CN113956596B - Low-dielectric high-toughness COP/LDPE alloy material and preparation method thereof - Google Patents
Low-dielectric high-toughness COP/LDPE alloy material and preparation method thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L45/00—Compositions of homopolymers or copolymers of compounds having no unsaturated aliphatic radicals in side chain, and having one or more carbon-to-carbon double bonds in a carbocyclic or in a heterocyclic ring system; Compositions of derivatives of such polymers
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- C—CHEMISTRY; METALLURGY
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/20—Applications use in electrical or conductive gadgets
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/08—Polymer mixtures characterised by other features containing additives to improve the compatibility between two polymers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2207/00—Properties characterising the ingredient of the composition
- C08L2207/06—Properties of polyethylene
- C08L2207/066—LDPE (radical process)
Abstract
The invention relates to the technical field of high polymer materials, in particular to a low-dielectric high-toughness COP/LDPE alloy material and a preparation method thereof. The low-dielectric high-toughness COP/LDPE alloy material comprises the following components: COP resin, LDPE resin, compatibilizer, and other additives; the ratio of the COP resin to the LDPE resin to the compatilizer is (65-76) to (20-30) in parts by weight: (3-5). The COP/LDPE alloy material has excellent notch impact strength, not only maintains low dielectric property, but also makes up the defect of insufficient toughness of COP resin, has good temperature resistance, can meet the application requirement of products, and has excellent properties of low dielectric property and high toughness; the low-dielectric high-toughness COP/LDPE alloy material provided by the invention can be processed into various parts by injection molding, and the prepared product has lower dielectric constant and dielectric loss and good impact resistance.
Description
Technical Field
The invention relates to the technical field of high polymer materials, in particular to a low-dielectric high-toughness COP/LDPE alloy material and a preparation method thereof.
Background
Cycloolefin Polymer is abbreviated as COP (Cyclic Olefin Polymer), and is an amorphous thermoplastic resin polymerized by taking cycloolefin (norbornene, ethylidene norbornene, dicyclopentadiene and the like) as a monomer. It has the characteristics of low density, low water absorption, high transparency, high heat resistance, low dielectric loss, low dielectric constant (especially good high-frequency performance), high rigidity and the like, however, the notch impact strength is low, the toughness is poor, and the alloy can not be used for parts with high impact requirements, so that the application of the alloy is severely limited.
Therefore, in order to overcome the drawbacks of the conventional COP materials, it is necessary to develop a modified COP material having good impact resistance without lowering the dielectric properties thereof.
The Chinese patent application with the application number of CN202010242865.4 and the publication date of 2020 and 07/10 discloses a transparent toughened cycloolefin copolymer, which comprises the following components in parts by weight: COP 77-92 parts; 5-20 parts of a toughening agent; 2-3 parts of a compatilizer; 0.3-0.5 part of antioxidant; 0.3-0.5 part of lubricant; the weight-average molecular weight of the COP is 10000-50000; the toughening agent is at least one of methacrylic acid-butadiene-styrene copolymer, acetic acid-vinyl acetate copolymer, ethylene-methyl acrylate copolymer, ethylene-butyl acrylate copolymer and styrene-acrylonitrile-butadiene core-shell polymer. However, the application focuses on ensuring the light transmittance and the toughness of the material, and does not mention whether the low dielectric property of the material can be well maintained, nor provides corresponding characterization data to reflect the dielectric property of the material.
Disclosure of Invention
The method aims to solve the problem that the prior COP material in the background art has insufficient toughness and cannot be used for parts with higher impact requirements, so that the application of the COP material is severely limited. The invention provides a low-dielectric high-toughness COP/LDPE alloy material, which comprises the following components: COP resin, LDPE resin, compatibilizer, and other additives;
the ratio of the COP resin to the LDPE resin to the compatilizer is (65-76) to (20-30) in parts by weight: (3-5).
The invention adopts LDPE resin and COP resin to prepare COP/LDPE alloy material, low Density Polyethylene (LDPE) is typical high toughness polyolefin resin, and has excellent impact resistance even at the temperature below 50 ℃ below zero, and the LDPE has no polar group in the molecular structure, has excellent dielectric property, has the dielectric constant of 2.25-2.35, has dielectric loss less than 0.0005, is slightly influenced by frequency, and is suitable for preparing high frequency insulating material; however, in the existing commercial products and literature data, a technical scheme for preparing an alloy material by adopting COP and LDPE is not disclosed, the invention effectively fills the research blank and the market blank of the COP/LDPE alloy material, provides the COP/LDPE alloy material to meet the market requirement, and considers that the COP is a noncrystalline material and the LDPE is a crystalline material, and a large technical obstacle exists in the mixing and compatibility process of the COP and the LDPE.
Therefore, on the one hand, the technical scheme of preparing the low-dielectric high-toughness COP/LDPE alloy material by adopting COP and LDPE is not disclosed in the existing commercial products and literature data, and the invention effectively fills the research blank and the market blank of the COP/LDPE alloy material.
On the other hand, the low-dielectric high-toughness COP/LDPE alloy material provided by the invention can be processed into various parts by injection molding, can be used for producing parts such as 5G components, electronic communication components, intelligent household appliance shells, intelligent wearable equipment, high-temperature connectors and the like, and has low dielectric constant and dielectric loss and good impact resistance, and can meet market demands.
In one embodiment, the COP resin has a glass transition temperature greater than 130 ℃ and a melt flow rate greater than 15g/10min (280 ℃,2.16 kg).
Preferred COP resins of the invention have a melt flow rate of greater than 15g/10min and a glass transition temperature of greater than 130 ℃. On one hand, when the melt flow rate is less than the limit value, the fluidity of the COP resin is insufficient, and the processing processes of mixing, melting, extruding, molding and the like of the COP resin and other components are influenced, so that the performance of the prepared COP/LDPE alloy material is adversely influenced; on the other hand, COP resin has high heat resistance, but the heat resistance is adversely affected by adding LDPE, and COP resin with the glass transition temperature of more than 130 ℃ is preferred to ensure that COP/LDPE alloy material has good heat resistance. According to the invention, COP resin with glass transition temperature of more than 130 ℃ and melt flow rate of more than 15g/10min is preferably selected, so that the performance of the prepared COP/LDPE alloy material is further improved.
In one embodiment, the LDPE resin has a melt flow rate of less than 3.0g/10min (190 ℃,2.16 kg).
Preference is given to LDPE resins having a melt flow rate of less than 3.0g/10 min: COP resin and LDPE resin are blended, melted and extruded to prepare COP/LDPE alloy, so the influence of processing parameters such as processing temperature and the like on the processing effect needs to be comprehensively considered aiming at the performance of the COP resin and the LDPE resin in the processing process; in the case of satisfying COP resin processing conditions (higher temperature), if the melt flow rate of the LDPE resin is greater than the limit value, the probability of decomposition of the LDPE resin at high temperature is greater, and the desired technical effect cannot be obtained on the contrary; on one hand, the low-melt-index LDPE still ensures the flowability at high temperature, and on the other hand, the low-melt-index LDPE has relatively excellent and stable performance in all aspects, and is favorable for further ensuring the improvement of the COP/LDPE alloy material performance. Preferably, the melt flow rate of the LDPE resin is 1.0-3.0 g/10min, the LDPE resin with the melt flow rate of 1.0-3.0 g/10min can meet the performance requirement, and the LDPE with the parameter is easy to obtain in the market and has high selectivity.
In one embodiment, the compatibilizer is at least one of ethylene propylene diene monomer grafted maleic anhydride and styrene-ethylene-butylene-styrene block copolymer grafted maleic anhydride; the grafting rate of the maleic anhydride in the ethylene propylene diene monomer grafted maleic anhydride is more than 0.8%, and the grafting rate of the maleic anhydride in the styrene-ethylene-butylene-styrene block copolymer grafted maleic anhydride is more than 1.0%.
The compatilizer is preferably ethylene propylene diene monomer grafted maleic anhydride (EPDM-g-MAH) and styrene-ethylene-butylene-styrene block copolymer grafted maleic anhydride (SEBS-g-MAH), compared with other compatilizers grafted by maleic anhydride, the EPDM and the SEBS are saturated polyolefin elastomers, have lower dielectric constant and excellent impact resistance, and have smaller changes in the two indexes (dielectric constant and impact resistance) on maleic anhydride grafts (namely EPDM-g-MAH and SEBS-g-MAH), and the two grafts are selected as the compatilizer, so that the influence on the dielectric property and the impact property of the alloy material is smaller, and the improvement on the COP/LDPE alloy material property is further guaranteed; EPDM-g-MAH with the grafting rate of maleic anhydride being more than 0.8% and SEBS-g-MAH with the grafting rate of maleic anhydride being more than 1.0% are preferred, and through experiments, if the grafting rates of the EPDM-g-MAH and the SEBS-g-MAH are lower than the limited values, the addition amount of the compatilizer needs to be increased; and EPDM-g-MAH or SEBS-g-MAH with the grafting rate of the parameter is easy to obtain in the market and has high selectivity.
In one embodiment, the other additives include antioxidants and lubricants.
In one embodiment, the composition comprises the following components in parts by weight: 65-76 parts of COP resin, 20-30 parts of LDPE resin, 3-5 parts of compatilizer, 0.3-0.5 part of antioxidant and 0.1-0.3 part of lubricant.
In one embodiment, the antioxidants include primary antioxidants and secondary antioxidants; the main antioxidant is one or a combination of more of an antioxidant 1010 and an antioxidant 1076; the auxiliary antioxidant is one or a combination of antioxidants 168 and 626.
In one embodiment, the mass ratio of the primary antioxidant to the secondary antioxidant is 1.
In one embodiment, the lubricant is one or more of ethylene bis stearamide, zinc stearate and calcium stearate.
The invention also provides a preparation method of the low-dielectric high-toughness COP/LDPE alloy material, which comprises the following steps:
s100, weighing the COP resin, the LDPE resin, the compatilizer, the antioxidant and the lubricant according to a certain weight, and mixing to obtain a mixture M;
s200, adding the mixture M into a double-screw extruder, and performing melt extrusion granulation on the materials in the double-screw extruder to obtain the low-dielectric high-toughness COP/LDPE alloy material.
Compared with the prior art, the invention has the following effects:
the COP/LDPE alloy material provided by the invention has excellent notch impact strength and low dielectric property, overcomes the defect of insufficient toughness of COP resin, has good temperature resistance, can meet the application requirements of products, and has excellent properties of low dielectric property and high toughness. Therefore, the low-dielectric high-toughness COP/LDPE alloy material provided by the invention can be processed into various parts by injection molding, can be used for producing parts such as 5G components, electronic communication components, intelligent household appliance shells, intelligent wearable equipment, high-temperature connectors and the like, and has low dielectric constant and dielectric loss and good impact resistance, and can meet market demands.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the following description will clearly and completely describe the technical solutions in the embodiments of the present invention, and it is obvious that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, which can be obtained by a person skilled in the art without making any creative effort based on the embodiments in the present invention, belong to the protection scope of the present invention.
The invention provides a preparation method of a low-dielectric high-toughness COP/LDPE alloy material, which comprises the following steps:
(1) Weighing the COP resin, the LDPE resin, the compatilizer, the antioxidant and the lubricant according to a certain weight, putting the mixture into a high-speed mixer, and mixing for 2-3 min to disperse and uniformly mix the raw material components to obtain a mixture M;
(2) Adding the mixture M into a double-screw extruder, and performing melt extrusion granulation on the materials in the double-screw extruder to obtain a product, namely obtaining the low-dielectric high-toughness COP/LDPE alloy material; wherein the melt extrusion temperature is 240-280 ℃, the length-diameter ratio of a screw of the double-screw extruder is (40-48) to 1, and the rotating speed of the screw is (400-500) rpm.
The invention also provides the following examples and comparative examples:
the formulations (unit: parts by weight) of the examples and comparative examples provided by the present invention are shown in table 1 below:
TABLE 1
Wherein, the raw material components in the examples and comparative examples in table 1 are consistent in type selection, and the components are specifically:
the COP resin is K22R produced by the Japanese Ralstonia, the glass transition temperature of the COP resin is 143 ℃, and the melt flow rate is 32g/10min (280 ℃,2.16 kg);
the LDPE resin is DJ210 produced by Shanghai petrochemical industry, and the melt flow rate of the LDPE resin is 2.1g/10min (190 ℃,2.16 kg);
the compatilizer is styrene-ethylene-butylene-styrene block copolymer grafted maleic anhydride (SEBS-g-MAH), specifically FG1901 produced by Keteng of the United states, and the grafting rate of the maleic anhydride in the SEBS-g-MAH is about 1.7%;
the antioxidant is an antioxidant 1010 and an antioxidant 168 produced by BASF, wherein the mass ratio of the antioxidant 1010 to the antioxidant 168 is 1; the lubricant is calcium stearate produced by Singapore FACI.
According to the formula shown in Table 1, the raw material components in the examples and the comparative examples are prepared into COP/LDPE alloy materials according to the following preparation method, and the preparation steps are as follows:
(1) Weighing the COP resin, the LDPE resin, the compatilizer, the antioxidant and the lubricant according to a certain weight, putting into a high-speed mixer, and mixing for 3min to disperse and uniformly mix the raw material components to obtain a mixture M; (2) Adding the mixture M into a double-screw extruder, and performing melt extrusion granulation on the materials in the double-screw extruder to obtain a product, namely obtaining the low-dielectric high-toughness COP/LDPE alloy material; wherein the melt extrusion temperature is 240 ℃ to 280 ℃ (the temperatures of all zones of the double-screw extruder are 240 ℃, 260 ℃, 280 ℃ and 280 ℃ from one zone to ten zones in turn, the head temperature was 280 ℃ C.) and the screw length-diameter ratio of the twin-screw extruder was 44, and the screw rotation speed was 450rpm.
The COP/LDPE alloy materials prepared in the examples and the comparative examples were tested for the related performance indexes under the same test conditions, and the test results are shown in the following table 2:
TABLE 2
Wherein the notched impact strength test standard of the cantilever beam (Izod) is ISO180; the test standard for dielectric constant is IEC60250: the test frequency is 1MHz; the heat distortion temperature was measured according to ISO 75-2.
As can be seen from the test results of table 2:
the test results of examples 1-5 show that: the COP/LDPE alloy material provided by the invention has lower dielectric constant and dielectric loss, and good impact resistance and heat resistance; the prepared COP/LDPE alloy material has excellent notch impact strength, and the notch impact strength of the normal-temperature cantilever beam is more than or equal to 25KJ/m 2 The impact strength of the low-temperature cantilever beam notch is more than or equal to 12KJ/m 2 The defect of poor impact strength of a COP resin notch is obviously improved, the dielectric constant is as low as 2.33, the dielectric loss is as low as 0.0014 under the test frequency of 1MHz, and the COP resin has good temperature resistance and can meet the application requirements of products;
comparative example 1 is compared with example 1 except that the LDPE resin, the compatibilizer in example 1 were replaced with COP resin, and the results show that: the impact property of the material is poor by using the COP resin alone, and the dielectric constant and the dielectric loss are obviously higher than those of the material in the embodiment 1;
comparative example 2 compares to examples 1 and 2, except that the compatibilizer in examples 1 and 2 was replaced with an LDPE resin, and the results show that: comparative example 2 shows an improvement in impact properties and a reduction in dielectric constant and dielectric loss as compared with comparative example 1 using COP resin alone, but the improvement in impact strength is small, and particularly, low-temperature impact strength is still poor, compared to examples 1-2, which show a significant improvement in impact properties while the dielectric constant and dielectric loss are maintained at a low level.
Compared with the example 1, the difference of the comparative example 3 is that the proportion of the COP resin and the LDPE resin in the example 1 is adjusted, the amount of the COP resin is increased, the amount of the LDPE resin is reduced, and the result shows that: the impact strength of comparative example 3 was significantly reduced, and especially the low-temperature impact strength was also only 6.3KJ/m 2 The toughness of the material is insufficient, so that the application of the material is severely limited; compared with the example 5, the difference of the comparative example 4 is that the proportion of the COP resin and the LDPE resin in the example 5 is adjusted, the amount of the COP resin is reduced, and the amount of the LDPE resin is increased, and the result shows that: compared with example 5, the impact property, dielectric constant and dielectric loss are equivalent to those of example 5, but the heat resistance is obviously reduced, and the insufficient heat resistance can meet the application requirements of products. According to the invention, by limiting the proportion of the COP resin, the LDPE resin and the compatilizer, the COP/LDPE alloy material prepared through the synergistic effect of the components has relatively low dielectric constant and dielectric loss and good impact resistance, makes up the defect of toughness of the COP resin, keeps good heat resistance and can meet the application requirement of the product.
It should be noted that:
in addition to the practical choices embodied in the above specific examples, the COP resin may be selected from COP resins having a glass transition temperature of greater than 130 ℃ and a melt flow rate of greater than 15g/10min (280 ℃,2.16 kg), and the glass transition temperature and the melt flow rate may be within the above ranges, including but not limited to the practical choices embodied in the above examples;
in addition to the practical choices embodied in the above specific examples, the melt flow rate of the LDPE resin may be less than 3.0g/10min (190 ℃,2.16 kg) and includes, but is not limited to, the practical choices embodied in the above examples; the melt flow rate of the LDPE resin is preferably selected from 1.0 to 3.0g/10min.
In addition to the practical options presented in the specific examples above, the compatibilizer may be at least one of ethylene propylene diene monomer grafted maleic anhydride (EPDM-g-MAH), styrene-ethylene-butylene-styrene block copolymer grafted maleic anhydride (SEBS-g-MAH); the grafting rate of the maleic anhydride in the EPDM-g-MAH is more than 0.8 percent, the grafting rate of the maleic anhydride in the SEBS-g-MAH is more than 1.0 percent, and the grafting rate of the maleic anhydride can be within the corresponding range, including but not limited to the practical choices embodied in the above embodiments;
in addition to the practical choices embodied in the above specific examples, the ratio of the COP resin, the LDPE resin and the compatibilizer is (65-76) to (20-30): (3-5); the combination of the components in the above-mentioned mass ratio ranges can include, but is not limited to, the practical choices as embodied in the above-mentioned examples.
In addition to the actual choices embodied in the above specific embodiments, the antioxidant may be compounded by using a primary antioxidant and a secondary antioxidant in other proportions, wherein the primary antioxidant may be one or a combination of more than one of the antioxidants 1010 and 1076, and the secondary antioxidant may be one or a combination of more than one of the antioxidants 168 and 626, including but not limited to the actual choices embodied in the above embodiments; preferably, the main antioxidant and the auxiliary antioxidant are compounded according to the mass ratio of 1;
in addition to the practical choices embodied in the above specific embodiments, the lubricant may be selected from one or more of ethylene bis stearamide, zinc stearate, and calcium stearate, including but not limited to the practical choices embodied in the above embodiments.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and these modifications or substitutions do not depart from the spirit of the corresponding technical solutions of the embodiments of the present invention.
Claims (10)
1. The low-dielectric high-toughness COP/LDPE alloy material is characterized by comprising the following components: COP resin, LDPE resin, compatibilizer, and other additives;
the ratio of the COP resin to the LDPE resin to the compatilizer is (65-76) to (20-30) in parts by weight: (3-5).
2. The low-dielectric high-toughness COP/LDPE alloy material as claimed in claim 1, wherein the COP resin has a glass transition temperature of greater than 130 ℃ and a melt flow rate of greater than 15g/10min.
3. The low-dielectric high-toughness COP/LDPE alloy material as claimed in claim 1, wherein the melt flow rate of the LDPE resin is less than 3.0g/10min.
4. The low-dielectric high-toughness COP/LDPE alloy material as claimed in claim 1, wherein the compatibilizer is at least one of ethylene propylene diene monomer grafted maleic anhydride and styrene-ethylene-butylene-styrene block copolymer grafted maleic anhydride;
the grafting rate of maleic anhydride in the ethylene propylene diene monomer grafted maleic anhydride is more than 0.8%, and the grafting rate of maleic anhydride in the styrene-ethylene-butylene-styrene block copolymer grafted maleic anhydride is more than 1.0%.
5. The low dielectric high toughness COP/LDPE alloy material as claimed in claim 1, wherein said other additives comprise antioxidants and lubricants.
6. The low-dielectric high-toughness COP/LDPE alloy material as claimed in claim 5, comprising the following components in parts by weight:
65-76 parts of COP resin, 20-30 parts of LDPE resin, 3-5 parts of compatilizer, 0.3-0.5 part of antioxidant and 0.1-0.3 part of lubricant.
7. The low-dielectric high-toughness COP/LDPE alloy material as claimed in claim 5, wherein the antioxidant comprises a primary antioxidant and a secondary antioxidant;
the main antioxidant is one or a combination of more of an antioxidant 1010 and an antioxidant 1076; the auxiliary antioxidant is one or a combination of antioxidants 168 and 626.
8. The low-dielectric high-toughness COP/LDPE alloy material as claimed in claim 7, wherein the mass ratio of the primary antioxidant to the secondary antioxidant is 1.
9. The low dielectric high toughness COP/LDPE alloy material as claimed in claim 5, wherein the lubricant is one or more of ethylene bis stearamide, zinc stearate, calcium stearate.
10. The preparation method of the low dielectric high toughness COP/LDPE alloy material as claimed in claims 1 to 9, characterized by comprising the following steps:
s100, weighing the COP resin, the LDPE resin, the compatilizer, the antioxidant and the lubricant according to a certain weight, and mixing to obtain a mixture M;
s200, adding the mixture M into a double-screw extruder, and performing melt extrusion granulation on the materials in the double-screw extruder to obtain the low-dielectric high-toughness COP/LDPE alloy material.
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| Cyclic olefin copolymers;Ronald R. Lamonte等;《Advanced Materials and Processes》;20010301;第159卷(第3期);第33-36页 * |
| Mechanical properties and compatibility of sulfonated poly (ethylene terephthalate)/cyclic olefin copolymer/maleic anhydride-grafted polyethylene-octene elastomer;Hsien-Tang Chiu等;《Polymer-Plastics Technology and Engineering》;20100622;第47卷(第7期);第649-654页 * |
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