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CN115353691A - Liquid crystal polymer material for 5G communication field and preparation method thereof - Google Patents

Liquid crystal polymer material for 5G communication field and preparation method thereof Download PDF

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CN115353691A
CN115353691A CN202211007165.2A CN202211007165A CN115353691A CN 115353691 A CN115353691 A CN 115353691A CN 202211007165 A CN202211007165 A CN 202211007165A CN 115353691 A CN115353691 A CN 115353691A
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liquid crystal
polymer material
crystal polymer
titanium dioxide
syndiotactic polystyrene
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CN115353691B (en
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周江
王钦
虞成城
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Shenzhen Sunway Communication Co Ltd
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Shenzhen Sunway Communication Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K7/00Use of ingredients characterised by shape
    • C08K7/02Fibres or whiskers
    • C08K7/04Fibres or whiskers inorganic
    • C08K7/14Glass
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20Oxides; Hydroxides
    • C08K3/22Oxides; Hydroxides of metals
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00Use of organic ingredients
    • C08K5/04Oxygen-containing compounds
    • C08K5/09Carboxylic acids; Metal salts thereof; Anhydrides thereof
    • C08K5/098Metal salts of carboxylic acids
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20Oxides; Hydroxides
    • C08K3/22Oxides; Hydroxides of metals
    • C08K2003/2237Oxides; Hydroxides of metals of titanium
    • C08K2003/2241Titanium dioxide

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Abstract

The invention relates to a liquid crystal polymer material used in the field of 5G communication and a preparation method thereof, belonging to the technical field of communication materials. The liquid crystal polymer material for the 5G communication field comprises the following raw materials in parts by weight: 30 to 80 portions of syndiotactic polystyrene, 20 to 60 portions of titanium dioxide, 1 to 5 portions of calcium stearate, 0.1 to 1 portion of antioxidant and 0.1 to 30 portions of glass fiber. The liquid crystal polymer material is prepared by mixing titanium dioxide with high dielectric constant with the syndiotactic polystyrene resin, and the liquid crystal polymer material with high dielectric constant and low dielectric loss is obtained.

Description

Liquid crystal polymer material for 5G communication field and preparation method thereof
Technical Field
The invention belongs to the technical field of communication materials, and particularly relates to a liquid crystal polymer material used in the field of 5G communication and a preparation method thereof.
Background
With the continuous development of 5G network technology, the future life is more and more intelligent and digitalized, and the interconnection of everything is gradually going into each family. The development of new technologies such as automatic driving, intelligent furniture, VR/AR, metauniverse and the like is technically supported by a large data processing center, an ultra-low delay transmission mode and a large batch of cloud computing. With the increasing perfection of 5G network deployment, terminal manufacturers have higher requirements for miniaturization of signal modules and scale and speed of data transmission, and the requirements for low dielectric loss materials are increasing.
The Chinese patent with the publication number of CN103923449B discloses a PC/ABS (polycarbonate/acrylonitrile-styrene-butadiene copolymer alloy) composite material for laser direct molding, and the dielectric loss is 0.007; however, polycarbonate and its alloy resin have higher dielectric loss than low frequency in high frequency band, and thus are not suitable for LDS antennas in the 5G communication era. There is a trend toward the development of communication materials with low dielectric loss (dielectric loss less than 0.002) in the high frequency band.
Disclosure of Invention
In order to overcome the defects of the prior art, the technical problems to be solved by the invention are as follows: how to prepare a liquid crystal polymer material with low loss and high dielectric constant for the 5G communication field.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows: a liquid crystal polymer material for the field of 5G communication comprises the following raw materials in parts by weight: 30 to 80 portions of syndiotactic polystyrene, 20 to 60 portions of titanium dioxide, 1 to 5 portions of calcium stearate, 0.1 to 1 portion of antioxidant and 0.1 to 30 portions of glass fiber.
The invention adopts another technical scheme that: a preparation method of a liquid crystal polymer material used in the field of 5G communication comprises the following steps:
s1: respectively drying the syndiotactic polystyrene resin, the titanium dioxide and the glass fiber;
s2: dispersing the dried syndiotactic polystyrene resin, titanium dioxide, calcium stearate and antioxidant to obtain a mixture;
s3: and melting and mixing the mixture, adding glass fiber, extruding, bracing, cooling and granulating to obtain the liquid crystal polymer material.
The invention has the beneficial effects that: the liquid crystal polymer material for the 5G communication field takes the syndiotactic polystyrene as a matrix material, is modified by adding the titanium dioxide, the titanium dioxide is titanium oxide and has higher dielectric constant, the overall dielectric constant of the prepared liquid crystal polymer material is improved by mixing the titanium dioxide with high dielectric constant with the syndiotactic polystyrene resin, the liquid crystal polymer material with low loss factor and high dielectric constant is obtained, and the application of the syndiotactic polystyrene composite in the high 5G communication field is effectively improved.
Detailed Description
In order to explain the technical content, the objects and the effects of the present invention in detail, the following description will be given with reference to the embodiments.
The most key concept of the invention is as follows: mixing the titanium dioxide with high dielectric constant with the syndiotactic polystyrene resin to improve the overall dielectric constant of the prepared liquid crystal polymer material.
The invention relates to a liquid crystal polymer material used in the field of 5G communication, which comprises the following raw materials in parts by weight: 30 to 80 portions of Syndiotactic Polystyrene (SPS), 20 to 60 portions of titanium dioxide, 1 to 5 portions of calcium stearate, 0.1 to 1 portion of antioxidant and 0.1 to 30 portions of glass fiber.
Preferably, the feed comprises the following raw materials in parts by weight: 50-60 parts of Syndiotactic Polystyrene (SPS), 30-50 parts of titanium dioxide, 2-4 parts of calcium stearate, 0.3-0.8 part of antioxidant and 1-25 parts of glass fiber.
As can be seen from the above description, the beneficial effects of the present invention are: syndiotactic polystyrene is used as a matrix material, titanium dioxide is added for modification, the titanium dioxide is titanium oxide and has a high dielectric constant, the titanium dioxide with a high dielectric constant is mixed with syndiotactic polystyrene resin, the overall dielectric constant of the prepared liquid crystal polymer material is improved, the liquid crystal polymer material with a low loss factor and a high dielectric constant is obtained, and the application of the syndiotactic polystyrene composite in the field of high-5G communication is effectively improved. The glass fiber is a reinforcing material, and can improve the physical properties of the liquid crystal polymer material.
Furthermore, the molecular weight of the Syndiotactic Polystyrene (SPS) resin is 30W-50W, and the polymerization degree is 3000-5000.
As can be seen from the above description, syndiotactic polystyrene resin has a molecular weight of 30W-50W, a good fluidity at a polymerization degree of 3000-5000, and a certain mechanical property, and even after a high proportion of inorganic filler is added, has a certain processability and strength.
The other technical scheme of the invention is as follows: a preparation method of a liquid crystal polymer material used in the field of 5G communication comprises the following steps:
s1: respectively drying the syndiotactic polystyrene resin, the titanium dioxide and the glass fiber;
s2: dispersing the dried syndiotactic polystyrene resin, titanium dioxide, calcium stearate and antioxidant to obtain a mixture;
s3: and melting and mixing the mixture, adding glass fiber, extruding, drawing into strips, cooling and granulating to obtain the liquid crystal polymer material.
From the above description, it can be seen that mixing titanium dioxide having a high dielectric constant with a syndiotactic polystyrene resin improves the overall dielectric constant of the liquid crystal polymer material prepared.
The calcium stearate is used as a lubricant to increase the lubricating property between the syndiotactic polystyrene resin and equipment during melting and mixing, and prevent the resin from being adhered to the equipment and repeatedly heated and carbonized to generate impurities.
Furthermore, the drying time is 4-8 h.
From the above description, the purpose of the drying treatment is to reduce the water content in the raw materials, avoid pores in the extruded granules due to the evaporation of moisture in the melting and mixing process, and simultaneously avoid the influence of water stains on the surface of the product after the modified liquid crystal polymer material is subsequently injection molded into the product by an injection molding machine; moreover, the water content has influence on the dielectric property of the material, the larger the water content is, the worse the dielectric property is, and the dielectric property of the liquid crystal polymer material can be improved after drying.
Further, the time for the dispersion treatment is 2 to 10min.
As can be seen from the above description, the dispersion treatment time is short and the mixture uniformity is poor; long dispersion time and low efficiency.
Further, in the step S3, a double-screw extruder is used for melt mixing and extrusion, and the temperature of the double-screw extruder from a die head to a feeding port is 280-300 ℃, 290-320 ℃, 280-290 ℃, 270-290 ℃ and 240-270 ℃ in sequence.
As can be seen from the above description, the temperature parameters of the twin-screw extruder are set according to Tg, tm and decomposition temperature of syndiotactic polystyrene, wherein 280-300 ℃ is the die temperature, 290-320 ℃, 280-290 ℃, 270-290 ℃ and 240-270 ℃ are the temperatures of the 5/4/3/2/1 zones of the screw of the twin-screw extruder in sequence, and higher temperatures of the temperatures can cause the SPS to be oxidized and decomposed in the screw, the mechanical properties of the SPS to be reduced, the resin to be yellowed, and lower temperatures of the SPS to cause the resin to be poor in fluidity, and the SPS to be insufficiently mixed with the inorganic filler, so that the processability of the SPS is poor.
Further, in the dispersion treatment of S2, the syndiotactic polystyrene resin and titanium dioxide are premixed.
From the above description, it can be known that syndiotactic polystyrene and titanium dioxide are usually premixed by using a high-speed mixer or a planetary mixer, the premixed resin and titanium dioxide powder pass through a mixing zone and a plasticizing zone in a twin-screw extruder, and the extruded titanium dioxide can be relatively uniformly mixed in the syndiotactic polystyrene because the screw temperature is high enough and the syndiotactic polystyrene is molten at the temperature and is secondarily mixed under the shearing force of the screw.
Example 1 of the present invention is:
a preparation method of a liquid crystal polymer material used in the field of 5G communication comprises the following steps:
s1: respectively drying 59g of syndiotactic polystyrene resin, 20g of titanium dioxide and 15g of glass fiber at 80 ℃ for 7h;
s2: premixing the dried syndiotactic polystyrene resin and titanium dioxide at 480rpm for 10min, mixing with 5g of calcium stearate and 1g of antioxidant, and dispersing in a high-speed mixer for 8min to obtain a mixture;
s3: and putting the mixture into a double-screw extruder for melting and mixing, adding glass fiber through a side material port of the double-screw extruder, and then extruding, drawing strips, cooling and granulating to obtain the liquid crystal polymer material.
The temperatures of the twin-screw extruder from the die head to the feeding port were 290 ℃,300 ℃,310 ℃,285 ℃,280 ℃ and 260 ℃, respectively. The twin-screw extruder was rotated at 150rpm, the feeding frequency was 5Hz, and the side feeding frequency was also 5Hz.
The Syndiotactic Polystyrene (SPS) resin has molecular weight of 30-50W and polymerization degree of 3000-5000. The model of the titanium dioxide is QTO-25M. The antioxidants are basf antioxidant 1010 and basf antioxidant 168 in a ratio of 1:1 composite powder.
Example 2 of the present invention is:
example 2 differs from example 1 in that: 44g of syndiotactic polystyrene resin and 35g of titanium dioxide
Example 3 of the present invention is:
example 3 differs from example 1 in that: 34g of syndiotactic polystyrene resin and 45g of titanium dioxide
Example 4 of the present invention is:
a preparation method of a liquid crystal polymer material used in the field of 5G communication comprises the following steps:
s1: 40g of syndiotactic polystyrene resin, 60g of titanium dioxide and 0.1g of glass fiber are respectively dried for 4 hours at 80 ℃;
s2: premixing dried syndiotactic polystyrene resin and titanium dioxide at 480rpm for 10min, mixing with 1g of calcium stearate and 0.1g of antioxidant, and dispersing in a high-speed mixer for 2min to obtain a mixture;
s3: and putting the mixture into a double-screw extruder for melting and mixing, adding glass fiber through a side material port of the double-screw extruder, and then extruding, drawing strips, cooling and granulating to obtain the liquid crystal polymer material.
The temperatures of the twin-screw extruder from the die head to the feed port were 280 ℃,290 ℃,290 ℃,280 ℃,270 ℃ and 240 ℃, respectively. The twin screw extruder speed was 150RPM, the feed frequency was 5Hz, and the side feed frequency was also 5Hz.
The Syndiotactic Polystyrene (SPS) resin has molecular weight of 30-50W and polymerization degree of 3000-5000. The model of the titanium dioxide is QTO-25M.
Example 5 of the present invention is:
a preparation method of a liquid crystal polymer material used in the field of 5G communication comprises the following steps:
s1: 80g of syndiotactic polystyrene resin, 20g of titanium dioxide and 30g of glass fiber are respectively dried for 8 hours at 80 ℃;
s2: premixing dried syndiotactic polystyrene resin and titanium dioxide at 480rpm for 10min, mixing with 4g of calcium stearate and 0.7g of antioxidant, and dispersing in a high-speed mixer for 10min to obtain a mixture;
s3: and putting the mixture into a double-screw extruder for melting and mixing, adding glass fiber through a side material port of the double-screw extruder, and then extruding, drawing strips, cooling and granulating to obtain the liquid crystal polymer material.
The temperatures of the twin-screw extruder from the die head to the feeding port were 300 ℃,320 ℃,290 ℃,290 ℃ and 270 ℃, respectively. The twin screw extruder was operated at 150RPM with a 5Hz feed frequency and a 5Hz side feed frequency.
The Syndiotactic Polystyrene (SPS) resin has molecular weight of 30-50W and polymerization degree of 3000-5000. The model of the titanium dioxide is QTO-25M.
Comparative example 1 of the present invention is:
comparative example 1 differs from example 1 in that: 100g of syndiotactic polystyrene resin, titanium dioxide, calcium stearate antioxidant and glass fiber were not added.
Comparative example 2 of the present invention is:
comparative example 2 differs from example 1 in that: the syndiotactic polystyrene resin was 64g, the glass fiber was 30g, and no titanium dioxide was added.
The liquid crystal polymer materials prepared in examples 1 to 3 and comparative examples 1 to 2 were tested for flexural strength, tensile strength, dielectric constant and dissipation factor, and the test results are shown in table 1.
TABLE 1
Figure BDA0003808354100000061
Figure BDA0003808354100000071
As can be seen from Table 1, the increase of titanium dioxide improves the dielectric constant of the liquid crystal polymer material, the addition of syndiotactic polystyrene reduces the dielectric dissipation factor, and the addition of glass fiber improves the flexural strength and tensile strength.
In conclusion, the liquid crystal polymer material for the 5G communication field provided by the invention takes the syndiotactic polystyrene as a matrix material, the modification is carried out by adding the titanium dioxide, the titanium dioxide is titanium oxide and has a higher dielectric constant, the overall dielectric constant of the prepared liquid crystal polymer material is improved by mixing the titanium dioxide with a high dielectric constant with the syndiotactic polystyrene resin, the liquid crystal polymer material with a low loss factor and a high dielectric constant is obtained, and the application of the syndiotactic polystyrene composite in the high 5G communication field is effectively improved.
The above description is only an example of the present invention and is not intended to limit the scope of the present invention, and all equivalent modifications made by the present invention as described in the specification of the present invention or directly or indirectly applied to the related technical fields are included in the scope of the present invention.

Claims (7)

1. A liquid crystal polymer material for the field of 5G communication is characterized by comprising the following raw materials in parts by weight: 30 to 80 portions of syndiotactic polystyrene, 20 to 60 portions of titanium dioxide, 1 to 5 portions of calcium stearate, 0.1 to 1 portion of antioxidant and 0.1 to 30 portions of glass fiber.
2. The liquid crystal polymer material for 5G communication as claimed in claim 1, wherein the SPS resin has a molecular weight of 30W to 50W and a degree of polymerization of 3000 to 5000.
3. A preparation method of a liquid crystal polymer material used in the field of 5G communication is characterized by comprising the following steps:
s1: respectively drying the syndiotactic polystyrene resin, the titanium dioxide and the glass fiber;
s2: dispersing the dried syndiotactic polystyrene resin, titanium dioxide, calcium stearate and antioxidant to obtain a mixture;
s3: and melting and mixing the mixture, adding glass fiber, extruding, bracing, cooling and granulating to obtain the liquid crystal polymer material.
4. The method for preparing a liquid crystal polymer material used in the field of 5G communication according to claim 3, wherein the drying treatment time is 4 to 8 hours.
5. The method for preparing a liquid crystal polymer material used in the field of 5G communication according to claim 3, wherein the time for the dispersion treatment is 2 to 10min.
6. The method for preparing a liquid crystal polymer material used in the field of 5G communication according to claim 3, wherein a twin-screw extruder is used in S3 for melt-kneading and extrusion, and the temperature of the twin-screw extruder from a die head to a feed port is 280-300 ℃, 290-320 ℃, 280-290 ℃, 270-290 ℃ and 240-270 ℃ in this order.
7. The method for preparing a liquid crystal polymer material used in the field of 5G communication according to claim 3, wherein the dispersing step S2 comprises premixing the syndiotactic polystyrene resin and titanium dioxide.
CN202211007165.2A 2022-08-22 2022-08-22 Liquid crystal polymer material for 5G communication field and preparation method thereof Active CN115353691B (en)

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20020004004A (en) * 2000-06-29 2002-01-16 유현식 Method of Preparing Modified Syndiotactic Polystyrene by Extruder
CN107459805A (en) * 2016-06-06 2017-12-12 华为技术有限公司 A kind of antenna for base station cover and its manufacture method
CN108219460A (en) * 2018-02-07 2018-06-29 深圳华力兴新材料股份有限公司 A kind of NMT technologies PPS/SPS engineering plastics and preparation method
CN110903612A (en) * 2019-12-20 2020-03-24 江门市德众泰工程塑胶科技有限公司 Liquid crystal polyester composition and preparation method thereof
CN110951177A (en) * 2019-12-13 2020-04-03 Oppo广东移动通信有限公司 Nano-injection composite material and preparation method thereof, housing assembly and electronic device
CN113480310A (en) * 2021-07-14 2021-10-08 重庆大学 High-density and high-dielectric-constant tantalum pentoxide-based ceramic and preparation method thereof

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20020004004A (en) * 2000-06-29 2002-01-16 유현식 Method of Preparing Modified Syndiotactic Polystyrene by Extruder
CN107459805A (en) * 2016-06-06 2017-12-12 华为技术有限公司 A kind of antenna for base station cover and its manufacture method
CN108219460A (en) * 2018-02-07 2018-06-29 深圳华力兴新材料股份有限公司 A kind of NMT technologies PPS/SPS engineering plastics and preparation method
CN110951177A (en) * 2019-12-13 2020-04-03 Oppo广东移动通信有限公司 Nano-injection composite material and preparation method thereof, housing assembly and electronic device
CN110903612A (en) * 2019-12-20 2020-03-24 江门市德众泰工程塑胶科技有限公司 Liquid crystal polyester composition and preparation method thereof
CN113480310A (en) * 2021-07-14 2021-10-08 重庆大学 High-density and high-dielectric-constant tantalum pentoxide-based ceramic and preparation method thereof

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