CN102040808B - Glass fiber enhanced PET/PBT (Polyethylene Terephthalate)/(Polybutylene Terephthalate) alloy with high glossiness and low warping degree and preparation method thereof - Google Patents
Glass fiber enhanced PET/PBT (Polyethylene Terephthalate)/(Polybutylene Terephthalate) alloy with high glossiness and low warping degree and preparation method thereof Download PDFInfo
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- CN102040808B CN102040808B CN2010105902210A CN201010590221A CN102040808B CN 102040808 B CN102040808 B CN 102040808B CN 2010105902210 A CN2010105902210 A CN 2010105902210A CN 201010590221 A CN201010590221 A CN 201010590221A CN 102040808 B CN102040808 B CN 102040808B
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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
- B29C48/88—Thermal treatment of the stream of extruded material, e.g. cooling
- B29C48/911—Cooling
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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
- B29C48/001—Combinations of extrusion moulding with other shaping operations
- B29C48/0022—Combinations of extrusion moulding with other shaping operations combined with cutting
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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
Abstract
The invention discloses a glass fiber enhanced PET/PBT (Polyethylene Terephthalate)/(Polybutylene Terephthalate) alloy with high glossiness and low warping degree and a preparation method thereof. The PET/PBT alloy comprises the following components by mass percentage content: 15-60% of PBT, 19-60% of PET, 3-10% of compatilizer, 0.3-0.9% of antioxygen, 0.5-1% of nucleating accelerating agent, 3-8% of composite nucleating agent, 10-30% of glass fiber and 0.4-1% of processing aid. According to the invention, the PET and the PBT are fused to obtain the PET/PBT alloy, and the PET/PBT alloy has the advantages of quick crystallizing speed rate, good physical performance, high distortion temperature, high surface glossiness, low contractibility rate, stable dimension, low warping degree and lower cost; and the PET/PBT alloy of the invention can be used for completely replacing the bakelite powder under a specific occasion.
Description
Technical field
The present invention relates to the thermoplastic macromolecule material technical field, relate in particular to the low warp glass fiber REINFORCED PET of a kind of high gloss/PBT Alloy And Preparation Method.
Background technology
PET (poly ethylene terephthalate, polyethylene terephthalate) realizes industrialized linear thermoplastic's polymkeric substance by Dupont company nineteen fifty-three the earliest, is a kind of crystalline high polymer with higher melt temperature (Tm) and second-order transition temperature (Tg); Can in awide temperature range, keep good physicals and mechanical property, its resistance to fatigue, rub resistance are good, and stability to aging is excellent; Electrical insulating property is outstanding; Stable to most of organic solvents and mineral acid, and production energy consumption is very low, and processibility is good; Thereby be widely used in fields such as synthon, film and engineering plastics; But because the rigidity of PET makes its crystallization velocity slower, the shortcoming that forming mould temperature height and shaping cycle are long makes it be restricted in the engineering plastics Application for Field.
And PBT (poly butylene terephthalate, polybutylene terephthalate) molecule segment flexibility is better than PET, and mechanical property is good, heat-drawn wire is low, crystallization rate is very fast.
Therefore, research and development PET/PET alloy has important significance for theories and practical value.And at present in the prior art, bakelite belongs to thermosetting resin, have be difficult for reclaiming, than great, shortcomings such as color single (being grey black), character are more crisp, processing difficulties, therefore, substitute how to seek bakelite also is a problem demanding prompt solution.
Summary of the invention
The invention provides the low warp glass fiber REINFORCED PET of a kind of high gloss/PBT Alloy And Preparation Method, this alloy crystallization rate is fast, mechanical property and heat-drawn wire is high, surface gloss is high, shrinking percentage is low, dimensional stabilizing, low warpage, cost are lower, can substitute bakelite uses.
Technical scheme of the present invention is:
A kind of high gloss hangs down warp glass fiber REINFORCED PET/PBT alloy, and is composed of the following components by the quality percentage composition:
PBT 15～60％
PET 19～60％
Compatilizer 3～10%
Oxidation inhibitor 0.3～0.9%
Nucleation accelerating agent 0.5～1%
Composite nucleating agent 3～8%
Spun glass 10～30%
Processing aid 0.4～1%.
Above-mentioned high gloss hangs down the preparation method of warp glass fiber REINFORCED PET/PBT alloy, comprising:
Step 1, take by weighing each component by above-mentioned quality percentage composition, and with the PET that takes by weighing and PBT in 110～130 ℃ of temperature following time of drying more than 4 hours, other components are dry more than 2 hours under 60～80 ℃ of temperature;
Step 2, the PET with after the drying treatment, PBT, compatilizer, oxidation inhibitor, nucleation accelerating agent, composite nucleating agent and processing aid are put into high-speed mixer and are mixed, and stir 5～15min at normal temperatures;
Step 3, the mixed material of step 2 is joined in the hopper of twin screw extruder, spun glass is added inlet from the glass in twin screw stage casing add, through melt blending extrude, water-cooled, air-dry, pelletizing;
Wherein, the temperature of twin screw extruder is set to: a district: 200～210 ℃; Two districts: 210～220 ℃; Three districts: 220～230 ℃; District: 230～240 ℃; Five districts: 240～250 ℃; Six districts: 240～250 ℃; Seven districts: 240～250 ℃; Eight districts: 250～260 ℃; Head temperature: 240～250 ℃; Screw speed is controlled at 200～400r/min.
The present invention adopts composite nucleating agent; Be aided with nucleation accelerating agent PET and PBT fusion are made the PET/PBT alloy; Effectively promoted the fusion of PET and PBT; And this PET/PBT alloy crystallization rate is fast, mechanical property good and heat-drawn wire is high, surface gloss is high, shrinking percentage is low, dimensional stabilizing, low warpage, cost are lower, can be applied to fields such as electronic apparatus, automobile; And under certain occasion, can substitute the use of bakelite fully with PBT/PET alloy of the present invention, can overcome the shortcoming of bakelite, and surperficial texture can be the same with bakelite.
Embodiment
PET of the present invention and PBT fusion make the PET/PBT alloy, and this PET/PBT alloy is composed of the following components by the quality percentage composition:
PBT 15～60％
PET 19～60％
Compatilizer 0～10%
Oxidation inhibitor 0.3～0.9%
Nucleation accelerating agent 0.5～1%
Composite nucleating agent 3～8%
Spun glass 10～30%
Processing aid 0.4～1%.
The present invention adopts composite nucleating agent, is aided with nucleation accelerating agent PET and PBT fusion are made the PET/PBT alloy, has effectively promoted the fusion of PET and PBT.
Wherein PET can be the isoviscous resin of middle height, limiting viscosity 0.83～0.92 deciliter/gram; PBT can be the isoviscous resin of middle height, limiting viscosity 0.98～1.1 deciliter/gram; Compatilizer can be in ethylene-methacrylic acid copolymer EMA or the ethylene-methyl acrylate-glycidyl methacrylate copolymer a kind of;
Oxidation inhibitor can be mixed by primary antioxidant four [β-(3, the 5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester and auxiliary antioxidant tricresyl phosphite (24-di-tert-butyl-phenyl) ester;
Nucleation accelerating agent can be organic nucleation accelerating agent, and like macromole carboxylic acid and its esters, TRIMETHOXY BENZOIC ACID (FOR MANUFACTURING OF T.M. sodium salt etc., this nucleation accelerating agent has the reduction melting viscosity, promotes crystallization velocity, promotes the effects such as dispersion of each component;
Composite nucleating agent can be mixed by Bruggemann P250 (the optimization mixture of the nucleation-accelerant of a kind of organic composition and inorganic components) and 3500 purpose talcum powder, and this talcum powder is the ultra-fine inorganic filler, has nucleogenesis;
Spun glass can be long fine for alkali-free, and diameter is: 9～14 μ m; Processing aid can be mutual-phenenyl two acid bromide two alcohol ester's cyclic oligomer, and such as the U.S. CBT of Cyclics company functional resin, this product has big ring oligomerization ester structure, can increase substantially the flowability and the processibility of product.
The preparation method of PET/PBT alloy of the present invention comprises:
Step 1, take by weighing each component by above-mentioned described quality percentage composition, and with the PET that takes by weighing and PBT in 110～130 ℃ of temperature following time of drying more than 4 hours, other components are dry more than 2 hours under 60～80 ℃ of temperature; This is because PET and PBT are prone to the moisture absorption, therefore, before blending and modifying, must carry out drying treatment to it;
Step 2, the PET with after the drying treatment, PBT, compatilizer, oxidation inhibitor, nucleation accelerating agent, composite nucleating agent and processing aid are put into high-speed mixer and are mixed, and stir 5～15min at normal temperatures;
Step 3, the mixed material of step 2 is joined in the hopper of twin screw extruder, spun glass is added inlet from the glass in twin screw stage casing add, through melt blending extrude, water-cooled, air-dry, pelletizing; Twin screw extruder can be used parallel double-screw extruder, screw diameter 35-75mm;
Wherein, the temperature of twin screw extruder is set to: a district: 200～210 ℃; Two districts: 210～220 ℃; Three districts: 220～230 ℃; Four districts: 230～240 ℃; Five districts: 240～250 ℃; Six districts: 240～250 ℃; Seven districts: 240～250 ℃; Eight districts: 250～260 ℃; Head temperature: 240～250 ℃; Screw speed is controlled at 200～400r/min.
Below in conjunction with embodiment the present invention is done a detailed elaboration.Wherein in following each embodiment, main anti-oxidant and auxiliary antioxidant are respectively the Irganox 1010 and 168 that Switzerland's vapour crust produces; Nucleation accelerating agent adopts organic nucleation accelerating agent, trade names POLYCIZER A55; Composite nucleating agent is mixed by Bruggemann P250 and 3500 purpose talcum powder; Processing aid is the CBT functional resin of U.S. Cyclics company.
Embodiment one
With PET and PBT 110 ℃ dry 4 hours down, remaining auxiliary agent 70 ℃ dry 2 hours down.Take by weighing PET 40.5kg, PBT 35kg, compatilizer 4kg, composite nucleating agent 3kg (wherein P2500.5kg, talcum powder 3kg), nucleation accelerating agent 1kg, antioxidant 1010 0.3kg, 1680.3kg, lubricant CBT 0.9kg; In high-speed mixer, mix 10min then.The material that mixes joins in the hopper of twin screw extruder, controls each section temperature and exists: a district: 210 ℃; Two districts: 220 ℃; Three districts: 230 ℃; Four districts: 240 ℃; Five districts: 250 ℃; Six districts: 240 ℃; Seven districts: 240 ℃; Eight districts: 230 ℃; Head temperature: 250 ℃, screw speed 350r/min adds inlet with spun glass 15kg from the glass in twin screw stage casing and adds, through melt blending extrude, water-cooled, air-dry, pelletizing, last bag becomes glass REINFORCED PET/PBT alloy finished product.
Embodiment two
With PET and PBT 120 ℃ dry 4 hours down, remaining auxiliary agent 60 ℃ dry 2 hours down.Take by weighing PET 30kg, PBT 30.3kg, compatilizer 10kg, composite nucleating agent 8kg (wherein P2505kg, talcum powder 3kg), nucleation accelerating agent 1kg, antioxidant 1010 0.1kg, 1680.2kg, lubricant CBT 0.4kg; In high-speed mixer, mix 10min then.The material that mixes joins in the hopper of twin screw extruder, controls each section temperature and exists: a district: 210 ℃; Two districts: 220 ℃; Three districts: 230 ℃; Four districts: 240 ℃; Five districts: 250 ℃; Six districts: 250 ℃; Seven districts: 240 ℃; Eight districts: 230 ℃; Head temperature: 250 ℃, screw speed 320r/min adds inlet with spun glass 20kg from the glass in twin screw stage casing and adds, through melt blending extrude, water-cooled, air-dry, pelletizing, last bag becomes glass REINFORCED PET/PBT alloy finished product.
Embodiment three
With PET and PBT 130 ℃ dry 4 hours down, remaining auxiliary agent 80 ℃ dry 2 hours down.Take by weighing PET 60kg, PBT 15kg, compatilizer 3kg, composite nucleating agent 4.6kg (wherein P2500.8kg, talcum powder 3.8kg), nucleation accelerating agent 0.5kg, antioxidant 1010 0.3kg, 1680.6kg, lubricant CBT 1kg; In high-speed mixer, mix 10min then.The material that mixes joins in the hopper of twin screw extruder, controls each section temperature and exists: a district: 210 ℃; Two districts: 220 ℃; Three districts: 230 ℃; Four districts: 240 ℃; Five districts: 250 ℃; Six districts: 240 ℃; Seven districts: 240 ℃; Eight districts: 230 ℃; Head temperature: 250 ℃, screw speed 200r/min adds inlet with spun glass 15kg from the glass in twin screw stage casing and adds, through melt blending extrude, water-cooled, air-dry, pelletizing, last bag becomes glass REINFORCED PET/PBT alloy finished product.
Embodiment four
With PET and PBT 110 ℃ dry 4 hours down, remaining auxiliary agent 70 ℃ dry 2 hours down.Take by weighing PET 19kg, PBT 60kg, compatilizer 3.2kg, composite nucleating agent 5.5kg (wherein P2505.5kg), nucleation accelerating agent 1kg, antioxidant 1010 0.3kg, 1680.6kg, lubricant CBT 0.4kg; In high-speed mixer, mix 10min then.The material that mixes joins in the hopper of twin screw extruder, controls each section temperature and exists: a district: 210 ℃; Two districts: 220 ℃; Three districts: 230 ℃; Four districts: 240 ℃; Five districts: 250 ℃; Six districts: 240 ℃; Seven districts: 240 ℃; Eight districts: 230 ℃; Head temperature: 250 ℃, screw speed 400r/min adds inlet with spun glass 10kg from the glass in twin screw stage casing and adds, through melt blending extrude, water-cooled, air-dry, pelletizing, last bag becomes glass REINFORCED PET/PBT alloy finished product.
Embodiment five
With PET and PBT 110 ℃ dry 4 hours down, remaining auxiliary agent 70 ℃ dry 2 hours down.Take by weighing PET 40kg, PBT 20.7kg, compatilizer 3.5kg, composite nucleating agent 3.5kg (wherein P2500.5kg, talcum powder 3kg), nucleation accelerating agent 1kg, antioxidant 1010 0.3kg, 1680.6kg, lubricant CBT 0.4kg; In high-speed mixer, mix 10min then.The material that mixes joins in the hopper of twin screw extruder, controls each section temperature and exists: a district: 210 ℃; Two districts: 220 ℃; Three districts: 230 ℃; Four districts: 240 ℃; Five districts: 250 ℃; Six districts: 240 ℃; Seven districts: 240 ℃; Eight districts: 230 ℃; Head temperature: 250 ℃, screw speed 320r/min adds inlet with spun glass 30kg from the glass in twin screw stage casing and adds, through melt blending extrude, water-cooled, air-dry, pelletizing, last bag becomes glass REINFORCED PET/PBT alloy finished product.
Embodiment six
With PET and PBT 110 ℃ dry 4 hours down, remaining auxiliary agent 70 ℃ dry 2 hours down.Take by weighing PET 20.7kg, PBT 40kg, compatilizer 3.5kg, composite nucleating agent 3.5kg (wherein P2500.5kg, talcum powder 3kg), nucleation accelerating agent 1kg, antioxidant 1010 0.3kg, 1680.6kg, lubricant CBT 0.4kg; In high-speed mixer, mix 10min then.The material that mixes joins in the hopper of twin screw extruder, controls each section temperature and exists: a district: 210 ℃; Two districts: 220 ℃; Three districts: 230 ℃; Four districts: 240 ℃; Five districts: 250 ℃; Six districts: 240 ℃; Seven districts: 240 ℃; Eight districts: 240 ℃; Head temperature: 250 ℃, screw speed 320r/min adds inlet with spun glass 30kg from the glass in twin screw stage casing and adds, through melt blending extrude, water-cooled, air-dry, pelletizing, last bag becomes glass REINFORCED PET/PBT alloy finished product.
The PET/PBT alloy of embodiment one to six is injection molded into standard test specimen, and test performance is as shown in table 1 below:
Table 1
Can find out from last table 1, the PET/PBT alloy that the present invention makes, the mechanical property aspect tensile strength, extension at break degree, modulus in flexure, flexural strength and shock strength is relatively good, dimensional stabilizing, low warpage; Heat-drawn wire is than higher, and surface luster is good; Vertically/horizontal molding shrinkage is lower, crystallization rate is also than comparatively fast; Merged the advantage of PBT and PET fully; Can be applied to fields such as electronic apparatus, automobile; And under certain occasion, can substitute the use of bakelite fully with PBT/PET alloy of the present invention, can overcome the shortcoming of bakelite, and surperficial texture can be the same with bakelite.
Above-described embodiment of the present invention does not constitute the qualification to protection domain of the present invention.Any modification of within spirit of the present invention and principle, being done, be equal to replacement and improvement etc., all should be included within the claim protection domain of the present invention.
Claims (7)
1. the low warp glass fiber REINFORCED PET of high gloss/PBT alloy is characterized in that, and is composed of the following components by the quality percentage composition:
Described PET is the isoviscous resin of middle height, limiting viscosity 0.83～0.92 deciliter/gram; Described PBT is the isoviscous resin of middle height, limiting viscosity 0.98～1.1 deciliter/gram; Described processing aid is mutual-phenenyl two acid bromide two alcohol ester's a cyclic oligomer.
2. high gloss according to claim 1 hangs down warp glass fiber REINFORCED PET/PBT alloy, it is characterized in that: compatilizer is a kind of in ethylene-methacrylic acid copolymer EMA or the ethylene-methyl acrylate-glycidyl methacrylate copolymer.
3. high gloss according to claim 1 hangs down warp glass fiber REINFORCED PET/PBT alloy; It is characterized in that: oxidation inhibitor is mixed by primary antioxidant four [β-(3, the 5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester and auxiliary antioxidant tricresyl phosphite (24-di-tert-butyl-phenyl) ester.
4. high gloss according to claim 1 hangs down warp glass fiber REINFORCED PET/PBT alloy, and it is characterized in that: nucleation accelerating agent is organic nucleation accelerating agent.
5. high gloss according to claim 1 hangs down warp glass fiber REINFORCED PET/PBT alloy, it is characterized in that: composite nucleating agent is mixed by Bruggemann P250 and 3500 purpose talcum powder.
6. high gloss according to claim 1 hangs down warp glass fiber REINFORCED PET/PBT alloy, it is characterized in that: spun glass is that alkali-free is long fine, and diameter is: 9～14 μ m.
7. the preparation method like the low warp glass fiber REINFORCED PET of the described high gloss of the arbitrary claim of claim 1 to 6/PBT alloy is characterized in that, comprising:
Step 1, take by weighing each component by the described quality percentage composition of claim 1, and with the PET that takes by weighing and PBT in 110～130 ℃ of temperature following time of drying more than 4 hours, other components are dry more than 2 hours under 60～80 ℃ of temperature;
Step 2, the PET with after the drying treatment, PBT, compatilizer, oxidation inhibitor, nucleation accelerating agent, composite nucleating agent and processing aid are put into high-speed mixer and are mixed, and stir 5～15min at normal temperatures;
Step 3, the mixed material of step 2 is joined in the hopper of twin screw extruder, spun glass is added inlet from the glass in twin screw stage casing add, through melt blending extrude, water-cooled, air-dry, pelletizing;
Wherein, the temperature of twin screw extruder is set to: a district: 200～210 ℃; Two districts: 210～220 ℃; Three districts: 220～230 ℃; Four districts: 230～240 ℃; Five districts: 240～250 ℃; Six districts: 240～250 ℃; Seven districts: 240～250 ℃; Eight districts: 250～260 ℃; Head temperature: 240～250 ℃; Screw speed is controlled at 200～400r/min.
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| CN2010105902210A CN102040808B (en) | 2010-12-15 | 2010-12-15 | Glass fiber enhanced PET/PBT (Polyethylene Terephthalate)/(Polybutylene Terephthalate) alloy with high glossiness and low warping degree and preparation method thereof |
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| CN102942790A (en) * | 2012-03-01 | 2013-02-27 | 上海真晨企业发展有限公司 | High temperature-resistant high-strength polyphenylene sulfide-based reactively reinforced and toughened composite material |
| CN103382297B (en) * | 2013-07-22 | 2015-08-12 | 上海电力学院 | Fine REINFORCED PET/polyester alloy of a kind of low warpage carbon and preparation method thereof |
| CN105273370A (en) * | 2014-07-25 | 2016-01-27 | 深圳市联创科技集团有限公司 | High-density polyester plastic having ceramic gloss, and preparation method thereof |
| CN104527160A (en) * | 2014-12-31 | 2015-04-22 | 宁波龙安包装科技有限公司 | Hot belt forming composite aluminum hard sheet |
| CN104817832A (en) * | 2015-05-21 | 2015-08-05 | 广东威林工程塑料有限公司 | Polybutylene terephthalate composite material |
| CN105295314B (en) * | 2015-10-20 | 2019-02-05 | 上海胜南复合材料有限公司 | A kind of high-performance exempts from primary coat PBT/PET alloy material and preparation method |
| CN105176021A (en) * | 2015-10-22 | 2015-12-23 | 福建师范大学 | Preparation method of high-impact-resistance polyethylene terephthalate particles |
| CN106380800A (en) * | 2016-10-08 | 2017-02-08 | 上海加略实业有限公司 | High heat-resistant spraying-free glass fiber reinforced PBT/PET alloy and preparation method thereof |
| CN108641313B (en) * | 2018-05-18 | 2020-08-07 | 绍兴振荣汽车零部件有限公司 | Valve body for vacuum booster and preparation method thereof |
| CN109294179A (en) * | 2018-09-25 | 2019-02-01 | 深圳市高科塑化有限公司 | A kind of dedicated PET composite material of charging pile plugs and sockets and preparation method thereof |
| TWI705106B (en) * | 2018-12-25 | 2020-09-21 | 南亞塑膠工業股份有限公司 | High heat-resistant and high-gloss PBT composite material for vehicle lamp reflector and preparation method thereof |
| CN110318121B (en) * | 2019-08-02 | 2022-03-29 | 福建经纬新纤科技实业有限公司 | PET/PBT blending modified fiber |
| CN115058102A (en) * | 2022-07-15 | 2022-09-16 | 中钢集团马鞍山矿山研究总院股份有限公司 | Glass fiber reinforced PBT/PET alloy material with smooth surface and preparation method thereof |
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| CN101759983A (en) * | 2008-12-23 | 2010-06-30 | 上海普利特复合材料股份有限公司 | Reinforced polyester alloy composite material and preparation method thereof |
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