CN111286163A - Reinforced flame-retardant low-warpage PBT (polybutylene terephthalate) alloy material and preparation method thereof - Google Patents
Reinforced flame-retardant low-warpage PBT (polybutylene terephthalate) alloy material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a reinforced flame-retardant low-warpage PBT alloy material and a preparation method thereof. The alloy material comprises the following components in parts by weight: 35-50 parts of polybutylene terephthalate; 5-15 parts of polycarbonate; 15-30 parts of glass fiber; 5-15 parts of inorganic filler; 5-20 parts of a compound flame retardant; 5-10 parts of a toughening agent; 0.2-0.4 part of compound antioxidant; 0.1-0.3 part of lubricant; 0.1-0.3 part of ester exchange inhibitor; 0.1-0.3 part of anti-dripping agent. The preparation method comprises the steps of uniformly mixing the materials except the glass fibers at a high speed, respectively feeding the mixed materials and the glass fibers into a main feeding port and a side feeding port of a double-screw extruder, and finally forming. According to the invention, the amorphous polymer PC is introduced into the raw material, so that the crystallinity of the system is reduced, the warping property of the PBT material is improved, and the toughened PBT can be reinforced; and a compound flame retardant is introduced, so that the product has the flame retardant characteristic. Finally, the PBT/PC alloy material has good mechanical property, flame retardant property and anti-warping property, thereby expanding the application range of the PBT/PC alloy material in the fields of high-grade electrical components, large electrical housings and the like.
Description
Technical Field
The invention relates to the technical field of high polymer materials, in particular to a reinforced flame-retardant low-warpage PBT alloy material and a preparation method thereof.
Background
Polybutylene terephthalate (PBT) has excellent heat resistance, good moldability, electrical insulation properties, and the like, and thus is widely used in the industries of electronics, electricity, automobile switches, and the like. However, injection molded articles tend to shrink and warp due to crystallization of the PBT, making it generally difficult to use the crystalline polymer PBT in a variety of precision and large-scale products; and the product does not have flame retardant property, and still has a worry in safety. Therefore, the development of PBT materials having both warp resistance and flame retardancy is urgent.
Disclosure of Invention
The invention aims to provide a reinforced flame-retardant low-warpage PBT alloy material and a preparation method thereof, and realizes an alloy material with flame-retardant and low-warpage characteristics so as to meet application requirements of related products.
In order to achieve the above purpose, the solution of the invention is:
the reinforced flame-retardant low-warpage PBT alloy material comprises the following raw materials in parts by weight: 35-50 parts of polybutylene terephthalate; 5-15 parts of polycarbonate; 15-30 parts of glass fiber; 5-15 parts of inorganic filler; 5-20 parts of a compound flame retardant; 5-10 parts of a toughening agent; 0.2-0.4 part of compound antioxidant; 0.1-0.3 part of lubricant; 0.1-0.3 part of ester exchange inhibitor; 0.1-0.3 part of anti-dripping agent.
The polybutylene terephthalate has an intrinsic viscosity of 0.8-1.0 dL/g.
The polycarbonate has a melt index of 20g/10min at 300 ℃ under 1.2 kg.
The glass fiber comprises at least one of common alkali-free glass fiber and flat glass fiber.
The inorganic filler comprises at least one of calcium carbonate, kaolin and glass beads.
The compound flame retardant is prepared by mixing a brominated flame retardant and an antimony synergistic flame retardant; wherein, the bromine flame retardant comprises at least one of decabromodiphenylethane, brominated epoxy and brominated styrene, and the antimony synergistic flame retardant comprises at least one of antimony trioxide and antimony trioxide master batch.
The toughening agent comprises at least one of ethylene-vinyl acetate copolymer, ethylene-methyl acrylate copolymer and ethylene-butyl acrylate-glycidyl methacrylate copolymer.
The compound antioxidant is prepared by mixing hindered phenol antioxidant and phosphite ester antioxidant; wherein the hindered phenol antioxidant comprises at least one of hindered phenol antioxidant 1010 and hindered phenol antioxidant 1076, and the phosphite antioxidant comprises at least one of phosphite antioxidant 626 and phosphite antioxidant 168.
The lubricant comprises at least one of silicone master batch, ethylene bisstearamide and pentaerythritol stearate.
The ester exchange inhibitor comprises at least one of triphenyl phosphite, disodium dihydrogen pyrophosphate and sodium dihydrogen phosphate.
The anti-dripping agent is polytetrafluoroethylene.
A preparation method of a reinforced flame-retardant low-warpage PBT alloy material comprises the following steps:
uniformly mixing polybutylene terephthalate, polycarbonate, inorganic filler, a compound flame retardant, a toughening agent, a compound antioxidant, a lubricant, an ester exchange inhibitor and an anti-dripping agent at high speed by a high-speed mixer to obtain a mixed material;
and step two, adding the mixed material into a main feeding port of a double-screw extruder, adding the glass fiber into a side feeding port of the double-screw extruder, and melting, extruding, cooling, drying and granulating the mixture into granules.
The temperature of each zone of the screw barrel of the double-screw extruder is set to be 210 ℃ and 250 ℃, and the rotating speed of the screw is 350 rpm.
After the technical scheme is adopted, the amorphous polymer PC is introduced into the raw materials, so that the crystallinity of the system is reduced, the warping property of the PBT material is improved, and the toughened PBT can be enhanced; and a compound flame retardant is introduced, so that the product has the flame retardant characteristic. Finally, the PBT/PC alloy material has good mechanical property, flame retardant property and anti-warping property, thereby expanding the application range of the PBT/PC alloy material in the fields of high-grade electrical components, large electrical housings and the like.
In addition, when the cross section of the glass fiber is flat, the strength of the formed product is greatly improved and the warping is greatly reduced; when the inorganic filler comprises kaolin, the orientation of glass fibers can be further improved, and the crystallization of PBT can be partially inhibited, so that the warping resistance of a filled product is improved, and the production cost can also be reduced.
Detailed Description
In order to further explain the technical solution of the present invention, the present invention is explained in detail by the following specific examples.
The invention relates to a reinforced flame-retardant low-warpage PBT alloy material which comprises the following raw materials in parts by weight: 35-50 parts of polybutylene terephthalate (PBT); 5-15 parts of Polycarbonate (PC); 15-30 parts of glass fiber; 5-15 parts of inorganic filler; 5-20 parts of a compound flame retardant; 5-10 parts of a toughening agent; 0.2-0.4 part of compound antioxidant; 0.1-0.3 part of lubricant; 0.1-0.3 part of ester exchange inhibitor; 0.1-0.3 part of anti-dripping agent.
The polybutylene terephthalate has an intrinsic viscosity of 0.8 to 1.0 dL/g.
The polycarbonate had a melt index of 20g/10min at 300 ℃ under 1.2 kg.
The glass fiber comprises at least one of common alkali-free glass fiber and flat glass fiber. The glass fiber with the flattened cross section can be dispersed isotropically in the injection molding process, and is beneficial to preventing the PBT material part from warping after being demoulded.
The inorganic filler comprises at least one of calcium carbonate, kaolin and glass beads. Wherein, the kaolin can partially inhibit the crystallization of the PBT material so as to improve the warping property, and is also a cost-reducing material.
The compound flame retardant is prepared by mixing a brominated flame retardant and an antimony synergistic flame retardant; wherein, the bromine flame retardant comprises at least one of decabromodiphenylethane, brominated epoxy and brominated styrene, and the antimony synergistic flame retardant comprises at least one of antimony trioxide and antimony trioxide master batch.
The toughening agent comprises at least one of ethylene-vinyl acetate copolymer, ethylene-methyl acrylate copolymer and ethylene-butyl acrylate-glycidyl methacrylate copolymer.
The compound antioxidant is prepared by mixing hindered phenol antioxidant and phosphite ester antioxidant; wherein the hindered phenol antioxidant comprises at least one of hindered phenol antioxidant 1010 and hindered phenol antioxidant 1076, and the phosphite antioxidant comprises at least one of phosphite antioxidant 626 and phosphite antioxidant 168.
The lubricant comprises at least one of silicone master batch, ethylene bisstearamide and pentaerythritol stearate.
The ester exchange inhibitor comprises at least one of triphenyl phosphite, disodium dihydrogen pyrophosphate and sodium dihydrogen phosphate.
The anti-dripping agent is polytetrafluoroethylene.
The invention also discloses a preparation method of the reinforced flame-retardant low-warpage PBT alloy material, which comprises the following steps:
uniformly mixing polybutylene terephthalate, polycarbonate, inorganic filler, a compound flame retardant, a toughening agent, a compound antioxidant, a lubricant, an ester exchange inhibitor and an anti-dripping agent at high speed by a high-speed mixer to obtain a mixed material;
and step two, adding the mixed material into a main feeding port of a double-screw extruder, adding the glass fiber into a side feeding port of the double-screw extruder, and melting, extruding, cooling, drying and granulating the mixture into granules.
The temperature of each zone of the screw barrel of the double-screw extruder is set to be 210 ℃ and 250 ℃, and the rotating speed of the screw is 350 rpm.
The technical effects of the present invention are illustrated below by specific examples and comparative examples.
Example 1
(1) Weighing the following components in parts by weight: PBT: 44 parts, PC: 7 parts of common alkali-free glass fiber: 22 parts, calcium carbonate: 10 parts of brominated epoxy: 8.5 parts, antimony trioxide: 2 parts of ethylene-methyl acrylate copolymer: 6 parts of antioxidant 1010: 0.1 part, antioxidant 168: 0.1 part of lubricant PETS (pentaerythritol stearate): 0.2 part, triphenyl phosphite: 0.1 part of polytetrafluoroethylene and 0.1 part of polytetrafluoroethylene;
(2) after raw materials except the glass fiber are uniformly mixed in a high-speed mixer, the glass fiber is fed from a side feeding port, and is melted and extruded by an extruder, wherein the extrusion temperature is 210-250 ℃, the screw rotation speed is 350rpm, and then the mixture is cooled, dried and granulated into granules, so that the product is obtained.
Example 2
(1) Weighing the following components in parts by weight: PBT: 44 parts, PC: 7 parts of common alkali-free glass fiber: 22 parts, kaolin: 10 parts of brominated epoxy: 8.5 parts, antimony trioxide: 2 parts of ethylene-methyl acrylate copolymer: 6 parts of antioxidant 1010: 0.1 part, antioxidant 168: 0.1 part, a lubricant PETS: 0.2 part, triphenyl phosphite: 0.1 part of polytetrafluoroethylene and 0.1 part of polytetrafluoroethylene;
(2) after raw materials except the glass fiber are uniformly mixed in a high-speed mixer, the glass fiber is fed from a side feeding port, and is melted and extruded by an extruder, wherein the extrusion temperature is 210-240 ℃, the screw rotation speed is 350rpm, and then the mixture is cooled, dried and granulated into granules, so that the product is obtained.
Example 3
(1) Weighing the following components in parts by weight: PBT: 44 parts, PC: 7 parts of flattened glass fiber: 22 parts, calcium carbonate: 10 parts of brominated epoxy: 8.5 parts, antimony trioxide: 2 parts of ethylene-methyl acrylate copolymer: 6 parts of antioxidant 1010: 0.1 part, antioxidant 168: 0.1 part, a lubricant PETS: 0.2 part, triphenyl phosphite: 0.1 part of polytetrafluoroethylene and 0.1 part of polytetrafluoroethylene;
(2) after raw materials except the glass fiber are uniformly mixed in a high-speed mixer, the glass fiber is fed from a side feeding port, and is melted and extruded by an extruder, wherein the extrusion temperature is 210-250 ℃, the screw rotation speed is 350rpm, and then the mixture is cooled, dried and granulated into granules, so that the product is obtained.
Example 4
(1) Weighing the following components in parts by weight: PBT: 44 parts, PC: 7 parts of flattened glass fiber: 22 parts, kaolin: 10 parts of brominated epoxy: 8.5 parts, antimony trioxide: 2 parts of ethylene-methyl acrylate copolymer: 6 parts of antioxidant 1010: 0.1 part, antioxidant 168: 0.1 part, a lubricant PETS: 0.2 part, triphenyl phosphite: 0.1 part of polytetrafluoroethylene and 0.1 part of polytetrafluoroethylene;
(2) after raw materials except the glass fiber are uniformly mixed in a high-speed mixer, the glass fiber is fed from a side feeding port, and is melted and extruded by an extruder, wherein the extrusion temperature is 210-250 ℃, the screw rotation speed is 350rpm, and then the mixture is cooled, dried and granulated into granules, so that the product is obtained.
Comparative example
(1) Weighing the following components in parts by weight: PBT: 51 parts of common alkali-free glass fiber: 22 parts, calcium carbonate: 10 parts of brominated epoxy: 8.5 parts, antimony trioxide: 2 parts of ethylene-methyl acrylate copolymer: 6 parts of antioxidant 1010: 0.1 part, antioxidant 168: 0.1 part, a lubricant PETS: 0.2 part, triphenyl phosphite: 0.1 part of polytetrafluoroethylene and 0.1 part of polytetrafluoroethylene;
(2) after raw materials except the glass fiber are uniformly mixed in a high-speed mixer, the glass fiber is fed from a side feeding port, and is melted and extruded by an extruder, wherein the extrusion temperature is 210-250 ℃, the screw rotation speed is 350rpm, and then the mixture is cooled, dried and granulated into granules, so that the product is obtained.
The examples 1 to 4 and the comparative example are all injection-molded into circular plates with the diameter of 100mm and the thickness of 3mm, the maximum height A of the circular plates after warping is tested by a vernier caliper after the circular plates are placed for 48h at constant temperature and humidity, the warping degree of the material is represented by the ratio of the maximum height A to the diameter D of the circular plates, and the warping degree is A/D. Warpage and other physical and chemical properties are shown in the following table:
as can be seen from example 1 and the comparative example, the addition of PC reduces the crystallinity of the system, so that the PBT material has better warping resistance and improved impact performance. From the results of the examples 1, 2, 3 and 4, compared with the common alkali-free glass fiber and calcium carbonate, the flattening glass fiber and the kaolin are combined to enable the filled product to have toughness and warping resistance; in addition, the addition of the compound flame retardant enables all the examples and the comparisons to have good flame retardant performance. In conclusion, example 4 can satisfy the requirements of both flame retardancy and low warpage in the fields of high-grade electrical components, large electrical housings, and the like.
By adopting the scheme, the amorphous polymer PC is introduced into the raw materials, so that the crystallinity of the system is reduced, the warping property of the PBT material is improved, and the toughened PBT can be reinforced; and a compound flame retardant is introduced, so that the product has the flame retardant characteristic. Finally, the PBT/PC alloy material has good mechanical property, flame retardant property and anti-warping property, thereby expanding the application range of the PBT/PC alloy material in the fields of high-grade electrical components, large electrical housings and the like.
In addition, when the cross section of the glass fiber is flat, the strength of the formed product is greatly improved and the warping is greatly reduced; when the inorganic filler comprises kaolin, the orientation of glass fibers can be further improved, and the crystallization of PBT can be partially inhibited, so that the warping resistance of a filled product is improved, and the production cost can also be reduced.
The above embodiments are not intended to limit the form and style of the present invention, and any suitable changes or modifications made by those skilled in the art should be considered as not departing from the scope of the present invention.
Claims (10)
1. The reinforced flame-retardant low-warpage PBT alloy material is characterized by comprising the following raw materials in parts by weight: 35-50 parts of polybutylene terephthalate; 5-15 parts of polycarbonate; 15-30 parts of glass fiber; 5-15 parts of inorganic filler; 5-20 parts of a compound flame retardant; 5-10 parts of a toughening agent; 0.2-0.4 part of compound antioxidant; 0.1-0.3 part of lubricant; 0.1-0.3 part of ester exchange inhibitor; 0.1-0.3 part of anti-dripping agent.
2. The reinforced flame-retardant low-warpage PBT alloy material in claim 1, wherein:
the polybutylene terephthalate has an intrinsic viscosity of 0.8-1.0 dL/g.
3. The reinforced flame-retardant low-warpage PBT alloy material in claim 1, wherein:
the polycarbonate has a melt index of 20g/10min at 300 ℃ under 1.2 kg.
4. The reinforced flame-retardant low-warpage PBT alloy material in claim 1, wherein:
the glass fiber comprises at least one of common alkali-free glass fiber and flat glass fiber.
5. The reinforced flame-retardant low-warpage PBT alloy material in claim 1, wherein:
the inorganic filler comprises at least one of calcium carbonate, kaolin and glass beads.
6. The reinforced flame-retardant low-warpage PBT alloy material in claim 1, wherein:
the compound flame retardant is prepared by mixing a brominated flame retardant and an antimony synergistic flame retardant; wherein, the bromine flame retardant comprises at least one of decabromodiphenylethane, brominated epoxy and brominated styrene, and the antimony synergistic flame retardant comprises at least one of antimony trioxide and antimony trioxide master batch.
7. The reinforced flame-retardant low-warpage PBT alloy material in claim 1, wherein:
the toughening agent comprises at least one of ethylene-vinyl acetate copolymer, ethylene-methyl acrylate copolymer and ethylene-butyl acrylate-glycidyl methacrylate copolymer.
8. The reinforced flame-retardant low-warpage PBT alloy material in claim 1, wherein:
the compound antioxidant is prepared by mixing hindered phenol antioxidant and phosphite ester antioxidant; wherein the hindered phenol antioxidant comprises at least one of hindered phenol antioxidant 1010 and hindered phenol antioxidant 1076, and the phosphite antioxidant comprises at least one of phosphite antioxidant 626 and phosphite antioxidant 168;
the lubricant comprises at least one of silicone master batch, ethylene bisstearamide and pentaerythritol stearate;
the ester exchange inhibitor comprises at least one of triphenyl phosphite, disodium dihydrogen pyrophosphate and sodium dihydrogen phosphate;
the anti-dripping agent is polytetrafluoroethylene.
9. The preparation method of the reinforced flame-retardant low-warpage PBT alloy material is characterized by comprising the following steps of:
uniformly mixing polybutylene terephthalate, polycarbonate, inorganic filler, a compound flame retardant, a toughening agent, a compound antioxidant, a lubricant, an ester exchange inhibitor and an anti-dripping agent at high speed by a high-speed mixer to obtain a mixed material;
and step two, adding the mixed material into a main feeding port of a double-screw extruder, adding the glass fiber into a side feeding port of the double-screw extruder, and melting, extruding, cooling, drying and granulating the mixture into granules.
10. The preparation method of the reinforced flame-retardant low-warpage PBT alloy material in claim 9, wherein the preparation method comprises the following steps:
the temperature of each zone of the screw barrel of the double-screw extruder is set to be 210 ℃ and 250 ℃, and the rotating speed of the screw is 350 rpm.
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| CN112679917A (en) * | 2020-12-09 | 2021-04-20 | 中广核瑞胜发（厦门）新材料有限公司 | Cold-heat-resistant high-strength high-toughness PBT (polybutylene terephthalate) composite material suitable for full-shading lamp and preparation and application thereof |
| CN112898749A (en) * | 2021-01-26 | 2021-06-04 | 苏州塑发生物材料有限公司 | Low-warpage high-toughness glass fiber reinforced polylactic acid composite material and preparation method thereof |
| CN113292838A (en) * | 2021-07-05 | 2021-08-24 | 广东聚石化学股份有限公司 | Halogen-free low-warpage low-linear-expansion-coefficient extrusion-grade thin-wall flame-retardant polycarbonate composite material and preparation method thereof |
| CN113444354A (en) * | 2021-07-14 | 2021-09-28 | 横店集团得邦工程塑料有限公司 | high-CTI high-impact-resistance flame-retardant PC-PBT composite material and preparation method thereof |
| CN113817297A (en) * | 2021-09-23 | 2021-12-21 | 湖南恒屹新材料有限公司 | High-impact high-flame-retardant weather-resistant PBT/PC alloy material |
| CN113999498A (en) * | 2021-09-29 | 2022-02-01 | 金发科技股份有限公司 | Low-after-shrinkage high-toughness flame-retardant PBT/PC composition and preparation method and application thereof |
| CN114350121A (en) * | 2021-12-30 | 2022-04-15 | 广州市聚赛龙工程塑料股份有限公司 | High-toughness polyester composite material and preparation method and application thereof |
| CN114456553A (en) * | 2022-03-01 | 2022-05-10 | 上海聚威新材料股份有限公司 | Anti-warping laser welding PC/PBT composite material and preparation method thereof |
| WO2022110673A1 (en) * | 2020-11-30 | 2022-06-02 | 金发科技股份有限公司 | Shock-absorbing, damping, halogen-containing, flame-retardant, reinforced pbt material, and preparation method therefor |
| WO2023160153A1 (en) * | 2022-02-28 | 2023-08-31 | 金发科技股份有限公司 | Pbt composite material, preparation method therefor and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2022110673A1 (en) * | 2020-11-30 | 2022-06-02 | 金发科技股份有限公司 | Shock-absorbing, damping, halogen-containing, flame-retardant, reinforced pbt material, and preparation method therefor |
| CN112679917A (en) * | 2020-12-09 | 2021-04-20 | 中广核瑞胜发（厦门）新材料有限公司 | Cold-heat-resistant high-strength high-toughness PBT (polybutylene terephthalate) composite material suitable for full-shading lamp and preparation and application thereof |
| CN112679917B (en) * | 2020-12-09 | 2022-11-25 | 中广核瑞胜发（厦门）新材料有限公司 | Cold-heat-resistant high-strength high-toughness PBT (polybutylene terephthalate) composite material suitable for full-shading lamp and preparation and application thereof |
| CN112898749A (en) * | 2021-01-26 | 2021-06-04 | 苏州塑发生物材料有限公司 | Low-warpage high-toughness glass fiber reinforced polylactic acid composite material and preparation method thereof |
| CN113292838A (en) * | 2021-07-05 | 2021-08-24 | 广东聚石化学股份有限公司 | Halogen-free low-warpage low-linear-expansion-coefficient extrusion-grade thin-wall flame-retardant polycarbonate composite material and preparation method thereof |
| CN113444354A (en) * | 2021-07-14 | 2021-09-28 | 横店集团得邦工程塑料有限公司 | high-CTI high-impact-resistance flame-retardant PC-PBT composite material and preparation method thereof |
| CN113817297A (en) * | 2021-09-23 | 2021-12-21 | 湖南恒屹新材料有限公司 | High-impact high-flame-retardant weather-resistant PBT/PC alloy material |
| CN113999498A (en) * | 2021-09-29 | 2022-02-01 | 金发科技股份有限公司 | Low-after-shrinkage high-toughness flame-retardant PBT/PC composition and preparation method and application thereof |
| CN113999498B (en) * | 2021-09-29 | 2023-05-05 | 金发科技股份有限公司 | Low-post-shrinkage high-toughness flame-retardant PBT/PC composition, and preparation method and application thereof |
| CN114350121A (en) * | 2021-12-30 | 2022-04-15 | 广州市聚赛龙工程塑料股份有限公司 | High-toughness polyester composite material and preparation method and application thereof |
| WO2023160153A1 (en) * | 2022-02-28 | 2023-08-31 | 金发科技股份有限公司 | Pbt composite material, preparation method therefor and application thereof |
| CN114456553A (en) * | 2022-03-01 | 2022-05-10 | 上海聚威新材料股份有限公司 | Anti-warping laser welding PC/PBT composite material and preparation method thereof |
| CN114456553B (en) * | 2022-03-01 | 2024-01-19 | 上海聚威新材料股份有限公司 | Anti-warp laser welding PC/PBT composite material and preparation method thereof |
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Application publication date: 20200616 |