CN112759904A - High-yellowing-resistance flame-retardant PBT (polybutylene terephthalate), and preparation method and application thereof - Google Patents
High-yellowing-resistance flame-retardant PBT (polybutylene terephthalate), and preparation method and application thereof Download PDFInfo
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- CN112759904A CN112759904A CN202011588160.4A CN202011588160A CN112759904A CN 112759904 A CN112759904 A CN 112759904A CN 202011588160 A CN202011588160 A CN 202011588160A CN 112759904 A CN112759904 A CN 112759904A
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- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 title claims abstract description 69
- 239000003063 flame retardant Substances 0.000 title claims abstract description 52
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 229920001707 polybutylene terephthalate Polymers 0.000 title description 70
- -1 polybutylene terephthalate Polymers 0.000 title description 3
- 238000004383 yellowing Methods 0.000 claims abstract description 51
- 229910001377 aluminum hypophosphite Inorganic materials 0.000 claims abstract description 24
- 229920005989 resin Polymers 0.000 claims abstract description 19
- 239000011347 resin Substances 0.000 claims abstract description 19
- 239000003365 glass fiber Substances 0.000 claims abstract description 15
- 238000012360 testing method Methods 0.000 claims abstract description 13
- 238000002156 mixing Methods 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 10
- 239000003822 epoxy resin Substances 0.000 claims description 7
- 229920000647 polyepoxide Polymers 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 6
- XOFYZVNMUHMLCC-ZPOLXVRWSA-N prednisone Chemical compound O=C1C=C[C@]2(C)[C@H]3C(=O)C[C@](C)([C@@](CC4)(O)C(=O)CO)[C@@H]4[C@@H]3CCC2=C1 XOFYZVNMUHMLCC-ZPOLXVRWSA-N 0.000 claims description 6
- 239000004793 Polystyrene Substances 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 5
- 229920002223 polystyrene Polymers 0.000 claims description 5
- 238000001125 extrusion Methods 0.000 claims description 4
- 238000002844 melting Methods 0.000 claims description 4
- 230000008018 melting Effects 0.000 claims description 4
- 238000000034 method Methods 0.000 claims description 4
- 239000002994 raw material Substances 0.000 claims description 3
- 239000011342 resin composition Substances 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 20
- 239000002131 composite material Substances 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 230000002195 synergetic effect Effects 0.000 description 3
- ZJKCITHLCNCAHA-UHFFFAOYSA-K aluminum dioxidophosphanium Chemical compound [Al+3].[O-][PH2]=O.[O-][PH2]=O.[O-][PH2]=O ZJKCITHLCNCAHA-UHFFFAOYSA-K 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 239000012760 heat stabilizer Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 239000003017 thermal stabilizer Substances 0.000 description 2
- 239000006057 Non-nutritive feed additive Substances 0.000 description 1
- 125000003636 chemical group Chemical group 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 239000007822 coupling agent Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 229920006351 engineering plastic Polymers 0.000 description 1
- 238000005469 granulation Methods 0.000 description 1
- 230000003179 granulation Effects 0.000 description 1
- LNEPOXFFQSENCJ-UHFFFAOYSA-N haloperidol Chemical class C1CC(O)(C=2C=CC(Cl)=CC=2)CCN1CCCC(=O)C1=CC=C(F)C=C1 LNEPOXFFQSENCJ-UHFFFAOYSA-N 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000002667 nucleating agent Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- ACVYVLVWPXVTIT-UHFFFAOYSA-N phosphinic acid Chemical compound O[PH2]=O ACVYVLVWPXVTIT-UHFFFAOYSA-N 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000012745 toughening agent Substances 0.000 description 1
- DXZMANYCMVCPIM-UHFFFAOYSA-L zinc;diethylphosphinate Chemical compound [Zn+2].CCP([O-])(=O)CC.CCP([O-])(=O)CC DXZMANYCMVCPIM-UHFFFAOYSA-L 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L67/00—Compositions of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Compositions of derivatives of such polymers
- C08L67/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses high-yellowing-resistance flame-retardant PBT, and a preparation method and application thereof. The high yellowing resistance flame retardant PBT comprises the following components in parts by weight: 55-80 parts of PBT resin; 8 to 10 parts of brominated flame retardant; 3-8 parts of aluminum hypophosphite; 20 to 35 parts of alkali-free glass fiber. The high yellowing resistance flame retardant PBT disclosed by the invention is cooperatively matched with aluminum hypophosphite and other components to realize the balance of final yellowing resistance and mechanical properties, so that the flame retardant PBT with low yellowing and good mechanical properties is obtained, the baking color difference value can be reduced to 3.2, the ultraviolet irradiation color difference value can be reduced to 3.5, the flame retardant PBT has excellent yellowing resistance, meanwhile, the flame retardant test of the material can reach V0 level, the flame retardant PBT has excellent mechanical properties, and the flame retardant PBT can be widely applied to the field of electronic and electric appliances.
Description
Technical Field
The invention relates to the technical field of engineering plastics, and particularly relates to high-yellowing-resistance flame-retardant PBT as well as a preparation method and application thereof.
Background
The flame-retardant reinforced PBT material is widely applied to lighting lamps, cooling fans, connectors, coil frameworks, electric appliance shells and other electronic and electrical components, but the PBT material can be yellowed under the conditions of illumination and baking, so that the use appearance and the service life of the material are influenced, and therefore, the development of the PBT material with high yellowing resistance is of great significance.
The prior art CN102070887A discloses a halogen-free flame-retardant reinforced PBT material with high yellowing resistance and high mechanical property and a preparation method thereof, wherein the PBT material comprises the following components in parts by weight: 37.5-49 parts of PBT resin; 8-25 parts of a halogen-free flame retardant compound; 10-50 parts of glass fiber; 1-3 parts of a photo-thermal stabilizer; 2-4 parts of a special nucleating agent; 1-3 parts of a composite coupling agent; 0.5-1 part of processing aid; 0-5 parts of a toughening agent. The PBT material mainly improves the anti-yellowing effect of the product under the photo-thermal effect by adding the photo-thermal stabilizer in a compounding way, aims at a specific halogen-free flame-retardant reinforced PBT material, and does not realize the improvement of the anti-yellowing performance of the flame-retardant PBT material by researching the flame-retardant PBT preparation raw material.
Disclosure of Invention
The invention aims to overcome the defect and defect that yellowing resistance of an anti-yellowing PBT composite material needs to be improved by adding a light-heat stabilizer, and provides the high-yellowing-resistance flame-retardant PBT which does not need to add the light-heat stabilizer, realizes low yellowing of the flame-retardant PBT composite material by cooperatively controlling the compatibility of aluminum hypophosphite and other preparation components, and has good mechanical property.
The invention also aims to provide a preparation method of the high yellowing resistance flame retardant PBT.
The invention further aims to provide application of the high yellowing resistance and flame retardation PBT in the field of electronic and electric appliances.
Still another object of the present invention is to provide an electronic and electric product.
The above purpose of the invention is realized by the following technical scheme:
the high yellowing-resistant flame-retardant PBT comprises the following components in parts by weight:
48-63 parts of PBT resin;
8 to 10 parts of brominated flame retardant;
3-8 parts of aluminum hypophosphite;
20 to 35 parts of alkali-free glass fiber.
The high anti-yellowing flame-retardant PBT comprises PBT resin, a brominated flame retardant, aluminum hypophosphite and alkali-free glass fiber, the flame-retardant PBT is mainly added with the synergistic effect of the brominated flame retardant and the alkali-free glass fiber to improve the flame-retardant effect and the mechanical property, and the aluminum hypophosphite is added to improve the anti-yellowing property.
In addition, the content of each component in the high yellowing resistance flame retardant PBT is also a very important influence factor, for example, if the content of the brominated flame retardant is too high, the overall flow performance is influenced, the later-stage processing forming is not facilitated, the mechanical performance of the material is influenced, the manufacturing cost is also increased, if the content is too low, the flame retardant effect of the flame retardant PBT cannot be well maintained, if the content of the alkali-free glass fiber is too low, the mechanical performance enhancement of the material and the realization of the corresponding V0-grade flame retardant performance are also influenced, and if the content is too high, the solid content is too high, and the subsequent granulation processing forming is influenced.
In the flame-retardant PBT compound, the yellowing of the material is related to the added aluminum hypophosphite, the more the aluminum hypophosphite is, the smaller the yellowing is, but when the content of the aluminum hypophosphite is too high, the yellowing is very small, but the mechanical property is obviously reduced, so that in order to obtain the flame-retardant PBT with low yellowing and good mechanical property, the aluminum hypophosphite and other components need to be matched in a synergistic manner, and the final balance of yellowing resistance and mechanical property is realized.
Preferably, the composition comprises the following components in parts by weight:
48-56 parts of PBT resin;
8 parts of a brominated flame retardant;
4 to 8 parts of aluminum hypophosphite
30 to 35 parts of alkali-free glass fiber.
Further preferably, the composition comprises the following components in parts by weight:
48-55 parts of PBT resin;
8 parts of a brominated flame retardant;
6 to 8 parts of aluminum hypophosphite
30 to 35 parts of alkali-free glass fiber.
More preferably, the composition comprises the following components in parts by weight:
48 parts of a PBT resin;
8 parts of a brominated flame retardant;
8 parts of aluminum hypophosphite
35 parts of alkali-free glass fiber.
Preferably, the PBT resin has a relative density of 1.30 to 1.32g/cm3。
Preferably, the PBT resin has a melting point of 215-230 ℃.
Preferably, the brominated flame retardant is brominated epoxy resin or brominated polystyrene.
In the selection of the flame retardant of the flame-retardant PBT, brominated epoxy resin or brominated polystyrene is preferably selected, and the brominated epoxy resin or the brominated polystyrene has good appearance performance, does not have the conditions of spots, bubbles and the like in the use process, has good surface uniformity and good product appearance performance; on the other hand, brominated epoxy resin or brominated polystyrene does not have the precipitation condition in the use process, and the fluidity is better, which is beneficial to processing and forming, and the comprehensive performance is more excellent.
The invention also provides a preparation method of the high yellowing resistance flame retardant PBT, which comprises the following steps:
s1, drying PBT;
s2, uniformly mixing the dried PBT, the brominated flame retardant and the aluminum hypophosphite in a high-speed mixer, adding the mixture into a double-screw extruder, feeding alkali-free glass fiber from the side of the extruder, plasticizing, mixing, extruding, cooling and granulating to obtain the high-yellowing-resistance flame-retardant PBT.
Preferably, the drying treatment in S1 is carried out at 130-140 ℃ for 3-5 hours.
Preferably, the extrusion temperature of the plasticizing mixing extrusion in S3 is 210-260 ℃.
The application of the high yellowing resistance flame retardant PBT in the field of electronic and electric appliances is also within the protection scope of the invention.
Preferably, the high yellowing-resistant flame-retardant PBT in the application is baked at 180 ℃ for 168 hours, the color difference delta E is 3.2-4.7, and the notch impact strength is 8.4-10.4 kJ/m2The flame retardant test of 1.6mm UL-94 thickness is V0 grade.
The color difference value delta E of the high-yellowing-resistance flame-retardant PBT composite material after being baked for 168 hours at 180 ℃ can be reduced to 3.2, and the PBT composite material is irradiated by ultraviolet light for 72 hours (0.68 w/m)2And the color difference value delta E at 65 ℃ can be reduced to 3.5, the yellowing resistance is excellent, the UL-94 flame retardant test (the thickness is 1.6mm) of the material can reach V0 level, the mechanical property is excellent, and the material can be widely applied to the field of electronic and electric appliances.
The invention also specifically protects an electronic and electric appliance product which is prepared from the raw materials comprising the high yellowing resistance flame retardant PBT.
Compared with the prior art, the invention has the beneficial effects that:
the invention discloses high yellowing resistance flame retardant PBT, wherein the addition of hypophosphorous acid can improve the yellowing resistance of materials, but is also not beneficial to the maintenance of the mechanical properties of the materials, and the final yellowing resistance and the mechanical properties of the PBT are balanced by the synergistic compatibility of the composition of aluminum hypophosphite and other components, so that the flame retardant PBT with low yellowing and good mechanical properties is obtained.
The color difference value delta E of the high-yellowing-resistance flame-retardant PBT composite material after being baked for 168 hours at 180 ℃ can be reduced to 3.2, and the PBT composite material is irradiated by ultraviolet light for 72 hours (0.68 w/m)265 ℃ can be reduced to 3.5, and has excellent yellowing resistanceMeanwhile, the UL-94 flame retardant test (thickness of 1.6mm) of the material can reach V0 level, and the material has excellent mechanical properties and can be widely applied to the field of electronic and electric appliances.
Detailed Description
The present invention will be further described with reference to specific embodiments, but the present invention is not limited to the examples in any way. The starting reagents employed in the examples of the present invention are, unless otherwise specified, those that are conventionally purchased.
The sources of the components of the invention are as follows:
the PBT resin is derived from: the manufacturer: taiwan chemical industry, trade mark: PBT 1200-211M
Brominated epoxy resins are derived from: the manufacturer: israel chemical group, brand: powder-F-2100
The aluminum hypophosphite is derived from: the manufacturer: suzhou union chemical industry, trade mark: aluminum hypophosphite
The alkali-free glass fiber is derived from: the manufacturer: chongqing International composite materials, Inc., under the designation ECS 303W.
In the examples, the properties were tested as follows:
the color difference Δ E (baked at 180 ℃ for 168h) was measured as follows: the color Lab value of the square plate is firstly tested to obtain L, a, b and three values respectively, then the color plate is baked for 168 hours in an oven at 180 ℃, and after baking is finished, the Lab value is tested again to obtain L1, a1 and b 1. The color difference calculation formula is as follows:
wherein, DeltaL is L1-L, Deltaa is a1-a, Deltab is b1-b
Color difference Delta E (ultraviolet irradiation for 72h, 0.68 w/m)265 ℃ C.) the test method is as follows: (test Standard ISO4892-2:2013)
The tensile strength was measured as follows: test standard ISO 527-;
the notched impact strength was tested as follows: test standard ISO 180-;
the flexural strength was tested as follows: test standard ISO 178-;
the UL-94 flame resistance test (thickness 1.6mm) test method is as follows: test standard UL-94-2019 test.
Examples 1 to 7
The high yellowing resistance and flame retardation PBT comprises the components shown in the table 1 in parts by weight.
Wherein the PBT resin has a relative density of 1.30-1.32g/cm3The melting point is 215-230 ℃. The manufacturer: taiwan chemical industry, trade mark: PBT 1200-211M
The brominated flame retardant is brominated epoxy resin.
The preparation method of the high anti-yellowing flame-retardant PBT comprises the following steps:
s1, drying PBT resin at 140 ℃ for 3 hours;
s2, uniformly mixing the dried PBT resin, the brominated flame retardant and the aluminum phosphinate in a high-speed mixer, adding the mixture into a double-screw extruder, feeding alkali-free glass fiber from the side of the extruder, plasticizing, mixing, extruding, cooling and granulating at 230 ℃ to obtain the high-yellowing-resistance flame-retardant PBT.
Table 1, high yellowing resistance flame retardant PBT compositions of examples 1-7
Comparative examples 1 to 7
The high yellowing resistance and flame retardation PBT comprises the components shown in the table 2 in parts by weight.
Wherein the PBT resin has a relative density of 1.30-1.32g/cm3The melting point is 215-230 ℃.
The brominated flame retardant is brominated epoxy resin.
The preparation method of the antimony-white-free high-GWIT brominated flame-retardant PBT comprises the following steps:
s1, drying PBT resin at 140 ℃ for 3 hours;
s2, uniformly mixing the dried PBT resin, the brominated flame retardant and the aluminum phosphinate in a high-speed mixer, adding the mixture into a double-screw extruder, feeding alkali-free glass fiber from the side of the extruder, plasticizing, mixing, extruding, cooling and granulating at 230 ℃ to obtain the high-yellowing-resistance flame-retardant PBT.
Table 2, high yellowing resistance and flame retardation PBT composition for comparative examples 1 to 7
Result detection
The performance tests of the high yellowing resistance and flame retardant PBT of the above examples and comparative examples include yellowing resistance and mechanical properties, and the specific test results are shown in tables 3 and 4 below.
Table 3. high yellowing resistance and flame retardance PBT detection results of examples
Table 4 comparative example PBT (polybutylene terephthalate) detection result with high yellowing resistance and flame retardance
As can be seen from the examples and the comparative examples, when the aluminum hypophosphite with a proper proportion is added, low yellowing can be realized, the mechanical property is good, the yellowing degree of the material is related to the added aluminum hypophosphite, and the more the aluminum hypophosphite is, the less the aluminum hypophosphite is yellowed. However, when the content of aluminum hypophosphite is too high, the mechanical properties are obviously reduced although the yellowing is small.
It should be understood that the above-described embodiments of the present invention are merely examples for clearly illustrating the present invention, and are not intended to limit the embodiments of the present invention. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. Any modification, equivalent replacement, and improvement made within the spirit and principle of the present invention should be included in the protection scope of the claims of the present invention.
Claims (10)
1. The high yellowing-resistant flame-retardant PBT is characterized by comprising the following components in parts by weight:
48-63 parts of PBT resin;
8 to 10 parts of brominated flame retardant;
3 to 8 parts of aluminum hypophosphite
20 to 35 parts of alkali-free glass fiber.
2. The PBT with high yellowing resistance and flame retardance according to claim 1, wherein the PBT resin has a relative density of 1.30-1.32g/cm3。
3. The PBT resin composition according to claim 2, wherein the PBT resin has a melting point of 215 to 230 ℃.
4. The PBT of claim 1, wherein the brominated flame retardant is a brominated epoxy resin or a brominated polystyrene.
5. The preparation method of the high yellowing resistance and flame retardance PBT of any one of claims 1-4, characterized by comprising the following steps:
s1, drying PBT;
s2, uniformly mixing the dried PBT, the brominated flame retardant and the aluminum hypophosphite in a high-speed mixer, adding the mixture into a double-screw extruder, feeding alkali-free glass fiber from the side of the extruder, plasticizing, mixing, extruding, cooling and granulating to obtain the high-yellowing-resistance flame-retardant PBT.
6. The method according to claim 5, wherein the drying in S1 is performed at a temperature of 130 ℃ to 140 ℃ for 3 to 5 hours.
7. The method of claim 5, wherein the extrusion temperature for the plasticization-mixing extrusion in S2 is 210 ℃ to 260 ℃.
8. The application of the high yellowing resistance and flame retardation PBT of any one of claims 1-4 in the field of electronic and electric appliances.
9. The application of claim 8, wherein the high yellowing resistance and flame retardation PBT is baked at 180 ℃ for 168 hours, the color difference delta E is 3.2-4.7, and the notch impact strength is 8.4-10.4 kJ/m2The flame retardant test of 1.6mm UL-94 thickness is V0 grade.
10. An electronic and electric product, which is characterized in that the electronic and electric product is prepared from the raw material comprising the high yellowing resistance and flame retardation PBT of any one of claims 1 to 3.
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Cited By (1)
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CN114773798A (en) * | 2022-03-09 | 2022-07-22 | 上海金发科技发展有限公司 | High-impact long-acting yellowing-resistant PBT (polybutylene terephthalate) -reinforced flame-retardant composite material as well as preparation method and application thereof |
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WO2018073819A1 (en) * | 2016-10-18 | 2018-04-26 | Bromine Compounds Ltd. | Flame-retarded polyester formulations |
CN109749375A (en) * | 2019-01-22 | 2019-05-14 | 广东顺德同程新材料科技有限公司 | A kind of fire retardant polybutylene terephthalate material and preparation method thereof |
CN110121525A (en) * | 2016-10-18 | 2019-08-13 | 溴化合物有限公司 | Flame retardant polyester composition |
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Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
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WO2018073819A1 (en) * | 2016-10-18 | 2018-04-26 | Bromine Compounds Ltd. | Flame-retarded polyester formulations |
CN110121525A (en) * | 2016-10-18 | 2019-08-13 | 溴化合物有限公司 | Flame retardant polyester composition |
CN109749375A (en) * | 2019-01-22 | 2019-05-14 | 广东顺德同程新材料科技有限公司 | A kind of fire retardant polybutylene terephthalate material and preparation method thereof |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN114773798A (en) * | 2022-03-09 | 2022-07-22 | 上海金发科技发展有限公司 | High-impact long-acting yellowing-resistant PBT (polybutylene terephthalate) -reinforced flame-retardant composite material as well as preparation method and application thereof |
CN114773798B (en) * | 2022-03-09 | 2024-03-15 | 上海金发科技发展有限公司 | High-impact long-acting yellowing-resistant PBT reinforced flame-retardant composite material and preparation method and application thereof |
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