CN108047659B - PBT/PC/ASA composite material and preparation method thereof - Google Patents
PBT/PC/ASA composite material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a PBT/PC/ASA composite material, which comprises the following components in parts by weight: 30-50 parts of PBT resin; 10-15 parts by weight of PC resin; 5-10 parts by weight of ASA resin; 10-30 parts of special glass fiber; 4-10 parts of glass beads; 3-7 parts of a compound low-temperature toughening agent; 0.1-0.8 part by weight of antioxidant; 0.1 to 0.5 parts by weight of a lubricant. The invention also discloses a preparation method of the PBT/PC/ASA composite material. The ternary composite material prepared by the invention has the characteristics of low molding shrinkage and warp resistance, and can keep better impact toughness in a low-temperature environment.
Description
Technical Field
The invention belongs to the field of composite wave-absorbing material manufacturing, and particularly relates to a PBT/PC/ASA composite material and a preparation method thereof.
Background
Polybutylene terephthalate (PBT) is a thermoplastic engineering plastic with excellent comprehensive performance, and has higher mechanical strength, outstanding chemical reagent resistance, heat resistance and good electrical insulation performance. Meanwhile, the crystallization speed is high, the fluidity is good, the molding period is short, the injection molding processability is good, and the method is widely applied to the fields of automobile, electronic and electrical, mechanical manufacturing and the like. However, PBT has the defects of large molding shrinkage, low-temperature impact strength and the like.
The PC resin has higher impact strength, the ASA is an acrylonitrile-acrylate-styrene terpolymer and has good weather resistance and good dimensional stability, and if the PBT, the PC and the ASA are prepared into ternary blended alloy, the prepared alloy not only has the advantages of the PBT resin, but also has the impact resistance of the PC and the weather resistance and the dimensional stability of the ASA.
The prior patent CN105504753A mentions a preparation method of PBT/PC/ASA alloy material, and the ultraviolet-resistant composite material is obtained by adding light absorbent for modification, but the material is not subjected to reinforced modification, and the mechanical property of the material is lower. In actual production, glass fiber is usually adopted for reinforcement modification, so that the tensile strength, the bending strength and the impact strength can be improved. However, due to the anisotropic property of the common glass fiber, the glass fiber reinforced composite material has a serious warping problem when being used for preparing large thin-wall parts or parts with complex geometric shapes, and the application of the glass fiber reinforced composite material in certain fields is limited. In addition, the low-temperature impact strength can limit the application of the composite material in the field of low-temperature environment. Therefore, the development of the warp-resistant low-temperature impact-resistant glass fiber reinforced PBT/PC/ASA composite material is necessary.
Disclosure of Invention
The PBT/PC/ASA composite material provided by the invention has excellent warpage resistance and low-temperature impact property.
The invention also aims to provide a preparation method of the PBT/PC/ASA composite material.
The purpose of the invention is realized by the following technical scheme: a PBT/PC/ASA composite material comprises the following components in parts by weight:
the PBT resin is a polymer obtained by polycondensation of butanediol and terephthalic acid or a butylene terephthalate derivative, and the intrinsic viscosity of the PBT resin is 0.8-1.3 ml/g.
The PC resin is bisphenol A type aromatic polycarbonate, and the weight-average molecular weight of the polycarbonate is 20000-40000 g/mol.
The ASA resin is prepared by polymerizing SAN (styrene-acrylonitrile) serving as a matrix by an emulsion method or a bulk method, and the obtained rubber elastomer containing acrylate groups serves as a core, and a styrene-acrylonitrile copolymer serves as a shell, namely an acrylonitrile-styrene-acrylate terpolymer with a core-shell structure, wherein the weight content of the rubber elastomer containing acrylate groups in the terpolymer is 10-80%.
The special glass fiber is a flat glass fiber subjected to surface treatment by adopting a silane coupling agent with an epoxy group or an amino functional group, the ratio of the length diameter to the short diameter is 4:1, and the length diameter is 10-20 mu m.
The glass beads are solid glass beads, the size of the glass beads is 5-30 mu m, and the density of the glass beads is 0.1-0.7 g/ml.
The compound low-temperature flexibilizer is a composition of a styrene-acrylonitrile-glycidyl methacrylate copolymer and low-temperature vulcanized organic silicon rubber, wherein the weight ratio of the styrene-acrylonitrile-glycidyl methacrylate copolymer to the low-temperature vulcanized organic silicon rubber is 1.5: 1.
The antioxidant is one or two of hindered phenol and phosphite antioxidant, and the weight ratio of the hindered phenol to the phosphite antioxidant is 1: 2; the lubricant is one or a composition of two of silicone master batch or pentaerythritol stearate, and the weight ratio of the silicone master batch to the pentaerythritol stearate is 2:3 when the silicone master batch and the pentaerythritol stearate are compounded.
The preparation method of the PBT/PC/ASA composite material comprises the following steps:
(1) weighing the raw materials in parts by weight:
(2) adding the PBT resin, the PC resin, the ASA resin and the glass beads in the step (1) into a high-speed mixer, and mixing for 10-20 seconds;
(3) adding the compound low-temperature flexibilizer weighed in the step (1), the antioxidant and the lubricant into the mixture obtained in the step (2), and continuously mixing for 40 seconds;
(4) adding the mixed raw materials into a double-screw extruder, adding the special glass fiber weighed in the step (1) from a fiber adding port, carrying out melt extrusion at 220-260 ℃, cooling and granulating to obtain the composite material.
And (3) the rotating speed of the high-speed mixer in the step (2) is 400-600 rpm.
The PBT/PC/ASA composite material prepared by the invention uses the bow degree to represent the warpage resistance of the material, a JPCA printed board standard test method is adopted for testing, and the impact strength ratio of a sample strip under the conditions of low temperature and normal temperature is used for evaluating the low temperature impact resistance.
The principle of the invention is as follows:
the high impact resistance of PC and the low shrinkage of ASA in the ternary alloy material solve the problems of large molding shrinkage and low notch impact strength of PBT resin.
The mechanical property of the material can be improved by adding special glass fiber for reinforcement and modification. The use of the flat glass fiber can partially improve the warping problem of the common glass fiber caused by anisotropy. The surface of the flat glass fiber is modified by the silane coupling agent, and the silane coupling agent can simultaneously form effective chemical bonds or interaction with the matrix resin and the glass fiber, so that the compatibility between the glass fiber and the matrix resin is enhanced. On the other hand, the anti-warping performance of the material can be further improved by adding the highly symmetrical glass beads.
The glycidyl methacrylate can react with polyester, the styrene-acrylonitrile part has a structure similar to that of ASA resin, the styrene-acrylonitrile-glycidyl methacrylate can enhance the compatibility among resins, the low-temperature vulcanized silicone rubber can form transparent elastomers and has good low-temperature impact resistance, and the composition of the styrene-acrylonitrile-glycidyl methacrylate and the low-temperature vulcanized silicone rubber can be used as a compound low-temperature toughening agent to ensure good impact toughness of the material in a low-temperature environment.
Compared with the prior art, the invention has the advantages and effects that:
1. compared with the glass fiber reinforced PBT composite material, the ternary composite material prepared by the invention has the characteristics of low molding shrinkage and warp resistance, and can maintain better impact toughness in a low-temperature environment.
2. The anti-warping low-temperature impact-resistant glass fiber reinforced PBT/PC/ASA composite material prepared by the inventionThe material (example 3) has excellent mechanical properties, such as tensile strength of 76.4MPa, bending strength of 119.7MP and charpy notch impact strength of 62.2kJ/m2。
3. The warp-resistant low-temperature impact-resistant glass fiber reinforced PBT/PC/ASA composite material (example 3) prepared by the invention has outstanding warp-resistant performance and low-temperature resistance. The warping degree is 0.58%, and the anti-warping performance is obviously improved compared with that of a common glass fiber reinforced product (comparative example 2). The notch impact strength under the low temperature condition is 57.6kJ/m2The notched impact strength ratio under low temperature and normal temperature conditions is 92.6%, which is obviously higher than that of the ternary composite material in the prior art (comparative example 1).
Detailed Description
The present invention will be described in further detail with reference to examples, but the embodiments of the present invention are not limited thereto.
Example 1
Weighing 45 parts of PBT resin, 10 parts of PC resin, 5 parts of ASA resin, 3 parts of styrene-acrylonitrile-glycidyl methacrylate copolymer, 2 parts of low-temperature vulcanized silicone rubber, 0.6 part of antioxidant and 0.5 part of lubricant, adding the mixture into a high-speed mixer in a certain sequence, uniformly mixing, adding the mixture into a double-screw extruder through a main feeding hopper, adding 20 parts of special glass fiber into the double-screw extruder through a glass fiber port, melting, mixing, extruding and granulating the mixture by the double-screw extruder to obtain the warping-resistant low-temperature impact-resistant glass fiber reinforced PBT/PC/ASA composite material, wherein the temperatures of all sections are respectively: the temperature of a first area is 210 ℃, the temperature of a second area is 240 ℃, the temperature of a third area is 240 ℃, the temperature of a fourth area is 240 ℃, the temperature of a fifth area is 245 ℃, the temperature of a sixth area is 240 ℃, the temperature of a seventh area is 235 ℃, the temperature of an eighth area is 235 ℃, and the temperature of a machine head is 245 ℃; the rotation speed of the main machine is 300 rpm.
Example 2
Weighing 30 parts of PBT resin, 15 parts of PC resin, 10 parts of ASA resin, 3 parts of styrene-acrylonitrile-glycidyl methacrylate copolymer, 2 parts of low-temperature vulcanized silicone rubber, 0.6 part of antioxidant and 0.5 part of lubricant, adding the mixture into a high-speed mixer in a certain sequence, uniformly mixing, adding the mixture into a double-screw extruder through a main feeding hopper, adding 20 parts of special glass fiber into the double-screw extruder through a glass fiber port, melting, mixing, extruding and granulating the mixture by the double-screw extruder to obtain the warping-resistant low-temperature impact-resistant glass fiber reinforced PBT/PC/ASA composite material, wherein the temperatures of all sections are respectively: the temperature of a first area is 210 ℃, the temperature of a second area is 240 ℃, the temperature of a third area is 240 ℃, the temperature of a fourth area is 240 ℃, the temperature of a fifth area is 245 ℃, the temperature of a sixth area is 240 ℃, the temperature of a seventh area is 235 ℃, the temperature of an eighth area is 235 ℃, and the temperature of a machine head is 245 ℃; the rotation speed of the main machine is 300 rpm.
Example 3
Weighing 45 parts of PBT resin, 10 parts of PC resin, 5 parts of ASA resin, 6 parts of glass beads, 3 parts of styrene-acrylonitrile-glycidyl methacrylate copolymer, 2 parts of low-temperature vulcanized silicone rubber, 0.6 part of antioxidant and 0.5 part of lubricant, adding the mixture into a high-speed mixer in a certain sequence, uniformly mixing, adding the mixture into a double-screw extruder through a main feeding hopper, adding 16 parts of special glass fiber through a glass fiber port, and melting, mixing, extruding and granulating the mixture by the double-screw extruder to obtain the warping-resistant low-temperature impact-resistant glass fiber reinforced PBT/PC/ASA composite material, wherein the temperatures of all sections are respectively: the temperature of a first area is 210 ℃, the temperature of a second area is 240 ℃, the temperature of a third area is 240 ℃, the temperature of a fourth area is 240 ℃, the temperature of a fifth area is 245 ℃, the temperature of a sixth area is 240 ℃, the temperature of a seventh area is 235 ℃, the temperature of an eighth area is 235 ℃, and the temperature of a machine head is 245 ℃; the rotation speed of the main machine is 300 rpm.
Example 4
Weighing 45 parts of PBT resin, 10 parts of PC resin, 5 parts of ASA resin, 10 parts of glass microspheres, 5 parts of styrene-acrylonitrile-glycidyl methacrylate copolymer, 0.6 part of antioxidant and 0.5 part of lubricant, adding the mixture into a high-speed mixer in a certain sequence, uniformly mixing, adding the mixture into a double-screw extruder through a main feeding hopper, adding 10 parts of special glass fiber through a glass fiber port, and melting, mixing, extruding and granulating the mixture by the double-screw extruder to obtain the warping-resistant low-temperature impact-resistant glass fiber reinforced PBT/PC/ASA composite material, wherein the temperature of each section is respectively: the temperature of a first area is 210 ℃, the temperature of a second area is 240 ℃, the temperature of a third area is 240 ℃, the temperature of a fourth area is 240 ℃, the temperature of a fifth area is 245 ℃, the temperature of a sixth area is 240 ℃, the temperature of a seventh area is 235 ℃, the temperature of an eighth area is 235 ℃, and the temperature of a machine head is 245 ℃; the rotation speed of the main machine is 300 rpm.
Comparative example 1
Weighing 65 parts of PBT resin, 20 parts of PC resin, 7 parts of ASA resin, 1 part of triphenyl phosphate, 5 parts of polymethyl methacrylate-butadiene-styrene copolymer and 0.6 part of antioxidant, adding the materials into a high-speed mixer in a certain sequence, uniformly mixing, adding the materials into a double-screw extruder through a main feeding hopper, melting, mixing, extruding and granulating the materials by the double-screw extruder to obtain the PBT/PC/ASA composite material, wherein the temperature of each section is respectively as follows: the temperature of a first area is 190 ℃, the temperature of a second area is 230 ℃, the temperature of a third area is 235 ℃, the temperature of a fourth area is 235 ℃, the temperature of a fifth area is 235 ℃, the temperature of a sixth area is 235 ℃, the temperature of a seventh area is 235 ℃, the temperature of an eighth area is 235 ℃, and the temperature of a machine head is 230 ℃; the rotation speed of the main machine is 300 rpm.
Comparative example 2
Weighing 45 parts of PBT resin, 10 parts of PC resin, 5 parts of ASA resin, 3 parts of styrene-acrylonitrile-glycidyl methacrylate copolymer, 2 parts of low-temperature vulcanized silicone rubber, 0.6 part of antioxidant and 0.5 part of lubricant, adding the mixture into a high-speed mixer in a certain sequence, uniformly mixing, adding the mixture into a double-screw extruder through a main feeding hopper, adding 20 parts of common glass fiber by weight into the double-screw extruder through a glass fiber port, melting, mixing, extruding and granulating the mixture by the double-screw extruder to obtain the warping-resistant low-temperature impact-resistant glass fiber reinforced PBT/PC/ASA composite material, wherein the temperature of each section is respectively: the temperature of a first area is 210 ℃, the temperature of a second area is 240 ℃, the temperature of a third area is 240 ℃, the temperature of a fourth area is 240 ℃, the temperature of a fifth area is 245 ℃, the temperature of a sixth area is 240 ℃, the temperature of a seventh area is 235 ℃, the temperature of an eighth area is 235 ℃, and the temperature of a machine head is 245 ℃; the rotation speed of the main machine is 300 rpm.
The examples and comparative examples were tested for performance according to the following criteria:
test specimens were prepared by injection molding after drying the material at 120 ℃ for 4 hours in a forced air drying cabinet. Tensile strength, flexural strength and impact strength were tested according to ISO 527-2, ISO 178 and ISO 179 standards, respectively; the warping resistance is characterized by the bow degree of the material, and the material is tested by adopting a JPCA printed board standard test method, wherein a test sample is a 60 multiplied by 1mm square board. The results of the performance tests of inventive examples 1-4 and the results of comparative examples are shown in table 1.
TABLE 1 test results of composite materials obtained in examples 1 to 4 and comparative examples 1 to 2
The anti-warping low-temperature impact resistant glass fiber reinforced PBT/PC/ASA composite material of the embodiment 3 has excellent mechanical properties. Tensile strength of 76.4MPa, bending strength of 119.7MPa and charpy notch impact strength of 62.2kJ/m at normal temperature2. The notch impact strength is 57.6kJ/m under the low temperature condition of minus 40 DEG C2The low-temperature/normal-temperature impact strength ratio is 92.6%, which is obviously higher than that of the comparative example 1 (common ternary composite material). The warping degree of the material is 0.58%, and the warping resistance is obviously improved compared with that of a common glass fiber reinforced product (comparative example 2).
The following conclusions were drawn from the test data of the examples and comparative examples: the reinforced PBT/PC/ASA composite material prepared by adopting the silane coupling agent surface modified flat glass fiber has excellent mechanical property. Meanwhile, the glass beads and the flat glass fibers are used, so that the warping degree of the glass fiber reinforced composite material can be reduced, and the warping problem of a product caused by the anisotropy of the glass fibers is improved. The compound low-temperature toughening agent is adopted, so that the low-temperature/normal-temperature notch impact strength is higher, and the low-temperature toughness is outstanding.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (5)
1. The PBT/PC/ASA composite material is characterized by comprising the following raw materials in parts by weight:
the PBT resin is a polymer obtained by carrying out polycondensation reaction on butanediol and terephthalic acid, and the intrinsic viscosity of the PBT resin is 0.8-1.3 dl/g;
the PC resin is bisphenol A type aromatic polycarbonate, and the weight-average molecular weight of the polycarbonate is 20000-40000 g/mol;
the ASA resin is prepared by polymerizing SAN (styrene-acrylonitrile) serving as a matrix by an emulsion method or a bulk method, and taking a rubber elastomer containing acrylate groups as a core and a styrene-acrylonitrile copolymer as a shell, namely an acrylonitrile-styrene-acrylate terpolymer with a core-shell structure, wherein the weight content of the rubber elastomer containing acrylate groups in the terpolymer is 10-80%;
the special glass fiber is a flat glass fiber subjected to surface treatment by adopting a silane coupling agent with an epoxy group or an amino functional group, the ratio of the length diameter to the short diameter is 4:1, and the length diameter is 10-20 mu m;
the compound low-temperature flexibilizer is a composition of a styrene-acrylonitrile-glycidyl methacrylate copolymer and low-temperature vulcanized organic silicon rubber, wherein the weight ratio of the styrene-acrylonitrile-glycidyl methacrylate copolymer to the low-temperature vulcanized organic silicon rubber is 1.5: 1.
2. The PBT/PC/ASA composite of claim 1 wherein: the glass beads are solid glass beads, the size of the glass beads is 5-30 mu m, and the density of the glass beads is 0.1-0.7 g/ml.
3. The PBT/PC/ASA composite of claim 1 wherein: the antioxidant is one or two of hindered phenol and phosphite antioxidant, and the weight ratio of the hindered phenol to the phosphite antioxidant is 1: 2; the lubricant is one or a composition of two of silicone master batch or pentaerythritol stearate, and the weight ratio of the silicone master batch to the pentaerythritol stearate is 2:3 when the silicone master batch and the pentaerythritol stearate are compounded.
4. The preparation method of the PBT/PC/ASA composite material according to any one of claims 1 to 3, wherein the method comprises the following steps:
(1) weighing the raw materials in parts by weight:
(2) adding the PBT resin, the PC resin, the ASA resin and the glass beads in the step (1) into a high-speed mixer, and mixing for 10-20 seconds;
(3) adding the compound low-temperature flexibilizer weighed in the step (1), the antioxidant and the lubricant into the mixture obtained in the step (2), and continuously mixing for 40 seconds;
(4) adding the mixed raw materials into a double-screw extruder, adding the special glass fiber weighed in the step (1) from a fiber adding port, carrying out melt extrusion at 220-260 ℃, cooling and granulating to obtain the composite material.
5. The preparation method of the PBT/PC/ASA composite material according to claim 4, wherein the PBT/PC/ASA composite material is characterized in that: and (3) the rotating speed of the high-speed mixer in the step (2) is 400-600 rpm.
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| CN109836786A (en) * | 2019-03-04 | 2019-06-04 | 林元钦 | A kind of PC/ASA/PBT alloy material and preparation method thereof for 3D printing |
| CN113416322B (en) * | 2021-05-06 | 2022-03-04 | 常州大学 | Preparation method and application of polycarbonate low-temperature toughening master batch with compatibilization function |
| CN113337089B (en) * | 2021-07-22 | 2022-09-23 | 合肥圆融新材料有限公司 | Glass fiber reinforced PBT (polybutylene terephthalate) composite material and preparation method thereof |
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| EP0902052A1 (en) * | 1997-09-15 | 1999-03-17 | General Electric Company | Aliphatic polyester-acrylic blend molding composition |
| CN102504499A (en) * | 2011-10-26 | 2012-06-20 | 惠州市沃特新材料有限公司 | Polybutylece terephthalate (PBT) engineering plastic, and preparation method and application thereof |
| CN107083030A (en) * | 2017-06-02 | 2017-08-22 | 浙江华杰材料科技有限公司 | A kind of low warpage high-strength glass fiber enhanced PBT/ASA alloy materials and preparation method thereof |
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| CN102424717A (en) * | 2011-11-24 | 2012-04-25 | 南京鸿瑞塑料制品有限公司 | Preparation method for reinforced and toughened polymer material |
| CN104693744A (en) * | 2013-12-10 | 2015-06-10 | 青岛同创节能环保工程有限公司 | PC(polycarbonate)/PBT(polybutylece terephthalate) alloy with excellent low-temperature-resistant performance and weather-resistant performance and preparing method thereof |
| CN105713355A (en) * | 2015-12-25 | 2016-06-29 | 上海胜南复合材料有限公司 | High-performance warping-proof glass fiber reinforced PBT (polybutylene terephthalate)/PC (polycarbonate) alloy material |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0902052A1 (en) * | 1997-09-15 | 1999-03-17 | General Electric Company | Aliphatic polyester-acrylic blend molding composition |
| CN102504499A (en) * | 2011-10-26 | 2012-06-20 | 惠州市沃特新材料有限公司 | Polybutylece terephthalate (PBT) engineering plastic, and preparation method and application thereof |
| CN107083030A (en) * | 2017-06-02 | 2017-08-22 | 浙江华杰材料科技有限公司 | A kind of low warpage high-strength glass fiber enhanced PBT/ASA alloy materials and preparation method thereof |
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