CN102702699B - Glass-fiber-reinforced hydrolysis-resistant polyester material and preparation method thereof - Google Patents
Glass-fiber-reinforced hydrolysis-resistant polyester material and preparation method thereof Download PDFInfo
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- CN102702699B CN102702699B CN201210233325.5A CN201210233325A CN102702699B CN 102702699 B CN102702699 B CN 102702699B CN 201210233325 A CN201210233325 A CN 201210233325A CN 102702699 B CN102702699 B CN 102702699B
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Abstract
The invention provides a glass-fiber-reinforced hydrolysis-resistant polyester material which is prepared from the following raw materials in percentage by weight: 30-80% of polyester, 5-40% of glass fiber, 3-10% of compatilizer, 0.3-20% of hydrolytic reagent, 0.1-0.5% of antioxidant and 0.1-0.5% of lubricant. The invention also provides a preparation method of the glass-fiber-reinforced hydrolysis-resistant polyester material, which comprises the following steps: mixing the raw materials according to the percentage by weight, putting in a screw rod machine, extruding, and cooling with water to granulate, wherein the rotation speed of the screw rod machine is 180-600 rpm, and the temperature is 235-255 DEG C. The material provided by the invention has the advantages of better mechanical properties, high hydrolysis resistance, high mechanical property retentivity, favorable flowability, fewer surface floating fibers, excellent processability and low cost, and has very wide application prospects in the fields of electronics, electricity, automobiles, home appliances and the like.
Description
Technical field
The present invention relates to modification polyester materials and preparation method thereof, specifically, is a kind of Glass-fiber-reinforchydrolysis-resistantpolyester hydrolysis-resistantpolyester polyester material and preparation method thereof.
Background technology
Polyester material has the advantages such as very outstanding chemical reagent resistance, thermotolerance and excellent physical strength, electrical insulation characteristics and thermostability, but there is the shortcoming of notch shock sensitivity, the polyester material of glass fiber reinforcement then compensate for this defect of polyester material, makes it be widely used in electric, the field such as automobile, household electrical appliances.Because the water-intake rate of polyester material is lower, make it still can the work of normal table under comparatively wet environment, but because polyester contains ester bond, so polyester material will be degraded under the Working environment comparatively large in some relative humidity, temperature is higher, the acid produced in degradation process also can the degraded of catalyst, polyester material and corrosion further, polyester material performance is sharply reduced, affects it and normally use, seriously limit applying of polyester material.Therefore, a kind of Glass-fiber-reinforchydrolysis-resistantpolyester hydrolysis-resistantpolyester polyester material is researched and developed particularly important.
Chinese patent literature CN 200710125558.2, publication date on July 16th, 2008, disclose a kind of environment-protection flame-proof fiberglass reinforcing polyester alloy material and preparation method thereof, this polyester alloy material is made up of the raw material of following weight proportion: polycarbonate 50-70%, polyester 10-40%, compatilizer 3-5%, fire retardant 3-6%, oxidation inhibitor 0.1-1%, lubricant 0.3-1%, glass fibre 3.5-10%; Its preparation method is for matrix resin with polycarbonate, linear saturated polyester, add compatilizer, fire retardant, oxidation inhibitor, lubricant, glass fibre, form through twin screw extruder granulation, this Polycarbonate alloy material surface brightness is high, but can not learn its anti-hydrolytic performance; Chinese patent literature CN 2011102636.7.5, September 7 2011 applying date, disclose a kind of flame-proof glass fibre REINFORCED PET/PTT/PBT alloy material and preparation method thereof, the raw material adopted and weight part thereof are: PET 10-30 part, PTT 10-30 part, PBT 20-40 part, compatilizer 3-10 part, composite flame-retardant agent 5-20 part, oxidation inhibitor 0.1-0.5 part, lubricant 0.1-0.5 part, glass fibre 10-30 part, this alloy material excellent fireproof performance, shrinking percentage is dripped, dimensional stabilizing, surface gloss is high, but anti-hydrolytic performance method has no improvement.Glass-fiber-reinforced polyester material at present about excellent hydrolysis resistance have not been reported.
Summary of the invention
The object of the invention is, for deficiency of the prior art, to provide a kind of Glass-fiber-reinforchydrolysis-resistantpolyester hydrolysis-resistantpolyester polyester material.
Of the present invention again one object be that a kind of preparation method of Glass-fiber-reinforchydrolysis-resistantpolyester hydrolysis-resistantpolyester polyester material is provided.
For achieving the above object, the technical scheme that the present invention takes is:
A kind of Glass-fiber-reinforchydrolysis-resistantpolyester hydrolysis-resistantpolyester polyester material, described Glass-fiber-reinforchydrolysis-resistantpolyester hydrolysis-resistantpolyester polyester material is made up of the raw material of following weight percent:
Polyester 30-80%,
Glass fibre 5-40%,
Compatilizer 3-10%,
Hydrolysis agent 0.3-20%,
Oxidation inhibitor 0.1-0.5%,
Lubricant 0.1-0.5%.
Preferably, described Glass-fiber-reinforchydrolysis-resistantpolyester hydrolysis-resistantpolyester polyester material is made up of the raw material of following weight percent:
Polyester 60%,
Glass fibre 30%,
Compatilizer 3.8%,
Hydrolysis agent 5.5%,
Oxidation inhibitor 0.4%,
Lubricant 0.3%.
Described polyester is polyethylene terephthalate and/or polybutylene terephthalate.
Described glass fibre is E-CS glass fibre;
Described compatilizer is ethylene-methyl acrylate-glyceryl methacrylate terpolymer and/or Ethylene-butyl Acrylate-methacrylic Acid Glycerin Ester Copolymer;
Described hydrolysis agent is one or more in carbodiimide, cyclic anhydride, band epoxide group molecule, oxazole derivatives, isocyanic ester;
Described oxidation inhibitor is the compound system of Hinered phenols antioxidant and phosphite ester kind antioxidant;
Described oxidation inhibitor is the compound system of oxidation inhibitor 1098 and irgasfos 168;
Described lubricant is silicone powder MB-4 and/or TAF.
For realizing above-mentioned second object, the technical scheme that the present invention takes is:
As above the preparation method of arbitrary described Glass-fiber-reinforchydrolysis-resistantpolyester hydrolysis-resistantpolyester polyester material, described preparation method comprises the following steps:
(1) weight percent as described above weighs raw material;
(2) polyester raw material step 1) weighed dries 7-9 hour at 110 DEG C;
(3) all raw materials are put into high efficient mixer mixing discharging after 5-10 minute;
(4) mixed for step 3) raw material is put into screw machine to extrude and water-cooled granulation, the rotating speed of screw machine is 180-600 rev/min, and temperature is 235-255 DEG C.
The invention has the advantages that:
1, polyester material mechanical property of the present invention is better;
2, polyester material of the present invention is under long-term humidity or high-temperature work environment, and the mechanical property conservation rate of material is high, and anti-hydrolytic performance is good;
3, polyester material good fluidity of the present invention, surface floating fiber is few, and processing characteristics is excellent;
4, polyester material cost of the present invention is low;
Comprehensive above every advantage is known, and polyester material of the present invention has very wide application prospect in the field such as electric, automobile, household electrical appliances.
Embodiment
Below embodiment provided by the invention is elaborated.
Polyethylene terephthalate English name described is herein polyethylene terephthalate, be called for short PET, exchanged by dimethyl terephthalate (DMT) and glycol ester or first synthesize bishydroxyethyl terephthalate with terephthalic acid and ethylene glycol esterification, and then it is obtained to carry out polycondensation, belong to crystal type saturated polyester, molecular-weight average (2-3) × 10
4, weight average is 1.5-1.8 with the ratio of number-average molecular weight, preferred engineering plastics level; Described polybutylene terephthalate English name is polybutylene terephthalate, is called for short PBT, for oyster white is translucent to opaque, crystalline thermoplastic polyester, has high heat resistance, toughness, resistance to fatigue, self-lubricating, low-friction coefficient; Described glass fibre ECS is a kind of alkali free glass fibre chopped strand, specifically uses glass fibre megalith group chopped glass fiber ECS 13-4.5-534A, but is not limited only to this, and the present invention can also use other model alkali free glass fibre chopped strands; Described ethylene-methyl acrylate-glyceryl methacrylate terpolymer is the AX8900 of French Arkema; Described Ethylene-butyl Acrylate-methacrylic Acid Glycerin Ester Copolymer is that the PTW of E.I.Du Pont Company can be used for PET/PBT toughening modifying; Described cyclic anhydride specifically uses 1,1-cyclohexanediacetic acid acid anhydride; Described band epoxide group molecule comprises epoxy resin etc.; Described epoxy resin is the organic high molecular compound containing two or more epoxide groups in molecule, specifically uses the bright Chemical Co., Ltd. E-20(601 in Wuxi); Described oxazole derivatives specifically uses 2-oxazolidone; Described oxidation inhibitor 1098 English name Antioxidant 1098, Chinese another name N, N'-pair-(3-(3,5-di-tert-butyl-hydroxy phenyl) propionyl) hexanediamine, molecular formula: C
40h
64n
2o
4, be mainly used in synthesis and the processing of the polymkeric substance such as polymeric amide, polyolefine, polystyrene, ABS resin, acetal-based resin, urethane and rubber; Described irgasfos 168 English name Tns-(2.4-di-tert-butyl)-phosphite, Chinese: three [2.4-di-tert-butyl-phenyl] phosphorous acid ester, molecular formula: C
42h
63o
3p is the agent of a kind of low volatility organic synthesis resistance to the oxygen inhibiting polymerization, is widely used in polypropylene, polyethylene, ABS, the synthesis gathering all types of plastic such as carbonic acid fiber and vibrin and processing; Described silicone powder is Tongcheng City Xin get Chemical Co., Ltd. MB-4; Described TAF Chinese is the two ethylene hard fatty acids acid amides of N, N-, has good temperature tolerance, be mainly used in processing temperature require that high engineering plastic modification and PC, PPS strengthen, flame-retardant modified; Lubricant of the present invention is not limited to silicone powder MB-4 and/or TAF, also can be stearic amide, siloxanes etc.
embodiment 1 polyester material preparation () of the present invention
(1) following raw material is weighed by weight percentage: PBT 60%, glass fibre ECS13-4.5-534A 30%, compatilizer AX8900 3.8%, carbodiimide 0.5%, epoxy resin 5%, oxidation inhibitor 1,098 0.2%, irgasfos 168 0.2%, lubricant MB-4 0.3%;
(2) PBT step 1) weighed dries 8 hours at 110 DEG C;
(3) all raw materials are put into high efficient mixer mixing discharging after 8 minutes;
(4) mixed for step 3) raw material is put into twin screw extruder melting, mixing, to extrude and water-cooled, then pelletizing after drying, packaging, the rotating speed of screw machine is 260 revs/min, and each zone temperature of double-screw extruding machine barrel used is at 235-255 DEG C.
embodiment 2 polyester material preparation (two) of the present invention
(1) following raw material is weighed by weight percentage: PBT 40%, PET 20%, glass fibre ECS13-4.5-534A 30%, compatilizer AX8900 3.8%, carbodiimide 0.5%, isocyanic ester 5%, oxidation inhibitor 1,098 0.2%, irgasfos 168 0.2%, lubricant TAF 0.3%;
(2) PBT, PET of step 1) being weighed dry 8 hours at 110 DEG C;
(3) all raw materials are put into high efficient mixer mixing discharging after 5 minutes;
(4) mixed for step 3) raw material is put into twin screw extruder melting, mixing, to extrude and water-cooled, then pelletizing after drying, packaging, the rotating speed of screw machine is 500 revs/min, and each zone temperature of double-screw extruding machine barrel used is at 235-255 DEG C.
embodiment 3 polyester material preparation (three) of the present invention
(1) following raw material is weighed by weight percentage: PET 70%, glass fibre ECS13-4.5-534A 15%, compatilizer PTW 10%, cyclic anhydride 2%, oxazole derivatives 2.5%, oxidation inhibitor 1,098 0.1%, irgasfos 168 0.1%, lubricant TAF 0.2%, lubricant MB-4 0.1%;
(2) PET step 1) weighed dries 7.5 hours at 110 DEG C;
(3) all raw materials are put into high efficient mixer mixing discharging after 10 minutes;
(4) mixed for step 3) raw material is put into twin screw extruder melting, mixing, to extrude and water-cooled, then pelletizing after drying, packaging, the rotating speed of screw machine is 180 revs/min, and each zone temperature of double-screw extruding machine barrel used is at 235-255 DEG C.
embodiment 4 polyester material preparation (four) of the present invention
(1) following raw material is weighed by weight percentage: PBT 64%, glass fibre ECS13-4.5-534A 5%, compatilizer AX8900 5%, compatilizer PTW 5%, carbodiimide 20%, oxidation inhibitor 1,098 0.2%, irgasfos 168 0.3%, lubricant MB-4 0.5%;
(2) PBT step 1) weighed dries 9 hours at 110 DEG C;
(3) all raw materials are put into high efficient mixer mixing discharging after 10 minutes;
(4) mixed for step 3) raw material is put into twin screw extruder melting, mixing, to extrude and water-cooled, then pelletizing after drying, packaging, the rotating speed of screw machine is 200 revs/min, and each zone temperature of double-screw extruding machine barrel used is at 235-255 DEG C.
embodiment 5 polyester material preparation (five) of the present invention
(1) following raw material is weighed by weight percentage: PBT 35%, glass fibre ECS13-4.5-534A 40%, compatilizer AX8900 10%, epoxy resin 5%, isocyanic ester 4%, cyclic anhydride 5%, oxidation inhibitor 1,098 0.3%, irgasfos 168 0.2%, lubricant TAF 0.5%;
(2) PBT step 1) weighed dries 8 hours at 110 DEG C;
(3) all raw materials are put into high efficient mixer mixing discharging after 7 minutes;
(4) mixed for step 3) raw material is put into twin screw extruder melting, mixing, to extrude and water-cooled, then pelletizing after drying, packaging, the rotating speed of screw machine is 500 revs/min, and each zone temperature of double-screw extruding machine barrel used is at 235-255 DEG C.
embodiment 6 polyester material preparation (six) of the present invention
(1) following raw material is weighed by weight percentage: PBT 30%, PET 31.8%, glass fibre ECS13-4.5-534A 25%, compatilizer PTW 3%, carbodiimide 10%, oxidation inhibitor 1,098 0.05%, irgasfos 168 0.05%, lubricant MB-4 0.1%;
(2) PBT step 1) weighed dries 8 hours at 110 DEG C;
(3) all raw materials are put into high efficient mixer mixing discharging after 8 minutes;
(4) mixed for step 3) raw material is put into twin screw extruder melting, mixing, to extrude and water-cooled, then pelletizing after drying, packaging, the rotating speed of screw machine is 450 revs/min, and each zone temperature of double-screw extruding machine barrel used is at 235-255 DEG C.
embodiment 7 polyester material preparation (seven) of the present invention
(1) following raw material is weighed by weight percentage: PBT 19.3%, PET 40%, glass fibre ECS13-4.5-534A 10%, compatilizer PTW 10%, isocyanic ester 20%, oxidation inhibitor 1,098 0.1%, irgasfos 168 0.1%, lubricant TAF 0.5%;
(2) PBT, PET of step 1) being weighed dry 9 hours at 110 DEG C;
(3) all raw materials are put into high efficient mixer mixing discharging after 8 minutes;
(4) mixed for step 3) raw material is put into twin screw extruder melting, mixing, to extrude and water-cooled, then pelletizing after drying, packaging, the rotating speed of screw machine is 300 revs/min, and each zone temperature of double-screw extruding machine barrel used is at 235-255 DEG C.
embodiment 8 polyester material preparation (eight) of the present invention
(1) following raw material is weighed by weight percentage: PET 75%, glass fibre ECS13-4.5-534A 5%, compatilizer AX8900 10%, carbodiimide 9.5%, oxidation inhibitor 1,098 0.2%, irgasfos 168 0.2%, lubricant MB-4 0.1%;
(2) PET step 1) weighed dries 7 hours at 110 DEG C;
(3) all raw materials are put into high efficient mixer mixing discharging after 8 minutes;
(4) mixed for step 3) raw material is put into twin screw extruder melting, mixing, to extrude and water-cooled, then pelletizing after drying, packaging, the rotating speed of screw machine is 300 revs/min, and each zone temperature of double-screw extruding machine barrel used is at 235-255 DEG C.
comparative example 1
(1) following raw material is weighed by weight percentage: PBT 40%, glass fibre ECS13-4.5-534A 30%, compatilizer AX8900 3.8%, carbodiimide 0.5%, epoxy resin 25%, oxidation inhibitor 1,098 0.2%, irgasfos 168 0.2%, lubricant MB-4 0.3%;
(2) PBT step 1) weighed dries 8 hours at 110 DEG C;
(3) all raw materials are put into high efficient mixer mixing discharging after 8 minutes;
(4) mixed for step 3) raw material is put into twin screw extruder melting, mixing, to extrude and water-cooled, then pelletizing after drying, packaging, the rotating speed of screw machine is 260 revs/min, and each zone temperature of double-screw extruding machine barrel used is at 235-255 DEG C.
comparative example 2
(1) following raw material is weighed by weight percentage: PBT 40%, PET 25.2%, glass fibre ECS13-4.5-534A 30%, compatilizer AX8900 3.8%, carbodiimide 0.3%, oxidation inhibitor 1,098 0.2%, irgasfos 168 0.2%, lubricant TAF 0.3%;
(2) PBT, PET of step 1) being weighed dry 8 hours at 110 DEG C;
(3) all raw materials are put into high efficient mixer mixing discharging after 5 minutes;
(4) mixed for step 3) raw material is put into twin screw extruder melting, mixing, to extrude and water-cooled, then pelletizing after drying, packaging, the rotating speed of screw machine is 500 revs/min, and each zone temperature of double-screw extruding machine barrel used is at 235-255 DEG C.
comparative example 3
(1) following raw material is weighed by weight percentage: PBT 40%, PET 25.6%, glass fibre ECS13-4.5-534A 30%, compatilizer AX8900 3.8%, carbodiimide 0.3%, lubricant TAF 0.3%;
(2) PBT, PET of step 1) being weighed dry 8 hours at 110 DEG C;
(3) all raw materials are put into high efficient mixer mixing discharging after 5 minutes;
(4) mixed for step 3) raw material is put into twin screw extruder melting, mixing, to extrude and water-cooled, then pelletizing after drying, packaging, the rotating speed of screw machine is 500 revs/min, and each zone temperature of double-screw extruding machine barrel used is at 235-255 DEG C.
embodiment 9 performance test
Material polyester composite prepared by embodiment 1-2 and comparative example 1-3 prepared all is injection molded into standard examination bar by standard size, and performance is tested by international standard respectively.Anti-hydrolytic performance testing method is: standard is tried bar and be positioned in climatic test cabinet, 85 DEG C, and under the relative humidities of 95%, forced ventilation 1500 hours, every 500 hours sampling and testings.The performance test results is as shown in table 1.
Table 1 polyester property test result of the present invention
As shown in Table 1, polyester material of the present invention is compared with comparative example, under long humidity and hot conditions, can keep good mechanical property all the time, excellent hydrolysis resistance.In addition, the good fluidity of this material, surface floating fiber is few, and processing characteristics is excellent.
The above is only the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, under the prerequisite not departing from the inventive method; can also make some improvement and supplement, these improve and supplement and also should be considered as protection scope of the present invention.
Claims (3)
1. a Glass-fiber-reinforchydrolysis-resistantpolyester hydrolysis-resistantpolyester polyester material, it is characterized in that, described Glass-fiber-reinforchydrolysis-resistantpolyester hydrolysis-resistantpolyester polyester material is made up of the raw material of following weight percent: PBT 60%, glass fibre ECS13-4.5-534A 30%, compatilizer AX8900 3.8%, carbodiimide 0.5%, epoxy resin 5%, oxidation inhibitor 1,098 0.2%, irgasfos 168 0.2%, lubricant MB-4 0.3%.
2. a Glass-fiber-reinforchydrolysis-resistantpolyester hydrolysis-resistantpolyester polyester material, it is characterized in that, described Glass-fiber-reinforchydrolysis-resistantpolyester hydrolysis-resistantpolyester polyester material is made up of the raw material of following weight percent: PBT 40%, PET 20%, glass fibre ECS13-4.5-534A 30%, compatilizer AX8900 3.8%, carbodiimide 0.5%, isocyanic ester 5%, oxidation inhibitor 1,098 0.2%, irgasfos 168 0.2%, lubricant TAF 0.3%.
3. the preparation method of Glass-fiber-reinforchydrolysis-resistantpolyester hydrolysis-resistantpolyester polyester material as claimed in claim 1 or 2, it is characterized in that, described preparation method comprises the following steps:
(1) raw material is weighed by the weight percent described in claim 1 or 2;
(2) polyester raw material step 1) weighed dries 7-9 hour at 110 DEG C;
(3) all raw materials are put into high efficient mixer mixing discharging after 5-10 minute;
(4) mixed for step 3) raw material is put into screw machine to extrude and water-cooled granulation, the rotating speed of described screw machine is 180-600 rev/min, and temperature is 235-255 DEG C.
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| CN104120504B (en) * | 2013-04-24 | 2017-09-26 | 东丽纤维研究所（中国）有限公司 | A kind of hydrolysis-resistant polyester fiber and preparation method thereof |
| CN103554914B (en) * | 2013-10-31 | 2016-04-06 | 广东顺德鸿塑高分子材料有限公司 | Polyphenylene sulfide composite modification material of a kind of hydrolysis and preparation method thereof |
| CN104610711B (en) * | 2015-01-30 | 2016-06-15 | 上海日之升科技有限公司 | A kind of PBT material with good epoxy bond and preparation method thereof |
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| CN106519594B (en) * | 2016-09-23 | 2018-10-12 | 广东银禧科技股份有限公司 | A kind of PBT engineering plastic compositions of oil rub resistance hydrolysis and preparation method thereof for nanometer injection molding |
| CN107177173A (en) * | 2017-06-09 | 2017-09-19 | 东莞市联洲知识产权运营管理有限公司 | A kind of hydrolysis resistant PET composite material |
| CN109867919A (en) * | 2017-12-04 | 2019-06-11 | 广州汽车集团股份有限公司 | Polyethylene terephthalate composite material, product and preparation method |
| CN108059705B (en) * | 2017-12-14 | 2020-08-28 | 上海华峰新材料研发科技有限公司 | Aqueous polyurethane resin hydrolysis-resistant agent and preparation method and application thereof |
| CN109777051A (en) * | 2018-12-28 | 2019-05-21 | 江苏博云塑业股份有限公司 | A kind of polyester composite of hydrolysis and preparation method thereof |
| CN110499007B (en) * | 2019-09-17 | 2021-10-15 | 东莞市东翔塑胶有限公司 | High-temperature and high-humidity resistant halogen-free flame-retardant polyester composite material and preparation method thereof |
| CN112759900A (en) * | 2020-12-28 | 2021-05-07 | 苏州旭光聚合物有限公司 | Glass fiber reinforced polybutylene terephthalate composite material and preparation method thereof |
| CN114395223A (en) * | 2021-12-28 | 2022-04-26 | 上海普利特复合材料股份有限公司 | Hydrolysis-resistant, high-weather-resistance and high-strength glass fiber reinforced PP/PET material for photovoltaic back plate and preparation method thereof |
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