CN114573953A - PDCPD material for 5G base station housing and preparation method thereof - Google Patents

PDCPD material for 5G base station housing and preparation method thereof Download PDF

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CN114573953A
CN114573953A CN202111102873.XA CN202111102873A CN114573953A CN 114573953 A CN114573953 A CN 114573953A CN 202111102873 A CN202111102873 A CN 202111102873A CN 114573953 A CN114573953 A CN 114573953A
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base station
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张玉清
刘扬
徐国峰
陈虎斌
张履军
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Changzhou Jude New Material Co ltd
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    • C08G61/00Macromolecular compounds obtained by reactions forming a carbon-to-carbon link in the main chain of the macromolecule
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    • C08G61/04Macromolecular compounds containing only carbon atoms in the main chain of the macromolecule, e.g. polyxylylenes only aliphatic carbon atoms
    • C08G61/06Macromolecular compounds containing only carbon atoms in the main chain of the macromolecule, e.g. polyxylylenes only aliphatic carbon atoms prepared by ring-opening of carbocyclic compounds
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    • C08G2261/00Macromolecular compounds obtained by reactions forming a carbon-to-carbon link in the main chain of the macromolecule
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Abstract

The invention discloses a PDCPD material for a 5G base station housing and a preparation method thereof, wherein the material comprises a component A and a component B; the component A comprises the following raw materials in parts by weight: 40-60 parts of dicyclopentadiene, 0.1-0.15 part of Grubbs first-generation catalyst and 15-25 parts of wave-transmitting particles; the component B comprises the following raw materials in parts by weight: 40-60 parts of dicyclopentadiene, 2-8 parts of antimony trioxide, 3-10 parts of aluminum hydroxide, 0.1-0.15 part of tungsten hexachloride and 5-10 parts of light aging resistant agent; f atoms are introduced into the wave-transmitting particles to reduce the density of the intermediate 3, and two trifluoromethyl groups on the bisphenol AF prevent the molecules from being stacked and increase the free volume of the particles, so that the dielectric coefficient of the material is reduced, the light-resistant aging agent can convert light energy into heat energy to be released, and meanwhile, the molecules of the light-resistant aging agent are in a macromolecular latticed structure, so that the precipitation and volatilization caused by long-time use are effectively avoided.

Description

PDCPD material for 5G base station housing and preparation method thereof
Technical Field
The invention relates to the technical field of polymer material preparation, in particular to a PDCPD material for a 5G base station housing and a preparation method thereof.
Background
In the information age of today, various electronic appliances are integrated into various fields of production and life, and wireless signals used by the electronic appliances are provided by base station communication equipment which is usually built outdoors, so that a protective shell needs to be provided for the base station communication equipment;
however, the existing base station housing is mostly prepared from polyimide composite materials, the traditional polyimide has a large dielectric constant, 4G signal waves can well penetrate through the polyimide, but 5G signal waves cannot penetrate through the polyimide, so that 5G signal transmission is poor, the base station housing is located outdoors, the base station housing is illuminated for a long time, and then high molecules of the base station housing are subjected to light aging, and normal use is affected.
Disclosure of Invention
The invention aims to provide a PDCPD material for a 5G base station housing and a preparation method thereof, which solve the problems that the base station housing at the present stage influences 5G signal transmission and the base station housing can not normally protect a base station after long-time use through wave-transparent particles and a light-resistant aging agent.
The purpose of the invention can be realized by the following technical scheme:
the PDCPD material for the 5G base station housing comprises a component A and a component B;
the component A comprises the following raw materials in parts by weight: 40-60 parts of dicyclopentadiene, 0.1-0.15 part of Grubbs first-generation catalyst and 15-25 parts of wave-transmitting particles;
the component B comprises the following raw materials in parts by weight: 40-60 parts of dicyclopentadiene, 2-8 parts of antimony trioxide, 3-10 parts of aluminum hydroxide, 0.1-0.15 part of tungsten hexachloride and 5-10 parts of light aging resistant agent.
Further, the wave-transparent particles are prepared by the following steps:
step A1: dispersing an aluminum oxide ceramic wafer in ethanol, carrying out ultrasonic treatment for 1-1.5h under the condition of the frequency of 3-5kHz, filtering to remove filtrate, drying a filter cake to obtain a pretreated aluminum oxide ceramic wafer, placing a graphite crucible containing silicon monoxide in a high-temperature furnace, placing the aluminum oxide ceramic wafer on the upper part of the crucible, wrapping the aluminum oxide ceramic wafer with graphite paper, vacuumizing the high-temperature furnace, introducing nitrogen, heating to the temperature of 1400 ℃ and 1600 ℃ under the condition of the heating rate of 5-10 ℃, preserving heat for 1-1.5h, cooling to the temperature of 1000 ℃ under the condition of the cooling rate of 3-8 ℃, and then cooling to the room temperature along with the furnace to obtain nano silicon nitride;
step A2: dissolving formaldehyde in ethanol, adding paranitroaniline, stirring for 20-30min under the conditions of a rotation speed of 150-;
the reaction process is as follows:
Figure 311738DEST_PATH_IMAGE001
Figure 489648DEST_PATH_IMAGE002
Figure 687411DEST_PATH_IMAGE003
Figure 359700DEST_PATH_IMAGE004
step A3: mixing the boric acid chlorine whisker, the aluminum phosphate and the nano silicon nitride, performing ball milling for 20-30min under the condition that the rotating speed is 200-plus-300 r/min to prepare a mixture, dissolving graphite fluoride in N-methyl-2-pyrrolidone, adding the intermediate 3 and the mixture, stirring for 1-1.5h under the condition that the rotating speed is 1200-plus-1500 r/min, and performing heat preservation treatment for 1.5-2h under the condition that the temperature is 350-plus-380 ℃ to prepare the wave-transparent particles.
Further, the dosage ratio of the formaldehyde, the ethanol, the paranitroaniline and the bisphenol AF in the step A2 is 0.4mol:30mL:0.2mol:0.1mol, the dosage ratio of the intermediate 1, the tin powder and the concentrated hydrochloric acid is 4g:8.5g:20mL, the mass fraction of the concentrated hydrochloric acid is 37%, and the dosage ratio of the intermediate 2, the N-methyl-2-pyrrolidone and the hexafluoroisopropyl phthalic anhydride is 1mmol:4mL:1 mmol.
Further, the mass ratio of the boric acid chlorine whisker, the aluminum phosphate and the nano silicon nitride in the step A3 is 1:1:1, and the mass ratio of the graphite fluoride, the intermediate 3 and the mixture is 1:10: 2.5.
Further, the light aging resistant agent is prepared by the following steps:
step B1: adding m-hydroxybenzaldehyde, 2, 4-dihydroxybenzoic acid, zinc chloride, phosphorus oxychloride and sulfolane into a reaction kettle, reacting for 3-5h at the rotation speed of 200-300r/min and the temperature of 70-75 ℃ to obtain an intermediate 4, adding the intermediate 4, tetramethylpiperidylamine and ethanol into the reaction kettle, stirring and dropwise adding glacial acetic acid at the rotation speed of 150-200r/min, and after dropwise adding, performing reflux reaction for 4-6h at the temperature of 80-90 ℃ to obtain an intermediate 5;
the reaction process is as follows:
Figure 60940DEST_PATH_IMAGE005
Figure 176795DEST_PATH_IMAGE006
step B2: dissolving the intermediate 5 in tetrahydrofuran, stirring and adding epoxy chloropropane under the conditions of the rotation speed of 150-200r/min and the temperature of 35-45 ℃, adjusting the pH value of the reaction solution to 9-10, reacting for 1-3h to obtain an intermediate 6, dissolving cyanuric chloride in acetone, adding sodium hydroxide and the intermediate 6, reacting for 3-4h under the conditions of the rotation speed of 200-300r/min and the temperature of 0-5 ℃ to obtain an intermediate 7, adding the intermediate 7, melamine, sodium bicarbonate and acetone into a reaction kettle, and performing reflux reaction for 5-8h under the conditions of the rotation speed of 200-300r/min and the temperature of 80-90 ℃ to obtain the light-resistant aging agent.
The reaction process is as follows:
Figure 596275DEST_PATH_IMAGE007
Figure 72256DEST_PATH_IMAGE008
further, the using amount ratio of the m-hydroxybenzaldehyde, the 2, 4-dihydroxybenzoic acid, the zinc chloride, the phosphorus oxychloride and the sulfolane in the step B1 is 0.14mol:0.1mol:0.15mol:0.2mol:20mL, and the using amount ratio of the intermediate 4, the tetramethylpiperidylamine, the ethanol and the glacial acetic acid is 0.1mol:0.11mol:30mL:0.25 mL.
Further, the molar ratio of the intermediate 5 to the epichlorohydrin in the step B2 is 2:1, the molar ratio of the cyanuric chloride to the intermediate 6 to the cyanuric chloride to the sodium hydroxide to the intermediate 6 is 1:1:1.2, and the molar ratio of the intermediate 7 to the melamine to the sodium bicarbonate to the intermediate 7 to the melamine to the sodium bicarbonate is 1:2: 2.
The preparation method of the PDCPD material for the 5G base station housing specifically comprises the following steps:
step S1: weighing the component A and the component B, adding the component A and the component B into a mixing head, and uniformly mixing at the temperature of 22-28 ℃ to prepare a mixture with the viscosity of 0.1-0.3 Pa.s;
step S2: and (3) injecting the mixture into a mold with the temperature of 60-80 ℃ under the condition that the injection pressure is 4-7MPa, and curing for 2-5min under the condition that the mold closing pressure is 0.35-0.7MPa to prepare the PDCPD material for the 5G base station housing.
The invention has the beneficial effects that:
in the process of preparing the PDCPD material for the 5G base station housing, wave-transmitting particles and a light-resistant aging agent are prepared, the wave-transmitting material is prepared by reacting paranitroaniline, formaldehyde and bisphenol AF to prepare an intermediate 1, the intermediate 1 is reduced to prepare an intermediate 2, the intermediate 2 and hexafluoroisopropyl phthalic anhydride are polymerized to prepare an intermediate 3, the intermediate 3 belongs to polyamide acids, boric acid chlorine whisker, aluminum phosphate, nano silicon nitride and the intermediate 3 are mixed and are thermally imidized to prepare the wave-transmitting particles by solidification, the boric acid chlorine whisker, the aluminum phosphate, the nano silicon nitride and graphite fluoride in the wave-transmitting particles are inorganic fillers with low dielectric constants, the intermediate 3 is introduced with a large-volume side group structure to increase the free volume of a molecular chain, so that the number of polarized molecules in a unit volume is reduced, the dielectric constant is reduced, introducing F atoms with large radius, wherein a C-F bond has low polarizability and ionization, the F atoms can reduce the density of an intermediate 3, bisphenol AF contains two trifluoromethyl groups which can prevent the stacking of molecules and increase the free volume of the molecules, so that the dielectric constant of wave-transmitting particles is further reduced, 5G signal waves of a 5G base station housing are not influenced by the housing, a light aging resistant agent takes m-hydroxybenzaldehyde and 2, 4-dihydroxy benzoic acid as raw materials to react to prepare an intermediate 4, the intermediate 4 reacts with tetramethyl piperidinol to prepare an intermediate 5, the intermediate 5 reacts with epoxy chloropropane to prepare an intermediate 6, the intermediate 6 and cyanuric chloride react with one chlorine atom site on the cyanuric chloride through temperature control, the intermediate 7 reacts with melamine, two chlorine atom sites on the intermediate 7 react with amino groups on melamine to form a macromolecular latticed light aging resistant agent, the aging resistant agent contains a hindered amine structure and a carbonyl adjacent hydroxyl structure, when a base station housing is illuminated, peroxide can be accumulated inside the base station housing, the peroxide can initiate further oxidative degradation to generate alkoxy, the alkoxy is subjected to beta-fracture to form a new active free radical of alkyl or ketone, the hindered amine can effectively inhibit oxidation, meanwhile, an intramolecular hydrogen bond chelating ring is formed between the carbonyl adjacent hydroxyl structures, the chelating ring can be broken by light energy absorbed by illumination to reach a high-energy unstable state, in order to reach a low-energy stable state, the light aging resistant agent can excite intramolecular proton transfer, the excitation energy is converted into heat energy to be released, the intramolecular hydrogen bond chelating ring is formed again, and the effect of preventing light aging is further achieved, meanwhile, the light aging resistant agent molecules are in a macromolecular latticed structure, so that precipitation and volatilization caused by long-time use are effectively avoided.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
The PDCPD material for the 5G base station housing comprises a component A and a component B;
the component A comprises the following raw materials in parts by weight: 40 parts of dicyclopentadiene, 0.1 part of Grubbs first-generation catalyst and 15 parts of wave-transmitting particles;
the component B comprises the following raw materials in parts by weight: 40 parts of dicyclopentadiene, 2 parts of antimony trioxide, 3 parts of aluminum hydroxide, 0.1 part of tungsten hexachloride and 5 parts of light aging resistant agent;
the PDCPD material is prepared by the following steps:
step S1: weighing the component A and the component B, adding the component A and the component B into a mixing head, and uniformly mixing at the temperature of 22 ℃ to prepare a mixture with the viscosity of 0.1 Pa.s;
step S2: and (3) injecting the mixture into a mold with the temperature of 60 ℃ under the condition that the injection pressure is 4MPa, and curing for 2min under the condition that the mold closing pressure is 0.35MPa to prepare the PDCPD material for the 5G base station housing.
The wave-transparent particles are prepared by the following steps:
step A1: dispersing an aluminum oxide ceramic wafer in ethanol, carrying out ultrasonic treatment for 1.5h under the condition of 5kHz frequency, filtering to remove filtrate, drying a filter cake to obtain a pretreated aluminum oxide ceramic wafer, placing a graphite crucible containing silicon monoxide in a high-temperature furnace, placing the aluminum oxide ceramic wafer on the upper part of the crucible, wrapping the crucible with graphite paper, vacuumizing the high-temperature furnace, introducing nitrogen, heating to 1600 ℃ under the condition of 10 ℃ of heating rate, preserving heat for 1.5h, cooling to 1000 ℃ under the condition of 8 ℃ of cooling rate, and then cooling to room temperature along with the furnace to obtain nano silicon nitride;
step A2: dissolving formaldehyde in ethanol, adding p-nitroaniline, stirring for 30min under the conditions of the rotation speed of 200r/min and the temperature of 30 ℃, adding bisphenol AF, heating to the temperature of 90 ℃, reacting for 7h to prepare an intermediate 1, adding the intermediate 1, tin powder and concentrated hydrochloric acid into a reaction kettle, reacting for 30min under the conditions of the rotation speed of 150r/min and the temperature of 110 ℃, adjusting the pH value of a reaction solution to be 8-9 to prepare an intermediate 2, dissolving the intermediate 2 in N-methyl-2-pyrrolidone, adding hexafluoroisopropyl phthalic anhydride under the temperature of 20-25 ℃, and reacting for 20-25h to prepare an intermediate 3;
step A3: mixing boric acid chlorine whisker, aluminum phosphate and nano silicon nitride, performing ball milling for 30min at the rotation speed of 300r/min to obtain a mixture, dissolving graphite fluoride in N-methyl-2-pyrrolidone, adding the intermediate 3 and the mixture, stirring for 1.5h at the rotation speed of 1500r/min, and performing heat preservation treatment for 2h at the temperature of 380 ℃ to obtain the wave-transparent particles.
The light aging resistant agent is prepared by the following steps:
step B1: adding m-hydroxybenzaldehyde, 2, 4-dihydroxybenzoic acid, zinc chloride, phosphorus oxychloride and sulfolane into a reaction kettle, reacting for 5 hours at the rotation speed of 300r/min and the temperature of 75 ℃ to obtain an intermediate 4, adding the intermediate 4, tetramethylpiperidine amine and ethanol into the reaction kettle, stirring and dropwise adding glacial acetic acid at the rotation speed of 200r/min, and after dropwise adding, performing reflux reaction for 6 hours at the temperature of 90 ℃ to obtain an intermediate 5;
step B2: dissolving the intermediate 5 in tetrahydrofuran, stirring and adding epichlorohydrin under the conditions of the rotating speed of 200r/min and the temperature of 45 ℃, adjusting the pH value of a reaction solution to 10, reacting for 3 hours to obtain an intermediate 6, dissolving cyanuric chloride in acetone, adding sodium hydroxide and the intermediate 6, reacting for 4 hours under the conditions of the rotating speed of 300r/min and the temperature of 5 ℃ to obtain an intermediate 7, adding the intermediate 7, melamine, sodium bicarbonate and acetone into a reaction kettle, and performing reflux reaction for 8 hours under the conditions of the rotating speed of 300r/min and the temperature of 90 ℃ to obtain the light aging resistant agent.
Example 2
The PDCPD material for the 5G base station housing comprises a component A and a component B;
the component A comprises the following raw materials in parts by weight: 50 parts of dicyclopentadiene, 0.12 part of Grubbs first-generation catalyst and 20 parts of wave-transparent particles;
the component B comprises the following raw materials in parts by weight: 50 parts of dicyclopentadiene, 5 parts of antimony trioxide, 6 parts of aluminum hydroxide, 0.13 part of tungsten hexachloride and 8 parts of light aging resistant agent;
the PDCPD material is prepared by the following steps:
step S1: weighing a component A and a component B, adding the component A and the component B into a mixing head, and uniformly mixing at 25 ℃ to prepare a mixture with the viscosity of 0.2 Pa.s;
step S2: and (3) injecting the mixture into a mold with the temperature of 70 ℃ under the condition that the injection pressure is 5MPa, and curing for 3min under the condition that the mold closing pressure is 0.5MPa to prepare the PDCPD material for the 5G base station housing.
The wave-transparent particles are prepared by the following steps:
step A1: dispersing an aluminum oxide ceramic wafer in ethanol, carrying out ultrasonic treatment for 1.3h under the condition of the frequency of 4kHz, filtering to remove filtrate, drying a filter cake to obtain a pretreated aluminum oxide ceramic wafer, placing a graphite crucible filled with silicon monoxide in a high-temperature furnace, placing the aluminum oxide ceramic wafer on the upper part of the crucible, wrapping the aluminum oxide ceramic wafer with graphite paper, vacuumizing the high-temperature furnace, introducing nitrogen, heating to 1500 ℃ under the condition of the heating rate of 8 ℃, preserving heat for 1.3h, cooling to 1000 ℃ under the condition of the cooling rate of 5 ℃, and then cooling to room temperature along with the furnace to obtain nano silicon nitride;
step A2: dissolving formaldehyde in ethanol, adding p-nitroaniline, stirring for 25min under the conditions that the rotation speed is 180r/min and the temperature is 28 ℃, adding bisphenol AF, heating to 85 ℃, reacting for 6h to obtain an intermediate 1, adding the intermediate 1, tin powder and concentrated hydrochloric acid into a reaction kettle, reacting for 25min under the conditions that the rotation speed is 150r/min and the temperature is 105 ℃, adjusting the pH value of a reaction solution to be 8 to obtain an intermediate 2, dissolving the intermediate 2 in N-methyl-2-pyrrolidone, adding hexafluoroisopropyl phthalic anhydride under the condition that the temperature is 23 ℃, and reacting for 23h to obtain an intermediate 3;
step A3: mixing boric acid chlorine whisker, aluminum phosphate and nano silicon nitride, performing ball milling for 25min at the rotation speed of 300r/min to obtain a mixture, dissolving graphite fluoride in N-methyl-2-pyrrolidone, adding the intermediate 3 and the mixture, stirring for 1.3h at the rotation speed of 1500r/min, and performing heat preservation treatment for 1.8h at the temperature of 360 ℃ to obtain the wave-transparent particles.
The light aging resistant agent is prepared by the following steps:
step B1: adding m-hydroxybenzaldehyde, 2, 4-dihydroxybenzoic acid, zinc chloride, phosphorus oxychloride and sulfolane into a reaction kettle, reacting for 4 hours at the rotation speed of 200r/min and the temperature of 73 ℃ to obtain an intermediate 4, adding the intermediate 4, tetramethylpiperidine amine and ethanol into the reaction kettle, stirring and dropwise adding glacial acetic acid at the rotation speed of 180r/min, and after dropwise adding, performing reflux reaction for 5 hours at the temperature of 85 ℃ to obtain an intermediate 5;
step B2: dissolving the intermediate 5 in tetrahydrofuran, stirring and adding epoxy chloropropane under the conditions of the rotating speed of 180r/min and the temperature of 40 ℃, adjusting the pH value of a reaction solution to be 10, reacting for 2 hours to obtain an intermediate 6, dissolving cyanuric chloride in acetone, adding sodium hydroxide and the intermediate 6, reacting for 3.5 hours under the conditions of the rotating speed of 300r/min and the temperature of 3 ℃ to obtain an intermediate 7, adding the intermediate 7, melamine, sodium bicarbonate and acetone into a reaction kettle, and performing reflux reaction for 6 hours under the conditions of the rotating speed of 200r/min and the temperature of 85 ℃ to obtain the light aging resistant agent.
Example 3
The PDCPD material for the 5G base station housing comprises a component A and a component B;
the component A comprises the following raw materials in parts by weight: 60 parts of dicyclopentadiene, 0.15 part of Grubbs first-generation catalyst and 25 parts of wave-transmitting particles;
the component B comprises the following raw materials in parts by weight: 60 parts of dicyclopentadiene, 8 parts of antimony trioxide, 10 parts of aluminum hydroxide, 0.15 part of tungsten hexachloride and 10 parts of light aging resistant agent;
the PDCPD material is prepared by the following steps:
step S1: weighing a component A and a component B, adding the component A and the component B into a mixing head, and uniformly mixing at 28 ℃ to prepare a mixture with the viscosity of 0.3 Pa.s;
step S2: and (3) injecting the mixture into a mold with the temperature of 80 ℃ under the condition that the injection pressure is 7MPa, and curing for 5min under the condition that the mold closing pressure is 0.7MPa to prepare the PDCPD material for the 5G base station housing.
The wave-transparent particles are prepared by the following steps:
step A1: dispersing an aluminum oxide ceramic wafer in ethanol, carrying out ultrasonic treatment for 1.5h under the condition of 5kHz frequency, filtering to remove filtrate, drying a filter cake to obtain a pretreated aluminum oxide ceramic wafer, placing a graphite crucible containing silicon monoxide in a high-temperature furnace, placing the aluminum oxide ceramic wafer on the upper part of the crucible, wrapping the crucible with graphite paper, vacuumizing the high-temperature furnace, introducing nitrogen, heating to 1600 ℃ under the condition of 10 ℃ of heating rate, preserving heat for 1.5h, cooling to 1000 ℃ under the condition of 8 ℃ of cooling rate, and then cooling to room temperature along with the furnace to obtain nano silicon nitride;
step A2: dissolving formaldehyde in ethanol, adding p-nitroaniline, stirring for 30min under the conditions of the rotation speed of 200r/min and the temperature of 30 ℃, adding bisphenol AF, heating to the temperature of 90 ℃, reacting for 7h to obtain an intermediate 1, adding the intermediate 1, tin powder and concentrated hydrochloric acid into a reaction kettle, reacting for 30min under the conditions of the rotation speed of 150r/min and the temperature of 110 ℃, adjusting the pH value of a reaction solution to 9 to obtain an intermediate 2, dissolving the intermediate 2 in N-methyl-2-pyrrolidone, adding hexafluoroisopropyl phthalic anhydride under the temperature of 25 ℃, and reacting for 25h to obtain an intermediate 3;
step A3: mixing boric acid chlorine whisker, aluminum phosphate and nano silicon nitride, performing ball milling for 30min at the rotation speed of 300r/min to obtain a mixture, dissolving graphite fluoride in N-methyl-2-pyrrolidone, adding the intermediate 3 and the mixture, stirring for 1.5h at the rotation speed of 1500r/min, and performing heat preservation treatment for 2h at the temperature of 380 ℃ to obtain the wave-transparent particles.
The light aging resistant agent is prepared by the following steps:
step B1: adding m-hydroxybenzaldehyde, 2, 4-dihydroxybenzoic acid, zinc chloride, phosphorus oxychloride and sulfolane into a reaction kettle, reacting for 5 hours at the rotation speed of 300r/min and the temperature of 75 ℃ to obtain an intermediate 4, adding the intermediate 4, tetramethylpiperidine amine and ethanol into the reaction kettle, stirring and dropwise adding glacial acetic acid at the rotation speed of 200r/min, and after dropwise adding, performing reflux reaction for 6 hours at the temperature of 90 ℃ to obtain an intermediate 5;
step B2: dissolving the intermediate 5 in tetrahydrofuran, stirring and adding epichlorohydrin under the conditions of the rotating speed of 200r/min and the temperature of 45 ℃, adjusting the pH value of a reaction solution to 10, reacting for 3 hours to obtain an intermediate 6, dissolving cyanuric chloride in acetone, adding sodium hydroxide and the intermediate 6, reacting for 4 hours under the conditions of the rotating speed of 300r/min and the temperature of 5 ℃ to obtain an intermediate 7, adding the intermediate 7, melamine, sodium bicarbonate and acetone into a reaction kettle, and performing reflux reaction for 8 hours under the conditions of the rotating speed of 300r/min and the temperature of 90 ℃ to obtain the light aging resistant agent.
Comparative example 1
In this comparative example, the same procedure was used as in example 1 except that graphite fluoride was used instead of the wave-transmitting particles.
Comparative example 2
This comparative example has the same procedure as example 1 except that a light stabilizer 770 is used instead of the light aging resistor.
Comparative example 3
The comparative example is a base station protective material disclosed in Chinese patent CN 111363423A.
The sheet-like specimens obtained in examples 1 to 3 and comparative examples 1 to 3 were measured for dielectric constant at 25 ℃ and 10GHz according to the GB/T1409-2006 standard;
the tensile modulus and the tensile strength are tested according to the standard of ISO527, the impact strength is tested according to ISO180/A, and the materials prepared in the examples 1-3 and the comparative examples 1-3 are subjected to artificial accelerated aging for 2000h according to the GB/T16422.3-1997, and the tensile modulus, the tensile strength and the impact strength are continuously tested, and the results are shown in the following table;
example 1 Example 2 Example 3 Comparative example 1 Comparative example 2 Comparative example 3
Dielectric constant 1.89 1.95 1.92 3.18 1.93 3.51
Tensile modulus (MPa) 4612 4523 4546 4413 4527 4530
Tensile Strength (MPa) 51.4 52.3 51.5 48.7 51.8 59.3
Impact Strength (KJ/m)2 7.82 7.66 7.73 7.55 7.84 7.92
Tensile modulus after artificial aging (MPa) 4613 4518 4539 4426 3283 2189
Tensile Strength after Artificial aging (MPa) 51.6 52.5 51.9 49.2 38.3 32.6
Impact Strength after Artificial aging (KJ/m)2 7.79 7.71 7.69 7.53 4.52 4.23
From the above table, it can be seen that the dielectric constant of the PDCPD material for the 5G base station enclosure prepared in embodiments 1 to 3 is 1.89 to 1.95, and the mechanical strength of the material does not significantly decrease after artificial aging, indicating that the PDCPD material has a good wave-transmitting effect and does not affect normal transmission of the 5G model, and at the same time, the mechanical strength of the 5G base station enclosure does not significantly decrease after being irradiated by sunlight for a long time, so that the enclosure can normally protect the base station.
The foregoing is merely exemplary and illustrative of the principles of the present invention and various modifications, additions and substitutions of the specific embodiments described herein may be made by those skilled in the art without departing from the principles of the present invention or exceeding the scope of the claims set forth herein.

Claims (7)

1. A PDCPD material for a 5G base station housing is characterized in that: comprises a component A and a component B;
the component A comprises the following raw materials in parts by weight: 40-60 parts of dicyclopentadiene, 0.1-0.15 part of Grubbs first-generation catalyst and 15-25 parts of wave-transmitting particles;
the component B comprises the following raw materials in parts by weight: 40-60 parts of dicyclopentadiene, 2-8 parts of antimony trioxide, 3-10 parts of aluminum hydroxide, 0.1-0.15 part of tungsten hexachloride and 5-10 parts of light aging resistant agent;
the wave-transparent particles are prepared by the following steps:
step A1: treating the aluminum oxide ceramic wafer with ethanol to obtain a pretreated aluminum oxide ceramic wafer, placing a graphite crucible containing silicon monoxide in a high-temperature furnace, placing the aluminum oxide ceramic wafer on the upper part of the crucible, wrapping the aluminum oxide ceramic wafer with graphite paper, and heating at high temperature to obtain nano silicon nitride;
step A2: dissolving formaldehyde in ethanol, adding paranitroaniline, stirring, adding bisphenol AF, heating for reaction to obtain an intermediate 1, adding the intermediate 1, tin powder and concentrated hydrochloric acid into a reaction kettle, reacting, adjusting the pH value of a reaction solution to obtain an intermediate 2, dissolving the intermediate 2 in N-methyl-2-pyrrolidone, adding hexafluoroisopropyl phthalic anhydride, and reacting to obtain an intermediate 3;
step A3: carrying out ball milling on the boric acid chlorine whisker, the aluminum phosphate and the nano silicon nitride to prepare a mixture, dissolving graphite fluoride in N-methyl-2-pyrrolidone, adding the intermediate 3 and the mixture, stirring, and carrying out heat preservation treatment to prepare the wave-transmitting particles.
2. A PDCPD material for a 5G base station enclosure, according to claim 1, wherein: the dosage ratio of the formaldehyde, the ethanol, the paranitroaniline and the bisphenol AF in the step A2 is 0.4mol:30mL:0.2mol:0.1mol, the dosage ratio of the intermediate 1, the tin powder and the concentrated hydrochloric acid is 4g:8.5g:20mL, the mass fraction of the concentrated hydrochloric acid is 37%, and the dosage ratio of the intermediate 2, the N-methyl-2-pyrrolidone and the hexafluoroisopropylphthalic anhydride is 1mmol:4mL:1 mmol.
3. A PDCPD material for a 5G base station enclosure, according to claim 1, wherein: the mass ratio of the boric acid chlorine whisker, the aluminum phosphate and the nano silicon nitride in the step A3 is 1:1:1, and the mass ratio of the graphite fluoride, the intermediate 3 and the mixture is 1:10: 2.5.
4. A PDCPD material for a 5G base station enclosure, according to claim 1, wherein: the light aging resistant agent is prepared by the following steps:
step B1: adding m-hydroxybenzaldehyde, 2, 4-dihydroxybenzoic acid, zinc chloride, phosphorus oxychloride and sulfolane into a reaction kettle for reaction to obtain an intermediate 4, adding the intermediate 4, tetramethylpiperidine amine and ethanol into the reaction kettle, stirring, dropwise adding glacial acetic acid, and after dropwise addition is finished, performing reflux reaction to obtain an intermediate 5;
step B2: dissolving the intermediate 5 in tetrahydrofuran, stirring and adding epoxy chloropropane, adjusting the pH value of reaction liquid to 9-10, reacting to obtain an intermediate 6, dissolving cyanuric chloride in acetone, adding sodium hydroxide and the intermediate 6, reacting to obtain an intermediate 7, adding the intermediate 7, melamine, sodium bicarbonate and acetone into a reaction kettle, and performing reflux reaction to obtain the light aging resistant agent.
5. A PDCPD material for a 5G base station enclosure, according to claim 4, wherein: the dosage ratio of the m-hydroxybenzaldehyde, the 2, 4-dihydroxybenzoic acid, the zinc chloride, the phosphorus oxychloride and the sulfolane in the step B1 is 0.14mol:0.1mol:0.15mol:0.2mol:20mL, and the dosage ratio of the intermediate 4, the tetramethylpiperidylamine, the ethanol and the glacial acetic acid is 0.1mol:0.11mol:30mL:0.25 mL.
6. A PDCPD material for a 5G base station enclosure, according to claim 4, wherein: the molar ratio of the intermediate 5 to the epichlorohydrin in the step B2 is 2:1, the molar ratio of the cyanuric chloride to the sodium hydroxide to the intermediate 6 is 1:1:1.2, and the molar ratio of the intermediate 7 to the melamine to the sodium bicarbonate is 1:2: 2.
7. The method for preparing the PDCPD material for the 5G base station housing according to claim 1, wherein the method comprises the following steps: the method specifically comprises the following steps:
step S1: weighing the component A and the component B, adding the component A and the component B into a mixing head, and uniformly mixing at the temperature of 22-28 ℃ to prepare a mixture with the viscosity of 0.1-0.3 Pa.s;
step S2: and (3) injecting the mixture into a mold with the temperature of 60-80 ℃ under the condition that the injection pressure is 4-7MPa, and curing for 2-5min under the condition that the mold closing pressure is 0.35-0.7MPa to prepare the PDCPD material for the 5G base station housing.
CN202111102873.XA 2021-09-22 2021-09-22 PDCPD material for 5G base station housing and preparation method thereof Withdrawn CN114573953A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115182070A (en) * 2022-07-07 2022-10-14 广东樱基森实业有限公司 Antibacterial breathable fabric and preparation process thereof
CN115612297A (en) * 2022-10-17 2023-01-17 深圳市米韵科技有限公司 Low dielectric material for 5G base station shell and preparation method thereof

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115182070A (en) * 2022-07-07 2022-10-14 广东樱基森实业有限公司 Antibacterial breathable fabric and preparation process thereof
CN115182070B (en) * 2022-07-07 2023-02-24 广东樱基森实业有限公司 Antibacterial breathable fabric and preparation process thereof
CN115612297A (en) * 2022-10-17 2023-01-17 深圳市米韵科技有限公司 Low dielectric material for 5G base station shell and preparation method thereof

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Application publication date: 20220603