CN116265523A - High-temperature-resistant anti-interference lightweight elastomer material and preparation method thereof - Google Patents

High-temperature-resistant anti-interference lightweight elastomer material and preparation method thereof Download PDF

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CN116265523A
CN116265523A CN202310096450.4A CN202310096450A CN116265523A CN 116265523 A CN116265523 A CN 116265523A CN 202310096450 A CN202310096450 A CN 202310096450A CN 116265523 A CN116265523 A CN 116265523A
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interference
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钟荣栋
刘悦
李同兵
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Guangdong Antopu Polymer Technology Co ltd
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    • C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
    • C08J9/04—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
    • C08J9/06—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a chemical blowing agent
    • C08J9/10—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a chemical blowing agent developing nitrogen, the blowing agent being a compound containing a nitrogen-to-nitrogen bond
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    • C08J2327/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers
    • C08J2327/02—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment
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Abstract

The invention provides a high-temperature-resistant anti-interference lightweight elastomer material, which comprises the following components in parts by weight: 50-65 parts of polytetrafluoroethylene, 10-15 parts of low dielectric constant glass fiber, 3-5 parts of foaming agent, 0.5-2 parts of antioxidant, 2-4 parts of stabilizer, 3-6 parts of coupling agent, 0.5-2 parts of surfactant, 6-12 parts of antistatic master batch and 6-10 parts of hollow filler. The coupling agent is added to promote the glass fiber reinforced polytetrafluoroethylene with low dielectric constant, so that the prepared elastomer has excellent tensile strength and wear resistance, and can improve the cold flow resistance of the polytetrafluoroethylene; through the specific proportion of the foaming agent and the hollow filler, the synergistic effect of the foaming agent and the hollow filler can ensure the impact strength of the elastomer while realizing the weight reduction of the elastomer; in addition, the antistatic master batch is added, so that the phenomenon that polytetrafluoroethylene is easy to generate static electricity can be weakened, the electromagnetic shielding effect and the anti-interference effect are good, and the antistatic master batch can be widely applied to the preparation of high-frequency transmission cable materials.

Description

High-temperature-resistant anti-interference lightweight elastomer material and preparation method thereof
Technical Field
The invention relates to the technical field of high polymer materials, in particular to a high-temperature-resistant anti-interference lightweight elastomer material and a preparation method thereof.
Background
The high-frequency transmission technology is one of key technologies of 5G wireless communication, can effectively increase the availability of frequency band resources, and enhances the technical requirements of the 5G wireless communication technology on network development. To achieve high frequency transmission, a low dielectric constant, low dielectric loss material must be used, and Polytetrafluoroethylene (PTFE) has to be widely used as the material with the lowest dielectric constant in the current organic materials. In addition, the polytetrafluoroethylene has outstanding comprehensive performance compared with other chemical polymer materials, has the reputation of 'plastic king', has excellent chemical stability, heat resistance, cold resistance, chemical corrosion resistance, outstanding insulation, hydrophobicity, good lubricating flame retardance, atmospheric aging resistance, high-low temperature adaptability and the like, but has poor antistatic performance, and can generate static electricity in the high-frequency transmission process to cause interference to transmission signals.
One of the important global high-performance high-molecular polymer industrialization targets at present is to take the weight reduction of materials as a main means, and to reduce the consumption of social resources, wherein the materials with physical properties meeting the requirements of transportation packaging are used as few as possible, and obviously, the density reduction of the high-molecular materials is the simplest choice. The use of some of the blowing agents commonly used in the art can result in a decrease in the density of the material as well as a decrease in its strength, or in a poor and non-uniform foam cell morphology.
Therefore, in order to meet the requirements of anti-interference and light weight of the high-frequency transmission cable, an elastomer taking polytetrafluoroethylene as a main component is researched and has potential application value.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a high-temperature-resistant anti-interference lightweight elastomer material and a preparation method thereof, and the prepared elastomer has the characteristics of excellent tensile strength, high temperature resistance, wear resistance and light weight, has good signal shielding effect and anti-interference effect, and can be widely applied to the preparation of high-frequency transmission cable materials.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
the invention provides a high-temperature-resistant anti-interference lightweight elastomer material, which comprises the following components in parts by weight:
50-65 parts of polytetrafluoroethylene, 10-15 parts of low dielectric constant glass fiber, 3-5 parts of foaming agent, 0.5-2 parts of antioxidant, 2-4 parts of stabilizer, 3-6 parts of coupling agent, 0.5-2 parts of surfactant, 6-12 parts of antistatic master batch and 6-10 parts of hollow filler.
Although polytetrafluoroethylene is excellent in material properties and has a certain stability, it has a relative disadvantage that polytetrafluoroethylene has cold fluidity, that is, plastic deformation, that is, creep, which occurs under continuous load for a long time, which brings a certain limit to its application, and in order to improve its drawbacks, the present invention adopts glass fiber as a filler to improve its properties, and in order to realize high-frequency transmission application, adopts low dielectric constant glass fiber having a dielectric constant of not more than 4.5.
In some preferred embodiments, the low dielectric constant glass fiber has a dielectric constant of 4.4, selected from the Shandong Taishan glass fiber Inc.
In some preferred embodiments, the polytetrafluoroethylene is selected from the group consisting of large Jin Fuhua company (china) limited.
In some preferred embodiments, the blowing agent is a 15% by mass zno modified AC blowing agent having a particle size of 5 to 10 μm, the blowing agent to hollow filler mass ratio of 1:2.
the 15% ZnO modified AC foaming agent is prepared by mixing an activating agent ZnO and an AC foaming agent purchased from Duba chemical company, and the specific preparation method comprises the following steps: mixing the activating agent ZnO and the AC foaming agent in a mixer at a high speed according to a proportion, putting the mixture into a double-screw extruder for extrusion, wherein the temperature is 138 ℃, and the rotating speed of a main screw is 120r/min.
The conventional polymer foaming method includes a physical foaming method, which means that when a polymer is heated to a molten state, a physical foaming agent provides a gas for foaming the polymer, such as low boiling point liquid petroleum ether, water, butane, etc., through physical change, and the mixture is foamed under a certain pressure and temperature, and a chemical foaming method. The chemical foaming method makes the chemical foaming agent uniformly dispersed in the mixed polymer, under certain condition, the foaming agent releases gas through thermal degradation or chemical reaction, and the gas is fused into the composite material melt under high pressure, and overflows from the melt to form bubbles under the action of pressure drop, and finally the cooling and shaping are carried out.
In some preferred embodiments, the blowing agent is a 15% by mass ZnO modified AC blowing agent having a particle size of 5-10 μm and decomposing N by heat radiation in the polymer 2 The solubility in polytetrafluoroethylene is smaller, the dispersibility is better, the formed cells are good in morphology, small in diameter and uniform in distribution, and the foam walls of the cells generated by the prepared elastomer can be thicker by adopting the foaming agent, so that the impact strength is ensured while the density is reduced.
The addition of the antioxidant can optionally delay or inhibit the progress of the oxidation process of the polymer, age the tissue polymer and prolong the service life of the tissue polymer, and in some preferred embodiments, the antioxidant is a compound of phosphite esters and hindered phenol antioxidants, and the mass ratio of the phosphite esters to the hindered phenol antioxidants is (1.5-2): 1, the phosphite ester oxidant is preferably an antioxidant 168, and the hindered phenol antioxidant is preferably an antioxidant 1076, and the two antioxidants have synergistic effect, so that the ageing resistance of the prepared elastomer is effectively improved.
In some preferred embodiments, the stabilizer is calcium stearate and zinc stearate, and the mass ratio of the two is 1: (1-1.2).
The improved wettability between the fiber and the matrix can be achieved by treating the low dielectric glass fiber with a coupling agent, which in some preferred embodiments is a silane coupling agent or a titanate coupling agent, more preferably a silane coupling agent.
The silane coupling agent is one or more of vinyl triethoxysilane, vinyl triacetoxy silane, gamma-aminopropyl triethoxysilane and vinyl trimethoxy silane.
The silane coupling agent contains two different chemical functional groups, one end group is inorganic-philic, and the other end group is organic-philic. The inorganic end can be hydrolyzed to generate silanol, and the silanol is connected with the surface of the glass fiber with hydroxyl on the surface through hydrogen bonds; the organic end can generate stable covalent bonds with various organic functional groups, thereby playing a coupling effect. The silane coupling agent is prepared through hydrolysis of organic siloxane to produce silanol, reaction with hydroxyl radical on the surface of glass fiber to produce stable Si-0-Si bond structure. The use of the silane coupling agent reduces the surface free energy of the glass fiber, and the surface free energy of the fiber is an important parameter affecting the performances of infiltration, adsorption, adhesion and the like of the glass fiber, but the surface of the glass fiber generates active functional groups which are chemically bonded with the glass fiber, and the functional groups can be well physically or chemically bonded with matrix resin, so that the interface bonding strength of the fiber and the matrix in the material can be improved, the wear resistance and hardness of an elastomer can be improved, and the creep resistance and cold flow resistance of polytetrafluoroethylene are improved.
In some preferred embodiments, the surfactant is an anionic surfactant which is one or more of higher fatty acids and salts thereof, alkyl sulphates, alkyl sulphonates, alkyl phosphates, preferably sodium dodecyl sulphate.
In some preferred embodiments, the hollow filler is hollow glass beads, the particle size of the hollow glass beads is 50-60 μm, and the hollow glass beads with specific particle size are selected, so that the hollow filler has higher filling amount and more proper specific surface area, can effectively fill gaps in the elastomer, and increases fluidity; meanwhile, the foaming agent and the foaming agent are compounded in a specific proportion to generate a synergistic effect, so that the pore-forming rate of the elastomer can be improved, the density is reduced, and the weight of the elastomer is reduced.
In some preferred embodiments, the antistatic master batch is selected from the company of force-gathering limited, so that the surface resistance of polytetrafluoroethylene material can be reduced, the phenomenon that the polytetrafluoroethylene material is easy to generate static electricity is weakened, the electromagnetic shielding and antistatic interference effects are improved, and the accuracy and stability of the transmission signal are ensured.
The hollow glass microsphere is purchased from Shanghai electric International trade company, with the brand number of 5014, but is not limited to the present factory.
The invention also provides a preparation method of the high-temperature-resistant anti-interference lightweight elastomer material, which comprises the following steps:
(1) Placing polytetrafluoroethylene and a foaming agent into a reaction kettle, and uniformly mixing to obtain a premix;
(2) Adding a coupling agent, an antioxidant, a stabilizer, a hollow filler, a surfactant and antistatic master batches into the premix of the step (1), and continuously mixing to obtain a mixture;
(3) And (3) placing the mixture obtained in the step (2) in a parallel double-screw extruder, adding low-dielectric-constant glass fibers at the other side of the parallel double-screw extruder for melt extrusion, and granulating to obtain the high-temperature-resistant and anti-interference lightweight elastomer.
In some preferred embodiments, the mixing temperature in step (1) is 50-70 ℃ and the mixing time is 30-50 min; the mixing temperature in the step (2) is 75-85 ℃, and the mixing time is 40-60 min; the heating temperature of the parallel double-screw extruder is 280-360 ℃.
The beneficial effects are that: compared with the prior art, the invention has the following advantages:
(1) The low-dielectric-constant glass fiber is added, so that the size stability of the polytetrafluoroethylene can be enhanced, and the interface compatibility between the glass fiber and the polytetrafluoroethylene is promoted by the coupling agent, so that the prepared elastomer has excellent tensile strength and wear resistance, and the creep resistance and cold flow resistance of the polytetrafluoroethylene are improved.
(2) The invention adds 15% ZnO modified AC foaming agent, the formed foam has good shape, small diameter and even distribution, and the impact strength can be ensured while the density is reduced; meanwhile, the hollow filler with specific particle size is added, so that on one hand, gaps in the elastomer can be filled, the fluidity is increased, on the other hand, the hollow filler can generate a synergistic effect with the foaming agent, the pore-forming rate of the elastomer is improved, the density is reduced, and the aim of lightening the elastomer is fulfilled.
(3) The antistatic master batch is added, so that the phenomenon that polytetrafluoroethylene is easy to generate static electricity can be weakened, the electromagnetic shielding and antistatic interference efficiency under the frequency range of 5kHz is improved, and the accuracy and stability of a transmission signal are ensured.
(4) The prepared elastomer can be applied to the field of high-frequency transmission cable materials and has the advantages of light weight, low cost, social resource consumption reduction and the like.
Detailed Description
Examples
Example 1
In one aspect, the embodiment provides a high-temperature-resistant and anti-interference lightweight elastomer material, which comprises the following components in parts by weight: 58 parts of polytetrafluoroethylene, 15 parts of low dielectric constant glass fiber, 4 parts of 15% ZnO modified AC foaming agent, 168 parts of antioxidant, 1076.5 parts of antioxidant, 1.5 parts of calcium stearate, 1.5 parts of zinc stearate, 5 parts of gamma-aminopropyl triethoxysilane, 0.5 part of sodium dodecyl sulfate, 8 parts of antistatic master batch and 8 parts of hollow glass microsphere.
The 15% ZnO modified AC foaming agent used in the embodiment is prepared by mixing an activating agent ZnO and an AC foaming agent purchased from Duba chemical company, and the specific preparation method is as follows: mixing the activating agent ZnO and the AC foaming agent in a mixer at a high speed according to a proportion, putting the mixture into a double-screw extruder for extrusion, wherein the temperature is 138 ℃, and the rotating speed of a main screw is 120r/min.
The polytetrafluoroethylene is selected from the group consisting of large Jin Fuhua company (china);
the low dielectric constant glass fiber has a dielectric constant of 4.4, purchased from mountain taishan glass fiber limited;
the antistatic master batch is purchased from the company of force focusing limited;
the hollow glass beads are purchased from Shanghai electric International trade company, and the brand number is 5014.
The invention also provides a preparation method of the high-temperature-resistant anti-interference lightweight elastomer material, which comprises the following steps:
(1) Placing polytetrafluoroethylene and 15% by mass of ZnO modified AC foaming agent into a reaction kettle to react for 45min at 68 ℃ to obtain a uniformly mixed premix;
(2) Adding an antioxidant 168, an antioxidant 1076, zinc stearate, calcium stearate, hollow glass beads, gamma-aminopropyl triethoxysilane, sodium dodecyl sulfate and antistatic master batch into the premix of the step (1), and reacting for 55min at 80 ℃ to obtain a mixture;
(3) And (3) placing the mixture obtained in the step (2) in a parallel double-screw extruder, adding low-dielectric-constant glass fibers at the other side of the parallel double-screw extruder, carrying out melt extrusion at 320 ℃, and granulating to obtain the high-temperature-resistant and anti-interference lightweight elastomer.
Example 2
In one aspect, the embodiment provides a high-temperature-resistant and anti-interference lightweight elastomer material, which comprises the following components in parts by weight: 63 parts of polytetrafluoroethylene, 10 parts of low dielectric constant glass fiber, 4 parts of 15% ZnO modified AC foaming agent, 168 parts of antioxidant, 1076.5 parts of antioxidant, 1 part of calcium stearate, 1 part of zinc stearate, 4 parts of vinyl trimethoxy silane, 0.5 part of sodium dodecyl sulfate, 7 parts of antistatic master batch and 8 parts of hollow glass microsphere.
The preparation method of the 15% ZnO modified AC foaming agent is the same as that of the example 1;
the polytetrafluoroethylene is selected from the group consisting of large Jin Fuhua company (china);
the low dielectric constant glass fiber has a dielectric constant of 4.4, purchased from mountain taishan glass fiber limited;
the antistatic master batch is purchased from the company of force focusing limited;
the hollow glass beads are purchased from Shanghai electric International trade company, and the brand number is 5014.
The invention also provides a preparation method of the high-temperature-resistant anti-interference lightweight elastomer material, which comprises the following steps:
(1) Placing polytetrafluoroethylene and 15% by mass of ZnO modified AC foaming agent into a reaction kettle to react for 50min at 55 ℃ to obtain a uniformly mixed premix;
(2) Adding an antioxidant 168, an antioxidant 1076, zinc stearate, calcium stearate, hollow glass beads, vinyl trimethoxy silane, sodium dodecyl sulfate and antistatic master batch into the premix of the step (1), and reacting at 85 ℃ for 40min to obtain a mixture;
(3) And (3) placing the mixture obtained in the step (2) in a parallel double-screw extruder, adding low-dielectric-constant glass fibers at the other side of the parallel double-screw extruder, carrying out melt extrusion at 290 ℃, and granulating to obtain the high-temperature-resistant and anti-interference lightweight elastomer.
Example 3
In one aspect, the embodiment provides a high-temperature-resistant and anti-interference lightweight elastomer material, which comprises the following components in parts by weight: 52 parts of polytetrafluoroethylene, 15 parts of low dielectric constant glass fiber, 4.5 parts of 15% ZnO modified AC foaming agent, 168 parts of antioxidant, 1076.5 parts of antioxidant, 1 part of calcium stearate, 1.2 parts of zinc stearate, 5 parts of vinyl triethoxysilane, 0.8 part of sodium dodecyl sulfate, 10 parts of antistatic master batch and 9 parts of hollow glass microsphere.
The preparation method of the 15% ZnO modified AC foaming agent is the same as that of the example 1;
the polytetrafluoroethylene was purchased from Jin Fuhua company (china) limited;
the low dielectric constant glass fiber has a dielectric constant of 4.4, purchased from mountain taishan glass fiber limited;
the antistatic master batch is purchased from the company of force focusing limited;
the hollow glass beads are purchased from Shanghai electric International trade company, and the brand number is 5014.
The invention also provides a preparation method of the high-temperature-resistant anti-interference lightweight elastomer material, which comprises the following steps:
(1) Placing polytetrafluoroethylene and 15% by mass of ZnO modified AC foaming agent into a reaction kettle to react for 45min at 65 ℃ to obtain a uniformly mixed premix;
(2) Adding an antioxidant 168, an antioxidant 1076, zinc stearate, calcium stearate, hollow glass beads, vinyl triethoxysilane, sodium dodecyl sulfate and antistatic master batch into the premix of the step (1), and reacting at 80 ℃ for 50min to obtain a mixture;
(3) And (3) placing the mixture obtained in the step (2) in a parallel double-screw extruder, adding low-dielectric-constant glass fibers at the other side of the parallel double-screw extruder, carrying out melt extrusion at 350 ℃, and granulating to obtain the high-temperature-resistant and anti-interference lightweight elastomer.
Comparative example 1
The comparative example 1 provides a high temperature resistant and anti-interference lightweight elastomer material and a preparation method thereof, which are different from the example 1 in that the glass fiber used is a common glass fiber with a dielectric constant of 6.3, and is purchased from Shandong Taishan glass fiber Co.
Comparative example 2
The comparative example 2 provides a high temperature resistant and anti-interference lightweight elastomer material and a preparation method thereof, and the difference between the high temperature resistant and anti-interference lightweight elastomer material and the preparation method is that the mass ratio of the foaming agent to the hollow glass beads is 1:1.
comparative example 3
The comparative example 3 provides a high temperature resistant and interference resistant lightweight elastomer material and a preparation method thereof, which is different from the example 1 in that no antistatic masterbatch is added.
The elastomeric materials prepared in the above examples and comparative examples were subjected to the following performance tests:
(1) Tensile strength: the stretching rate is 50mm/min according to GB/T1040-2006 standard test;
(2) Elongation at break: elongation at break was measured according to GB/T1040-1992 standard;
(3) Impact strength: the thickness of the sample is 4mm according to GB/T1843-2008 standard test;
(4) Dielectric constant: according to GB/T5597-19991 standard test, the test frequency is 1GHz;
(5) Wear resistance: carrying out wear resistance test on the obtained thermoplastic elastomer by adopting a reciprocating friction and wear testing machine, wherein the load is 100g, the reciprocating sliding frequency is 20Hz, the sliding length is 5mm, and the friction time is 20min;
the wear resistance of the material can be reflected by the measured average friction coefficient, and the smaller the average friction coefficient is, the better the wear resistance is.
(6) Electromagnetic shielding effectiveness: the flange coaxial test device is adopted, the frequency range is 5kHz, the characteristic impedance is 50Ω, the voltage standing wave ratio is <1.2, and the transmission loss is <1dB.
The test results are shown in Table 1.
TABLE 1 Performance test results
Figure BDA0004071813820000071
Figure BDA0004071813820000081
As shown by the performance test results in Table 1, the lightweight elastomer prepared by the invention has excellent tensile strength and impact strength, high wear resistance, low dielectric constant and good battery shielding effectiveness, so that low loss and effective anti-interference are realized in the high-frequency transmission process, and the stability of transmission signals is ensured.

Claims (10)

1. The high-temperature-resistant anti-interference lightweight elastomer material is characterized by comprising the following raw materials in parts by weight:
50-65 parts of polytetrafluoroethylene, 10-15 parts of low dielectric constant glass fiber, 3-5 parts of foaming agent, 0.5-2 parts of antioxidant, 2-4 parts of stabilizer, 3-6 parts of coupling agent, 0.5-2 parts of surfactant, 6-12 parts of antistatic master batch and 6-10 parts of hollow filler.
2. The high temperature resistant and anti-interference lightweight elastomer material according to claim 1, wherein the foaming agent is 15% by mass of ZnO modified AC foaming agent.
3. The high temperature resistant and anti-interference lightweight elastomer material according to claim 2, wherein the particle size of the AC foaming agent is 5-10 μm, and the mass ratio of the foaming agent to the hollow filler is 1:2.
4. the high-temperature-resistant anti-interference lightweight elastomer material as claimed in claim 1, wherein the antioxidant is a compound of phosphite esters and hindered phenols, and the mass ratio of the phosphite esters to the hindered phenols is (1.5-2): 1.
5. the high-temperature-resistant anti-interference lightweight elastomer material as claimed in claim 1, wherein the stabilizer is calcium stearate and zinc stearate, and the mass ratio of the calcium stearate to the zinc stearate is 1: (1-1.2).
6. The high temperature resistant and interference resistant lightweight elastomeric material of claim 1, wherein said coupling agent is a silane coupling agent or a titanate coupling agent.
7. The high temperature resistant, tamper resistant, lightweight elastomeric material of claim 1, wherein said surfactant is an anionic surfactant.
8. The high-temperature-resistant anti-interference lightweight elastomer material as claimed in claim 2, wherein the hollow filler is hollow glass beads, and the particle size of the hollow glass beads is 50-60 μm.
9. A method for preparing a high temperature resistant and interference resistant lightweight elastomeric material according to any one of claims 1 to 8, comprising the steps of:
(1) Placing polytetrafluoroethylene and a foaming agent into a reaction kettle, and uniformly mixing to obtain a premix;
(2) Adding a coupling agent, an antioxidant, a stabilizer, a hollow filler, a surfactant and antistatic master batches into the premix of the step (1), and continuously mixing to obtain a mixture;
(3) And (3) placing the mixture obtained in the step (2) in a parallel double-screw extruder, adding low-dielectric-constant glass fibers at the other side of the parallel double-screw extruder for melt extrusion, and granulating to obtain the high-temperature-resistant and anti-interference lightweight elastomer.
10. The method for preparing the high-temperature-resistant and anti-interference lightweight elastomer material according to claim 9, wherein the mixing temperature in the step (1) is 50-70 ℃ and the mixing time is 30-50 min; the mixing temperature in the step (2) is 75-85 ℃, and the mixing time is 40-60 min; the heating temperature of the parallel double-screw extruder is 280-360 ℃.
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