coupling agent KH550 with the surface at twin screw extruder again, through melt extruding, matrix material is made in granulation.Wherein, each heating region temperature setting of screw rod is respectively: 245～250 ℃ in a district, 250～255 ℃ in two districts, 250～255 ℃ in three districts, 245～250 ℃ in four districts.
Embodiment 4
With the PET weight ratio be 52.9%, talcum powder 2%, PTW (toughness reinforcing, chain extension) 15% and 1010 (oxidation inhibitor) 0.1% do under room temperature state in super mixer and mix, afterwards, glass fibre (diameter 6-17 micron) 30% blending of handling through coupling agent KH550 with the surface at twin screw extruder again, through melt extruding, matrix material is made in granulation.Wherein, each heating region temperature setting of screw rod is respectively: 245～250 ℃ in a district, 250～255 ℃ in two districts, 250～255 ℃ in three districts, 245～250 ℃ in four districts.
Embodiment 5
With the PET weight ratio be 47.9%, talcum powder 2%, PTW (toughness reinforcing, chain extension) 20% and 1010 (oxidation inhibitor) 0.1% do under room temperature state in super mixer and mix, afterwards, glass fibre (diameter 6-17 micron) 30% blending of handling through coupling agent KH550 with the surface at twin screw extruder again, through melt extruding, matrix material is made in granulation.Wherein, each heating region temperature setting of screw rod is respectively: 245～250 ℃ in a district, 250～255 ℃ in two districts, 250～255 ℃ in three districts, 245～250 ℃ in four districts.
Comparative Examples
With the PET weight ratio be 67.9%, talcum powder 2% and 1010 (oxidation inhibitor) 0.1% does under room temperature state in super mixer and mixes, afterwards, glass fibre (diameter 6-17 micron) 30% blending of handling through coupling agent KH550 with the surface at twin screw extruder again, through melt extruding, matrix material is made in granulation.Wherein, each heating region temperature setting of screw rod is respectively: 245～250 ℃ in a district, 250～255 ℃ in two districts, 250～255 ℃ in three districts, 245～250 ℃ in four districts.
The prescription and the Mechanics Performance Testing of embodiment 1-5 and Comparative Examples the results are shown in following table:
Watch glass fiber reinforced polyester composite-material formula and material property table
| The matrix material title | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | Comparative Examples |
| ?PET(％) | ??65.4 | ??62.9 | ??57.9 | ??52.9 | ??47.9 | ??67.9 |
| Talcum powder (%) | ??2 | ??2 | ??2 | ??2 | ??2 | ??2 |
| ?PTW(％) | ??2.5 | ??5 | ??10 | ??15 | ??20 | ??- |
| ?1010(％) | ??0.1 | ??0.1 | ??0.1 | ??0.1 | ??0.1 | ??0.1 |
| Glass (%) | ??30 | ??30 | ??30 | ??30 | ??30 | ??30 |
| IZOD impacts (non-notch J/m) | ??240 | ??400 | ??600 | ??720 | ??1200 | ??280 |
| Charpy U impacts (non-notch kJ/m 2) | ??22 | ??33 | ??82 | ??95 | ??120 | ??16 |
| Tensile strength (MPa) | ??162 | ??138 | ??106 | ??98 | ??93 | ??135 |
| Elongation at break (%) | ??4.2 | ??5.0 | ??5.5 | ??7.0 | ??8.6 | ??2.0 |
| Modulus in flexure (MPa) | ??11270 | ??9850 | ??8300 | ??7500 | ??6950 | ??8100 |
Last table shows, uses PTW can play effect toughness reinforcing, chain extension in the matrix material of glass-fiber-reinforced polyester.Comparative example 1,2 and Comparative Examples are as can be known, when the PTW consumption is between 2.5～5.0, this toughness reinforcing, chain extension effect reaches a good equilibrium state, macro manifestations is greatly improved at the tensile strength of material not only and modulus in flexure, extension at break, and the resistance to impact shock of material and elongation at break all are significantly improved.And when the consumption of PTW during greater than 5 parts, by embodiment 3～5 and Comparative Examples as can be known because the flexibility of PTW self, at this moment the toughening effect of PTW obviously will be higher than it to chain extension effect that material rose, though macro manifestations all has great raising at the resistance to impact shock and the elongation at break of material, but the tensile strength and the modulus in flexure of material reduce significantly, yet this reduction is an acceptable for the glass fiber reinforced materials that the high-impact requirement is arranged.
Claims (8)
1. the matrix material of a glass-fiber-reinforced polyester, its composition (weight %) is:
Polyester 45-87
Nucleator 1-3.5
Toughness reinforcing, chainextender 1.5-20
Oxidation inhibitor 0.1-1
Glass fibre 10-37
In the above-mentioned composite-material formula, nucleator is a relative density 1.14～1.15, nylon 6 that fusing point is 215～225 ℃ or relative density 1.10～1.15, nylon 66 that fusing point is 250～270 ℃ or relative density 2.7～2.8, the talcum powder of order several 1250～2500; Toughness reinforcing, chainextender produces for Dupont company, and trade names are the ethylene copolymer that contains epoxy-functional of Elvaloy PTW; Glass fibre is handled through silane coupling agent KH55, and diameter is the 6-17 micron, and wherein silane coupling agent KH550 is that Yaohua Glass-making Plant, Shanghai produces, and chemical name is a γ-An Bingjisanyiyangjiguiwan; Oxidation inhibitor produces for Ciba company, and trade names are Irganox 1010, and chemical name is four [β-(3,5-di-tert-butyl-4-hydroxy phenyl) propionic acid] pentaerythritol ester; Polyester is a relative density 1.30～1.38,255～260 ℃ of fusing points, the polyethylene terephthalate of melt viscosity 0.3～0.6 or relative density 1.31～1.55,220～230 ℃ of fusing points, the polybutylene terephthalate of melt viscosity 0.3～0.6.
2. the matrix material of glass-fiber-reinforced polyester according to claim 1, wherein nucleator is a relative density 1.14～1.15, nylon 6 that fusing point is 215～225 ℃ or relative density 1.10～1.15, nylon 66 that fusing point is 250～270 ℃ or relative density 2.7～2.8, the talcum powder of order several 1250～2500.
3. the matrix material of glass-fiber-reinforced polyester according to claim 1, wherein toughness reinforcing, chainextender are that Dupont company produces, and trade names are the ethylene copolymer that contains epoxy-functional of Elvaloy PTW.
4. the matrix material of glass-fiber-reinforced polyester according to claim 1, wherein glass fibre is through handling through silane coupling agent KH550, and diameter is the 6-17 micron.
5. the matrix material of glass-fiber-reinforced polyester according to claim 1, wherein silane coupling agent KH550 is that Yaohua Glass-making Plant, Shanghai produces, chemical name is a γ-An Bingjisanyiyangjiguiwan;
6. the matrix material of glass-fiber-reinforced polyester according to claim 1, oxidation inhibitor are that Ciba company produces, and trade names are Irganox 1010, and chemical name is four [β-(3,5-di-tert-butyl-4-hydroxy phenyl) propionic acid] pentaerythritol ester;
7. the matrix material of glass-fiber-reinforced polyester according to claim 1, wherein polyester is a relative density 1.30～1.38,255～260 ℃ of fusing points, the polyethylene terephthalate of melt viscosity 0.3～0.6 or relative density 1.31～1.55,220～230 ℃ of fusing points, the polybutylene terephthalate of melt viscosity 0.3～0.6.
8. the preparation method of the matrix material of the described glass-fiber-reinforced polyester of claim 1, its step is with polyester 45～87%, nucleator 1～3.5%, toughness reinforcing, chainextender 1.5～20%, oxidation inhibitor 0.1～1% is done in super mixer and is mixed, melt extrude granulation at the same glass fibre of twin screw extruder (diameter 6-17 micron) 10～37% through 260～280 ℃ again.
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| Application Number | Priority Date | Filing Date | Title |
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| CNB021362505A CN1195016C (en) | 2002-07-29 | 2002-07-29 | Fibreglass reinforced polyester composite material and preparing method thereof |
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|---|---|---|---|
| CNB021362505A CN1195016C (en) | 2002-07-29 | 2002-07-29 | Fibreglass reinforced polyester composite material and preparing method thereof |
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| CN1472254A true CN1472254A (en) | 2004-02-04 |
| CN1195016C CN1195016C (en) | 2005-03-30 |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN100412133C (en) * | 2004-04-15 | 2008-08-20 | 上海普利特复合材料有限公司 | Flame retardant fiberglass enhanced PCT composite materal in low smoke |
| CN100448929C (en) * | 2004-04-15 | 2009-01-07 | 上海普利特复合材料有限公司 | Anti color distortion PDT material enhanced by halogeton flame retardant fiberglass |
| CN101070421B (en) * | 2006-12-22 | 2010-09-08 | 深圳市科聚新材料有限公司 | High-heat-resisting glass-fiber reinforced polyester composite material and preparing method |
| CN101225220B (en) * | 2007-12-25 | 2011-08-31 | 南通市东方实业有限公司 | Flame-retardant reinforced polybutylene terephthalate compound and production method thereof |
| CN102828654A (en) * | 2012-04-27 | 2012-12-19 | 山东国强五金科技股份有限公司 | Standard lever handle for plastic-steel doors and windows |
| CN106633677A (en) * | 2016-12-05 | 2017-05-10 | 钦州市钦南区生产力促进中心 | Glass fiber material and preparation method thereof |
| CN110713700A (en) * | 2018-07-13 | 2020-01-21 | 南通星辰合成材料有限公司 | Polyester composite material and preparation method and application thereof |
| CN113459623A (en) * | 2021-06-22 | 2021-10-01 | 安徽国风塑业股份有限公司 | High-temperature-resistant transparent polyester film and preparation method thereof |
| CN114643768A (en) * | 2022-04-21 | 2022-06-21 | 杭州和顺科技股份有限公司 | Food-grade air-resistance light-transmitting multilayer film |
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- 2002-07-29 CN CNB021362505A patent/CN1195016C/en not_active Expired - Lifetime
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| CN100412133C (en) * | 2004-04-15 | 2008-08-20 | 上海普利特复合材料有限公司 | Flame retardant fiberglass enhanced PCT composite materal in low smoke |
| CN100448929C (en) * | 2004-04-15 | 2009-01-07 | 上海普利特复合材料有限公司 | Anti color distortion PDT material enhanced by halogeton flame retardant fiberglass |
| CN101070421B (en) * | 2006-12-22 | 2010-09-08 | 深圳市科聚新材料有限公司 | High-heat-resisting glass-fiber reinforced polyester composite material and preparing method |
| CN101225220B (en) * | 2007-12-25 | 2011-08-31 | 南通市东方实业有限公司 | Flame-retardant reinforced polybutylene terephthalate compound and production method thereof |
| CN102828654A (en) * | 2012-04-27 | 2012-12-19 | 山东国强五金科技股份有限公司 | Standard lever handle for plastic-steel doors and windows |
| CN106633677A (en) * | 2016-12-05 | 2017-05-10 | 钦州市钦南区生产力促进中心 | Glass fiber material and preparation method thereof |
| CN110713700A (en) * | 2018-07-13 | 2020-01-21 | 南通星辰合成材料有限公司 | Polyester composite material and preparation method and application thereof |
| CN113459623A (en) * | 2021-06-22 | 2021-10-01 | 安徽国风塑业股份有限公司 | High-temperature-resistant transparent polyester film and preparation method thereof |
| CN114643768A (en) * | 2022-04-21 | 2022-06-21 | 杭州和顺科技股份有限公司 | Food-grade air-resistance light-transmitting multilayer film |
| CN114643767A (en) * | 2022-04-21 | 2022-06-21 | 杭州和顺科技股份有限公司 | Wear-resistant light-transmitting multilayer container and manufacturing method thereof |
| CN114643768B (en) * | 2022-04-21 | 2024-04-26 | 杭州和顺科技股份有限公司 | Food-grade air-resistance light-transmitting multilayer film |
| CN114643767B (en) * | 2022-04-21 | 2024-07-02 | 杭州和顺科技股份有限公司 | Wear-resistant light-transmitting multilayer container and manufacturing method thereof |
| CN114889284A (en) * | 2022-04-24 | 2022-08-12 | 杭州和顺科技股份有限公司 | High-barrier heat-resistant multilayer film and manufacturing method thereof |
| CN114889284B (en) * | 2022-04-24 | 2024-06-14 | 杭州和顺科技股份有限公司 | High-barrier heat-resistant multilayer film and manufacturing method thereof |
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Address after: No. 421, Lane 20, Siping Road, Shanghai Patentee after: Shanghai Pret Composites Co.,Ltd. Address before: No. 421, Lane 20, Siping Road, Shanghai Patentee before: PULITE COMPOSITE MATERIAL Co. L |
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Effective date of registration: 20190107 Address after: 402560 Longyun Road, Pulu Industrial Park, Tongliang District, Chongqing Co-patentee after: Shanghai Pret Composites Co.,Ltd. Patentee after: CHONGQNG PULITE NEW MATERIAL Co.,Ltd. Co-patentee after: ZHEJIANG PRET NEW MATERIALS Co.,Ltd. Address before: 200081 No. 20, Lane 421, Siping Road, Shanghai Patentee before: Shanghai Pret Composites Co.,Ltd. |
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Granted publication date: 20050330 |
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