CN110885496A - Antistatic heat-conducting polyolefin composition and preparation method thereof - Google Patents
Antistatic heat-conducting polyolefin composition and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a polyolefin composition, which mainly comprises the following components: 20-100 parts of polyolefin resin, 10-50 parts of functional filler, 0.1-5 parts of compatilizer and 0.1-1 part of additive, wherein the mass ratio of the polyolefin resin to the functional filler is (5-10): 1; wherein, the polyolefin resin is selected from one or more of polyethylene and polypropylene; the functional filler is ZnO/nano silicon oxide SBA-15. The invention combines the excellent electrical insulation property, low water absorption rate and low water vapor transmission rate of polyolefin, simultaneously realizes the functions of antistatic property and high thermal conductivity by adding a small amount of functional filler, has lower cost and obtains remarkable effect.
Description
Technical Field
The invention relates to an antistatic heat-conducting polyolefin composition and a preparation method thereof, belonging to the technical field of polyolefin functional mother materials.
Background
The polypropylene PP is one of five general-purpose plastics, has rich raw material sources, low price, easy processing and forming and excellent product comprehensive performance, and is widely applied. As a semicrystalline polymer material, PP has excellent properties such as high rigidity, corrosion resistance, and electrical insulation, but PP has the following disadvantages: (1) PP is a high-insulation material and has a volume resistivity of 1016～1018Omega cm, surface resistance 1016～1017Omega, a large amount of static charges can be generated on the surface in the process of friction, stripping or induction, which not only influences the use and manufacture of PP materials, but also has potential safety hazards; (2) PP has a very low coefficient of thermal conductivity and the material has poor thermal conductivity. Therefore, the research on the antistatic modification of polypropylene has been always a hot direction.
In the prior art, two methods for PP antistatic modification mainly comprise an antistatic agent adding method and a conductive filler adding method; the first method can achieve the antistatic effect only by depending on the humidity of the environment, so the application range is narrow; in the second method, the carbon fillers, mainly traditional carbon fillers such as conductive carbon black, are added in the prior art when the method is applied more mature; however, the most serious disadvantage of the conventional carbon-based filler is that the carbon-based filler is black, and when the carbon-based filler is added in a large amount, the color adjustability of the product is poor. The metal oxide and the conductive mica sheet can also be used as conductive fillers, the metal oxide can meet the requirements of transparency and static resistance, but the antistatic performance is poor, a large amount of the metal oxide and the conductive mica sheet are generally required to be added to achieve the antistatic effect, and the problems of uneven distribution and agglomeration can occur when the addition amount of the fillers is too large.
On the other hand, with the rapid development of the information industry, the demand of high heat dissipation interface materials is increasing, especially in the fields of electric appliances and microelectronics, because heat pipes, integrated circuits and power are used in large quantities in the field of electronic informationThe information products are developed towards high power words, high integration and the like, so that the novel polymer composite material can be widely applied to accessories of the information products, such as packaging materials of the products, and the development of the heat-conducting insulating composite material with excellent performance has great significance. In the prior art, the heat conduction materials mainly have 3 types: (1) metals such as Au, Ag, Cu, Fe, Mg, Al and the like, and although the metal materials have high thermal conductivity, the metal materials have poor electrical insulation, poor chemical corrosion resistance, heavy weight, difficult processing and forming and high production process cost; (2) metal oxides such as Al2O3ZnO, MgO, BeO and the like, metal nitrides such as magnesium nitride, calcium nitride, strontium nitride and the like, and although the materials have good electrical insulation, the impact performance is poor, and the production process cost is high; (3) non-metallic heat conductive materials such as carbon black, graphite, and the like have relatively high thermal conductivity, but have relatively poor electrical insulation and mechanical properties.
In addition to the above technical problems, there is a problem that has not been solved: the problem of the addition of the heat conducting material is that if the addition amount is less, the effect is not good or poor, and if the addition amount is more, the agglomeration phenomenon can occur, so that the whole master batch system is ineffective and cannot be used, which almost becomes a difficult problem which needs to be solved in the field all the time.
Therefore, it is apparent that the development of a novel polyolefin composition having both good antistatic properties and high thermal conductivity has positive practical significance.
Disclosure of Invention
The invention aims to provide an antistatic heat-conducting polyolefin composition which simultaneously has good antistatic performance and high heat conductivity.
In order to achieve the purpose of the invention, the technical scheme adopted by the invention is as follows: an antistatic heat-conducting polyolefin composition mainly comprises the following components in parts by mass:
wherein the mass ratio of the polyolefin resin to the functional filler is 5-10: 1;
wherein, the polyolefin resin is selected from one or more of polyethylene and polypropylene; the functional filler is ZnO/nano silicon oxide SBA-15, and the preparation method comprises the following steps:
(1) weighing nanometer silicon oxide SBA-15 and Zn (CH)3COO)2·2H2O, and the atomic ratio of Si/Zn is 1:1 to 30;
(2) reacting the above Zn (CH)3COO)2·2H2Putting O into NaOH ethanol water solution, adding a silane coupling agent and nano silicon oxide SBA-15 after uniformly stirring, putting into a high-pressure kettle after fully stirring, and reacting for at least 5 hours at 80-120 ℃;
(3) and after the reaction is finished, filtering, washing and drying to obtain the functional filler.
Hereinbefore, the polyolefin resin may be 25 parts, 30 parts, 35 parts, 40 parts, 50 parts, 60 parts, 70 parts, 80 parts, 90 parts, 92 parts, 94 parts, 95 parts, 96 parts, 98 parts.
6 parts, 7 parts, 8 parts, 10 parts, 15 parts, 20 parts, 22 parts, 24 parts, 25 parts, 30 parts, 35 parts, 40 parts and 45 parts of functional filler.
Preferably, the mass ratio of the polyolefin resin to the functional filler is 5-10: 1, more preferably 5 to 7: 1, more preferably 5: 1.
in the above, the preparation method of the functional filler ZnO/nano-silica SBA-15 can be seen in the following chemical reaction formula:
Zn2++2OH—═Zn(OH)2↓
Zn(OH)2↓+2OH—═Zn(OH)4 2—
Zn(OH)4 2—═Zn2++4OH—(Dissolution)
Zn2++2OH—═ZnO+H2O(Nucleation)
in the above, in the method for preparing the functional filler, the volume ratio of ethanol to water in the NaOH ethanol aqueous solution in the step (2) is preferably 1: 1; in this step, the reaction temperature is 80 to 120 ℃, preferably 80 to 100 ℃, more preferably 80 to 90 ℃, and may be 82 ℃, 85 ℃, 88 ℃, 95 ℃, 98 ℃, 105 ℃, 110 ℃, 115 ℃ or 118 ℃. The reaction time is at least 5h, and can be longer, for example, the reaction time is 8h, 10h, 12h or 16 h.
In the technical scheme, the compatilizer is selected from one or more of PE-g-MAH, PP-g-MAH and POE-g-MAH.
In the technical scheme, the additive is an antioxidant and/or a light stabilizer.
In the above technical scheme, the silane coupling agent is selected from one or more of vinyl silane coupling agent, triacetoxy vinyl silane, vinyl trimethoxy silane, vinyl tri (2-methoxyethoxy) silane, and vinyl triethoxy silane.
In the technical scheme, the zinc oxide in the functional filler is in a nano rod shape.
Preferably, in the step (1), the atomic ratio of Si/Zn is 1: 5-20. More preferably 1: 5-10. More preferably 1: 6-8.
The invention also discloses a preparation method of the antistatic heat-conducting polyolefin composition, which comprises the following steps:
(1) preparing a functional filler: weighing nanometer silicon oxide SBA-15 and Zn (CH)3COO)2·2H2O, and the atomic ratio of Si/Zn is 1:1 to 30;
reacting the above Zn (CH)3COO)2·2H2Putting O into NaOH ethanol water solution, adding a silane coupling agent and nano silicon oxide SBA-15 after uniformly stirring, putting into a high-pressure kettle after fully stirring, and reacting for at least 5 hours at 80-120 ℃; after the reaction is finished, filtering, washing and drying to obtain the functional filler;
(2) putting the components into a stirrer according to the proportion of claim 1, and stirring to mix uniformly; and putting the uniformly mixed materials into a double-screw extruder preheated to 160-210 ℃, and cooling, granulating and drying the extruded melt to obtain the polyolefin composition.
Preferably, in the step (2), the stirring speed is 100-150 r/min; the stirring time is not less than 20min, the diameter of a screw of the double-screw extruder is 40-70 mm, and the length-diameter ratio is 30-50.
Preferably, the zinc oxide in the functional filler is in a shape of a nano rod.
The invention also discloses an insulating heat-conducting transparent film prepared from the polyolefin composition.
The invention also discloses an insulating heat-conducting transparent plate prepared from the polyolefin composition.
The working mechanism of the invention is as follows: the polypropylene has excellent electrical insulation, low water absorption and low water vapor transmission rate, but has poor cold resistance and is easy to brittle failure at low temperature; the nano silicon oxide SBA-15 is a pipeline-shaped nano silicon oxide material, the cross section of the nano silicon oxide material is honeycomb-shaped, the porous channel is rich, the specific surface area is large, and the heat conductivity is good; the invention follows the mechanism of heat conduction path, the pipe-shaped nano silicon oxide SBA-15 is easy to form a heat conduction channel in resin, the heat conduction performance of the material can be greatly improved by adding a small amount of the nano silicon oxide SBA-15, the problem of filler agglomeration is avoided, and the cost is saved; on the other hand, the pipeline-shaped porous structure of the SBA-15 enables the pipeline-shaped porous structure to have a large specific surface area, the developed pores enable the pipeline-shaped porous structure to have strong adsorption capacity, the Zn source is adsorbed in the pore channels of the SBA-15 to be decomposed and recrystallized, the rod-shaped nano zinc oxide is generated on the pipeline-shaped nano zinc oxide, isolated and twin silicon hydroxyl groups on the surface of the pipeline-shaped nano zinc oxide have high chemical reaction activity, and the silane coupling agent is added to react with the silicon hydroxyl groups on the surface of the material to form Si-O bonds, so that the functional filler has good dispersibility and cohesiveness in the polyolefin resin, and finally, the functions of antistatic property and high thermal conductivity can be realized simultaneously after a small amount.
Due to the application of the technical scheme, compared with the prior art, the invention has the following advantages:
1. the invention develops a novel polyolefin composition, combines the excellent electrical insulation property, low water absorption rate and low water vapor transmission rate of polyolefin, simultaneously realizes the functions of antistatic property and high thermal conductivity by adding a small amount of functional filler, has lower cost and obtains remarkable effect;
2. according to the invention, the nano-silicon oxide SBA-15 is modified by adopting a one-step method to obtain the ZnO/nano-silicon oxide SBA-15 functional filler, the preparation method is simple and convenient, and the cost is low; the obtained functional filler has excellent dispersibility in PP, and can simultaneously have the functions of antistatic property and high thermal conductivity by adding a small amount of the functional filler;
3. in the polyolefin composition, the mass ratio of the polyolefin resin to the functional filler is 5-10: 1; therefore, the addition amount of the functional filler is very small, which is mainly benefited by the excellent dispersibility and cohesiveness of the functional filler, and the small addition amount not only can realize the functions of antistatic property and high thermal conductivity of the material, but also enables the material to have better light transmission performance and mechanical performance;
4. the preparation method is simple and easy to implement, has low cost and is suitable for popularization and application.
Drawings
FIG. 1 is a TEM image of the functional filler in the first embodiment.
Detailed Description
Example one
A preparation method of an antistatic heat-conducting polyolefin composition comprises the following steps:
(1) taking a certain amount of SBA-15(XFF01, Nanjing pioneer nanometer) and Zn (CH)3COO)2·2H2O, making the atomic ratio of Si/Zn to be 5, adding Zn (CH) into 0.2mol/L NaOH ethanol water (ethanol and deionized water volume ratio is 1:1)3COO)2·2H2O, adding a silane coupling agent and SBA-15 after uniformly stirring, placing the mixture in an autoclave for reaction for 10 hours at the temperature of 80 ℃ after fully stirring for 2 hours, filtering and washing the reaction product, and drying the reaction product at the temperature of 50 ℃ to obtain ZnO/SBA-15 nano functional filler with good dispersibility;
(2) weighing 10g of the ZnO/SBA-15 nano functional filler, 90g of homo-polypropylene, 10g of linear low-density polyethylene, 0.2g of compatilizer PP-g-MAH and 0.1g of antioxidant DNP, adding the materials into a stirrer, stirring for 20min, then putting the mixture into a hopper of an extruder, controlling the temperature of each section of the extruder to be between 160 ℃ and 210 ℃, controlling the rotation speed of a screw to be 150r/min, cooling and molding a melt in a water tank after extrusion, drawing the melt into a granulator, granulating and drying. A polyolefin composition is obtained.
Example two
A preparation method of an antistatic heat-conducting polyolefin composition comprises the following steps:
the process for preparing ZnO/SBA-15 nanometer functional filler is the same as that of the first embodiment;
weighing 15g of ZnO/SBA-15 nano functional filler, 90g of homo-polypropylene, 10g of linear low-density polyethylene, 0.2g of compatilizer PP-g-MAH and 0.1g of antioxidant DNP, adding the materials into a stirrer, stirring for 20min, then putting the mixture into a hopper of an extruder, controlling the temperature of each section of the extruder to be between 160 and 210 ℃, controlling the rotating speed of a screw to be 150r/min, cooling and molding a melt in a water tank after extrusion, drawing the melt into a granulator, granulating and drying. A polyolefin composition is obtained.
EXAMPLE III
A preparation method of an antistatic heat-conducting polyolefin composition comprises the following steps:
the process for preparing ZnO/SBA-15 nanometer functional filler is the same as that of the first embodiment;
weighing 20g of ZnO/SBA-15, 90g of homo-polypropylene, 10g of linear low-density polyethylene, 0.2g of compatilizer PP-g-MAH and 0.1g of antioxidant DNP, adding the materials into a stirrer, stirring for 20min, then putting the mixture into a hopper of an extruder, controlling the temperature of each section of the extruder to be between 160 and 210 ℃, controlling the rotation speed of a screw to be 150r/min, cooling and molding a melt in a water tank after extrusion, drawing the melt into a granulator, granulating and drying. A polyolefin composition is obtained.
Example four
A preparation method of an antistatic heat-conducting polyolefin composition comprises the following steps:
the process for preparing ZnO/SBA-15 nanometer functional filler is the same as that of the first embodiment;
weighing 30g of ZnO/SBA-15, 90g of homopolymerized polypropylene, 10g of linear low-density polyethylene, 0.2g of compatilizer PP-g-MAH and 0.1g of antioxidant DNP, adding the materials into a stirrer, stirring for 20min, then putting the mixture into a hopper of an extruder, controlling the temperature of each section of the extruder to be between 160 and 210 ℃, controlling the rotation speed of a screw to be 150r/min, cooling and molding a melt in a water tank after extrusion, drawing the melt into a granulator, granulating and drying. A polyolefin composition is obtained.
Comparative example 1
Weighing 20g of SBA-15(XFF01, Nanjing pioneer nanometer Limited company) treated by silane coupling agent, 90g of homopolymerized polypropylene, 10g of linear low-density polyethylene, 0.2g of compatilizer PP-g-MAH and 0.1g of antioxidant DNP, adding the mixture into a stirrer, stirring for 20min, then putting the mixture into a hopper of an extruder, controlling the temperature of each section of the extruder to be between 160 and 210 ℃, controlling the rotating speed of a screw to be 150r/min, cooling and molding a melt in a water tank after extrusion, drawing the melt into a granulator, granulating and drying. A polyolefin composition is obtained.
Comparative example No. two
Weighing 20g of ZnO (DK-ZnO-15, Beijing Germany island gold technology Co., Ltd.) treated by silane coupling agent, 90g of homopolymerized polypropylene, 10g of linear low density polyethylene, 0.2g of compatilizer PP-g-MAH and 0.1g of antioxidant DNP, adding into a stirrer, stirring for 20min, then putting the mixture into a hopper of an extruder, controlling the temperature of each section of the extruder between 160 and 210 ℃, controlling the rotating speed of a screw at 150r/min, cooling and molding a melt in a water tank after extrusion, drawing into a granulator, granulating and drying. A polyolefin composition is obtained.
Comparative example No. three
Weighing 20g of ZnO (DK-ZnO-15, Beijing German island gold technology Co., Ltd.) and SBA-15(XFF01, Nanjing pioneer nanometer Co., Ltd.), simply and physically blending, wherein the atomic ratio of Si/Zn is 5, adding the treated mixture, 90g of homopolymerized polypropylene, 10g of linear low density polyethylene, 0.2g of compatilizer PP-g-MAH and 0.1g of antioxidant DNP into a stirrer, stirring for 20min, then putting the mixture into a hopper of an extruder, cooling and molding a melt in a water tank after extrusion at the temperature of 160-210 ℃, rotating the screw at the speed of 150r/min, and drawing the melt into a granulator for granulation and drying. A polyolefin composition is obtained.
The master batches prepared in the above examples and comparative examples were respectively added to polypropylene to prepare films, wherein the mass content of the master batch was 30%, and the thickness of the film was 0.2 mm.
The films were tested for surface resistivity (GB/T1410-89), thermal conductivity (HotDisk 2500S type thermophysical property tester), light transmission (GB2410-1989), tensile strength (GB/T1040-1992), notched Izod impact strength (GB/T1843-1996), respectively. The properties of the BOPP films produced are detailed in the following table:
in the above table: s1 to S4 represent examples one to four, and D1 to D3 represent comparative examples one to three.
From the above table, it can be seen from the comparison of the properties of the first to the fourth examples that the change of the addition amount of the functional filler in the resin material does not greatly affect the mechanical properties such as the rigidity and impact strength of the film, but has a certain effect on the surface resistivity and thermal conductivity of the film. The surface resistivities of the four embodiments are all less than 1012Omega, which shows that the product of the invention can meet the requirement of antistatic performance, and when the addition amount is 20g, the surface resistivity of the film is minimum, and is 5.6x107The heat conductivity coefficient is 15.2W/m.K, the composite material has the most excellent antistatic performance and heat conductivity, the light transmittance is 96 percent, the tensile strength is 22MPa, and the notch impact strength is 29KJ/m2This shows that when the amount of the ZnO/SBA-15 functional filler added to the polyolefin composition is 20g and the amount of the master batch added to the polypropylene is 30%, the obtained film has the best performance, and is a good antistatic heat-conducting polyolefin material.
Compared with the first to third comparative examples, the material prepared by the invention has antistatic property and conductive property, good dispersibility also enables the material to have better light transmission property and mechanical property, and the surface resistivity of the first and third comparative examples is too large (more than 10) compared with the surface resistivity of the first and third comparative examples, namely more than 1012Omega) and cannot meet the requirement of antistatic performance, while the thermal conductivity of the comparative example is only 8.2W/mK and cannot meet the requirement of thermal conductivity.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (10)
1. An antistatic heat-conductive polyolefin composition characterized by: the adhesive mainly comprises the following components in parts by mass:
wherein the mass ratio of the polyolefin resin to the functional filler is 5-10: 1;
wherein, the polyolefin resin is selected from one or more of polyethylene and polypropylene; the functional filler is ZnO/nano silicon oxide SBA-15, and the preparation method comprises the following steps:
(1) weighing nanometer silicon oxide SBA-15 and Zn (CH)3COO)2·2H2O, and the atomic ratio of Si/Zn is 1:1 to 30;
(2) reacting the above Zn (CH)3COO)2·2H2Adding O into NaOH ethanol water solution, uniformly stirring (the volume ratio of ethanol to water is 1:1), adding a silane coupling agent and nano silicon oxide SBA-15, fully stirring, placing in a high-pressure kettle, and reacting at 80-120 ℃ for at least 5 hours;
(3) and after the reaction is finished, filtering, washing and drying to obtain the functional filler.
2. The antistatic, thermally conductive polyolefin composition according to claim 1, characterized in that: the compatilizer is selected from one or more of PE-g-MAH, PP-g-MAH and POE-g-MAH.
3. The antistatic, thermally conductive polyolefin composition according to claim 1, characterized in that: the additive is an antioxidant and/or a light stabilizer.
4. The antistatic, thermally conductive polyolefin composition according to claim 1, characterized in that: the silane coupling agent is selected from one or more of vinyl silane coupling agent, triacetoxy vinyl silane, vinyl trimethoxy silane, vinyl tri (2-methoxyethoxy) silane and vinyl triethoxy silane.
5. The antistatic, thermally conductive polyolefin composition according to claim 1, characterized in that: the zinc oxide in the functional filler is in a nano rod shape.
6. The antistatic, thermally conductive polyolefin composition according to claim 1, characterized in that: in the step (1), the atomic ratio of Si/Zn is 1: 5-20.
7. The preparation method of the antistatic heat-conducting polyolefin composition is characterized by comprising the following steps:
(1) preparing a functional filler: weighing nanometer silicon oxide SBA-15 and Zn (CH)3COO)2·2H2O, and the atomic ratio of Si/Zn is 1:1 to 30;
reacting the above Zn (CH)3COO)2·2H2Putting O into NaOH ethanol water solution, adding a silane coupling agent and nano silicon oxide SBA-15 after uniformly stirring, putting into a high-pressure kettle after fully stirring, and reacting for at least 5 hours at 80-120 ℃; after the reaction is finished, filtering, washing and drying to obtain the functional filler;
(2) putting the components into a stirrer according to the proportion of claim 1, and stirring to mix uniformly; and putting the uniformly mixed materials into a double-screw extruder preheated to 160-210 ℃, and cooling, granulating and drying the extruded melt to obtain the polyolefin composition.
8. The method of claim 7, wherein: the zinc oxide in the functional filler is in a nano rod shape.
9. An insulating, thermally conductive, transparent film prepared using the polyolefin composition of any of claims 1 to 6.
10. An insulating and heat-conducting transparent sheet prepared from the polyolefin composition of any one of claims 1 to 6.
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Cited By (3)
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|---|---|---|---|---|
| CN112646275A (en) * | 2020-12-23 | 2021-04-13 | 苏州度辰新材料有限公司 | Conductive polyolefin master batch and preparation method thereof |
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| CN113512256A (en) * | 2021-08-18 | 2021-10-19 | 苏州度辰新材料有限公司 | Antistatic polyolefin master batch and preparation method thereof |
| CN114591566A (en) * | 2022-01-27 | 2022-06-07 | 武汉金发科技有限公司 | Polyolefin composition and preparation method and application thereof |
| CN114591566B (en) * | 2022-01-27 | 2023-09-19 | 武汉金发科技有限公司 | Polyolefin composition and preparation method and application thereof |
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