CN114231031A - Foamed polyphenylene sulfide composition and preparation method and application thereof - Google Patents
Foamed polyphenylene sulfide composition and preparation method and application thereof Download PDFInfo
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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
- C08J9/12—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 physical blowing agent
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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
- C08J9/08—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 carbon dioxide
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- C08J2203/00—Foams characterized by the expanding agent
- C08J2203/02—CO2-releasing, e.g. NaHCO3 and citric acid
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- C08J2203/00—Foams characterized by the expanding agent
- C08J2203/06—CO2, N2 or noble gases
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- C08J2381/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing sulfur with or without nitrogen, oxygen, or carbon only; Polysulfones; Derivatives of such polymers
- C08J2381/02—Polythioethers; Polythioether-ethers
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Abstract
The invention discloses a foaming polyphenylene sulfide composition which comprises the following components in parts by weight: 65 parts of polyphenylene sulfide resin; 20-40 parts of low-dielectric glass fiber; in the foaming polyphenylene sulfide composition, more than 98 percent of the pore diameters are in the range of 1-100 microns, the average pore diameter is 20-40 microns, and the cell density is 109‑1015Per cm3(ii) a The average retention length of the low dielectric glass fiber in the resin matrix is 190-220 microns. The foaming polyphenylene sulfide composition has the advantage of low dielectric constant.
Description
Technical Field
The invention relates to the technical field of high polymer materials, in particular to a foamed polyphenylene sulfide composition and a preparation method and application thereof.
Background
With the advent of the 5G era, the requirements for transmission speed and loss of electronic signals are higher than those of 4G products, and generally, the dielectric constant of the 4G products for resin materials is only required to be less than 3.7(1GHz), while the dielectric constant of the 5G products for resin materials is required to be less than 3.2(1 GHz). There are generally three ways to reduce the dielectric constant of polymers, which are: firstly, fluorine atoms are introduced into a polymer molecular chain, so that the stacking density of the molecular chain is reduced, and the free motion space of the molecular chain is improved, thereby reducing the dielectric constant of the polymer; secondly, introducing bulky structures (such as polyhedral oligomeric silsesquioxane polymers, POSS) by physical or chemical methods, or introducing microporous structures, or introducing bulky molecular chain side groups (such as benzene rings); third, the dielectric constant of the blend is reduced by blending other lower dielectric constant materials, such as Polytetrafluoroethylene (PTFE) with a relative dielectric constant of 2.0(1GHz), or low dielectric glass fibers.
Polyphenylene Sulfide (PPS) has good high temperature resistance and thermal stability, excellent chemical corrosion resistance, excellent physical and mechanical properties, good adhesion performance, good dimensional stability, excellent flame retardance and good electrical properties. The polyphenylene sulfide resin has a plurality of excellent properties, so that the polyphenylene sulfide resin is widely applied to the industries of machinery, electronics, automobiles, aerospace, 5G and the like. However, polyphenylene sulfide resin has a dielectric constant of 3.8 to 5.0, and its application in the field of microelectronics is limited. It is necessary to reduce the dielectric constant by physical or chemical modification.
Chinese patent application CN112226082A discloses a membrane material based on 5G communication, wherein adamantyl quaternary ammonium salt silane is adopted to co-modify 60-70 parts of hyperbranched polyphenylene sulfide, 10-20 parts of hyperbranched sulfonated polyether ether ketone and 4-7 parts of micron-sized hollow mesoporous silica microspheres, and foaming treatment is carried out. The material has a large amount of bubbles and has the characteristic of low dielectric. However, because the micron-sized hollow mesoporous silica microspheres are introduced into the structure and the traditional foaming process is adopted, the obtained cells have different particle sizes and the minimum value of the dielectric constant cannot be realized under the limited modification condition.
Disclosure of Invention
The invention aims to provide a foaming polyphenylene sulfide composition which has the advantages of low dielectric property and high strength. The invention also aims to provide a preparation method and application of the foaming polyphenylene sulfide composition.
The invention is realized by the following technical scheme:
the foaming polyphenylene sulfide composition comprises the following components in parts by weight:
65 parts of polyphenylene sulfide resin;
20-40 parts of low-dielectric glass fiber;
in the foaming polyphenylene sulfide composition, more than 98 percent of the pore diameters are in the range of 1-100 microns, the average pore diameter is 20-40 microns, and the cell density is 109-1015Per cm3；
The average retention length of the low dielectric glass fiber in the resin matrix is 190-220 microns.
The polyphenylene sulfide resin is straight-chain polyphenylene sulfide resin.
The melt flow rate of the polyphenylene sulfide resin is 100-1800g/10min, and the test conditions are 316 ℃ and 5kg (according to ISO 1133-1-2011 standard test).
The dielectric constant Dk of the low dielectric glass fiber is less than 4.5, and the test condition is 1GHZ。
Whether 0-2 parts of auxiliary agent is added or not can be determined according to actual requirements, and the auxiliary agent can be at least one of an antioxidant and a lubricant.
The antioxidant may be: 1,3, 5-trimethyl-2, 4, 6-tris (3, 5-di-tert-butyl-4-hydroxybenzyl) benzene; 2, 5-di-tert-butyl-4-hydroxybenzyldimethylamine; diethyl-3, 5-di-tert-butyl-4-hydroxybenzyl phosphate; stearyl-3, 5-di-tert-butyl-4-hydroxybenzyl phosphate; 3, 5-di-tert-butyl-4-hydroxyphenyl-3, 5-distearyl-thiotriazolylamine; 2, 6-di-tert-butyl-4-hydroxymethylphenol; 2, 4-bis- (n-octylthio) -6- (4-hydroxy-3, 5-di-tert-butyl glyceryl allyl ether) -1,3, 5-triazine; n, N' -hexamethylenebis (3, 5-di-tert-butyl-4-hydroxy-hydrocinnamamide); n, N' -bis- (3- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionyl) hexamethylenediamine; octadecyl-3- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate; pentaerythrityl-tetrakis [3- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ]; triethylene glycol-bis [3- (3, 5-dimethyl-4-hydroxyphenyl) propionate ]; triethylene glycol bis [ beta- (3-tert-butyl-4-hydroxy-5-methylphenyl) propionate ]; 2, 2' -thiodiethyl-bis [3- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate, and the like.
The lubricant may be: at least one of a stearate lubricant, a fatty acid lubricant, and a stearate lubricant; the stearate lubricant is at least one selected from calcium stearate, magnesium stearate and zinc stearate; the fatty acid lubricant is at least one selected from fatty acid, fatty acid derivative and fatty acid ester; the stearate lubricant is at least one selected from pentaerythritol stearate.
The foaming polyphenylene sulfide composition is obtained by foaming through a physical foaming agent and/or foaming through a chemical foaming agent; the physical foaming agent is selected from at least one of compressed gas, soluble solid and volatile liquid with the boiling point lower than 110 ℃; the chemical foaming agent is selected from inorganic foaming agents and organic foaming agents, wherein the inorganic foaming agents are selected from at least one of carbonates, nitrites, potassium borohydride and sodium borohydride; the organic foaming agent is at least one selected from azo compounds, nitrite compounds and sulfonyl hydrazide compounds.
In particular, the compressed gas may be: inert gases such as nitrogen, carbon dioxide, and the like.
The soluble solid may be: the low boiling point liquid is mixed into the solid polymer particles at normal temperature or lower temperature, and then heated, so that the low boiling point liquid in the particles is vaporized, and the polymer contains a large amount of micro bubbles.
Volatile liquids with a boiling point below 110 ℃ may be: low carbon number hydrocarbons (pentane, isopentane, hexane, isohexane), freon, etc
The carbonates may be: sodium bicarbonate, ammonium carbonate, and the like;
the nitrite can be: sodium nitrite;
the azo may be: azodicarbonamide, azobisisobutyronitrile, and the like;
the nitrites can be: n, N-dinitrosopentamethylenetetramine (H blowing agent);
the sulfonyl hydrazines may be: 4,4' -oxybis-benzenesulfonyl hydrazide (i.e., OBSH blowing agent), 3-disulfonyl hydrazide diphenyl sulfone, benzenesulfonyl hydrazide (BSH), p-toluenesulfonyl hydrazide (TSH), and the like.
The dielectric constant Dk of the foaming polyphenylene sulfide composition is less than or equal to 3.2, and the testing condition is 1GHZ。
The preparation method of the foaming polyphenylene sulfide composition comprises the following steps: according to the proportion, the polyphenylene sulfide resin is extruded by a double-screw extruder, the screw is divided into 10 sections, wherein low-dielectric glass fiber is fed from the side of 6 sections, foaming agent is fed from the side of 8 sections, the temperature range of a screw cylinder is 1-4 sections 285-295 ℃, 5-7 sections 290-300 ℃, 8-10 sections 275-285 ℃ and the rotating speed range is 300-500 rpm.
The retention length of the low dielectric glass fiber is mainly controlled by the method of controlling the shearing strength of the screw (the invention mainly controls the shearing strength by controlling the rotating speed) or pre-crushing the low dielectric glass fiber, and the like.
The invention realizes micro-foaming (more than 98 percent of the pore diameter of the cells is 1-100 microns) by adding the foaming agent in 8 sections (the rear section of the screw), and further can finely adjust the foaming degree by a conventional method (the foaming degree is controlled by controlling the adding amount of the chemical foaming agent by the chemical foaming agent, and the foaming degree is finely adjusted by controlling the air input (saturation pressure) by a physical foaming agent such as carbon dioxide, namely, the cell density and the cell density are further adjusted) on the basis of micro-foaming.
Through experiments, under the preparation process of the invention, the addition of various foaming agents is as follows:
compressing gas: the saturation pressure range is more than 18 MPa;
volatile liquid with boiling point below 110 ℃: the adding amount is 4-6wt% of the total weight of the materials;
sodium bicarbonate, ammonium carbonate: the adding amount is 4-6wt% of the total weight of the materials;
sodium nitrite: the adding amount is 4-6wt% of the total weight of the materials;
sulfonyl hydrazides: the adding amount is 4-6wt% of the total weight of the materials;
the foamed polyphenylene sulfide composition provided by the invention is applied to preparing a workpiece for a high-frequency electromagnetic wave working occasion, such as a 5G base station antenna component.
The invention has the following beneficial effects:
according to the invention, by adopting a micro-foaming technology and controlling the retention length of the low-dielectric glass fiber by controlling the shear strength, the foamed polyphenylene sulfide composition disclosed by the invention has uniform cell distribution and uniform cell size, and further has the advantages of low dielectric and high strength.
Drawings
FIG. 1: the microscopic picture of the section view of the foamed polyphenylene sulfide composition obtained by the micro-foaming technology has uniform distribution and size of cells.
FIG. 2: a microscopic photograph of a cross-sectional view of a foamed polyphenylene sulfide composition was obtained using a conventional foaming technique (comparative example 2), wherein the cells were not uniform in size and distribution.
Detailed Description
The present invention will be described in detail with reference to specific examples. The following examples will assist those skilled in the art in further understanding the invention, but are not intended to limit the invention in any way. It should be noted that variations and modifications can be made by persons skilled in the art without departing from the spirit of the invention. All falling within the scope of the present invention.
The raw material sources used in the examples and comparative examples are as follows:
polyphenylene sulfide resin a: straight chain, designation 1150C, MFR =450g/10min (316 ℃, 5kg), zhejiang novand specialty plastics, inc;
polyphenylene sulfide resin B: straight chain, designation 1110C, MFR =100g/10min (316 ℃, 5kg), zhejiang novand specialty plastics, inc;
low dielectric glass fiber: the product is characterized by comprising the following components in parts by weight, wherein the product is the trademark TLD-CS10-3.0-T433, the dielectric constant (1GHZ) =4.2-4.4, the length is 3mm, and the Taishan glass fiber is prepared;
common glass fiber, the trade mark ECS10-3.0-T433, the dielectric constant (1GHZ) =6.6-6.8, the length is 3mm, Mount Taishan glass fiber;
chemical foaming agent: sodium bicarbonate, brand No.: POLYTHLENE F-70, Yonghe Fine chemical Co., Ltd;
physical foaming agent: carbon dioxide;
lubricant: TR044W, STRUKTOL Co. (ii) a
Examples and comparative examples preparation of foamed polyphenylene sulfide compositions: according to the proportion, the polyphenylene sulfide resin is extruded by a double-screw extruder, the screw is divided into 10 sections, wherein the glass fiber is fed from the side of 6 sections, the foaming agent is fed from the side of 8 sections (the foaming agent is added into the 7 th section of comparative example 1, and the foaming agent is added into the 6 th section of comparative example 2/6), the temperature range of the barrel is 1-4 sections 285-295 ℃, 5-7 sections 290-300 ℃, 8-10 sections 275-285 ℃ and the rotating speed range is 300-500rpm (see the table for details). Also, examples and comparative examples (except example 4) were fine-tuned in the degree of foaming by controlling the saturation pressure of carbon dioxide.
The test method comprises the following steps:
(1) tensile strength: tested according to ISO 527-2-2012.
(2) Density: tested according to ISO 1183-1-2012.
(3) Dielectric constant: the test frequency is 1GHz according to the test of GB/T5597-1999 standard. For the present composition, the lower the dielectric constant, the better.
(4) Section view of the foamed polyphenylene sulfide composition: and (3) injecting an ISO standard notch impact sample strip into the sample, and quickly breaking the sample after soaking the sample in liquid nitrogen for 2 minutes. Taking a sample of the cross section, placing the cross section under a quadratic element instrument (model YVM-3020, Dongguan Tokyo instruments Co., Ltd.) to watch the appearance (the magnification is 100 times), and measuring and counting the pore diameter and the average value of the cells by using quadratic element self-contained software; and calculating the density of the cells according to the density change before and after foaming and the number of the cells in the statistical area. Formula reference: researches on chain extension reaction and foaming behavior of thermoplastic polyamide elastomer [ J ] Chinese plastics, 2021,35(10):14-20. the concrete steps are as follows:
wherein the content of the first and second substances,
n-cell density, units/cm3；
n is the counted number of the foam holes;
area in cm of A-quadratic photograph2；
ρ1Density before foaming, g/cm3；
ρ2Density after foaming, g/cm3。
(5) Testing method of average retention length of glass fiber: and (3) putting 5g of the material particles into a ceramic crucible, putting the ceramic crucible into a muffle furnace, taking out the material particles after 20min, picking out a small amount of ash, dispersing the ash in a glass vessel filled with distilled water, slightly and uniformly vibrating the glass vessel, putting the glass vessel on a sample table with a quadratic element, and observing and counting the length and the average length of the glass fiber.
Table 1: examples foamed polyphenylene sulfide compositions having respective component contents (parts by weight) and test results
| Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | Example 6 | |
| Polyphenylene sulfide resin A | 65 | - | 65 | 65 | 65 | 65 |
| Polyphenylene sulfide resin B | - | 65 | - | - | - | - |
| Low dielectric glass fiber | 30 | 30 | 20 | 40 | 30 | 30 |
| Type of blowing agent | Physics of physics | Physics of physics | Physics of physics | Chemistry | Physics of physics | Physics of physics |
| Lubricant agent | 0.3 | 0.3 | - | 0.3 | 0.3 | 0.3 |
| Screw speed, rpm | 350 | 350 | 350 | 350 | 350 | 350 |
| Carbon dioxide saturation pressure (MPa) | 24 | 22 | 21 | N/A | 23 | 26 |
| Cell average pore diameter, microns | 24.1 | 37.6 | 39.5 | 28.0 | 33.5 | 21.3 |
| Whether more than 98% of the cell pores have a diameter in the range of 1-100 μm | Is that | Is that | Is that | Is that | Is that | Is that |
| Cell density, cell/cm3 | 109 | 1012 | 1011 | 1010 | 1015 | 1014 |
| Average retention length of glass fiber, micron | 210.6 | 197.2 | 199.8 | 203.0 | 204.1 | 218.6 |
| Tensile strength, MPa | 155 | 148 | 143 | 160 | 152 | 157 |
| Density, g/cm3 | 1.44 | 1.36 | 1.38 | 1.41 | 1.29 | 1.32 |
| Dielectric constant | 3.2 | 3 | 3.1 | 3.4 | 2.8 | 2.9 |
Example 4 the amount of chemical blowing agent added was 5 parts.
From examples 1 to 6, it is understood that the foaming by the micro-foaming means of the present invention is controlled within the range of the present invention, and further the glass fiber retention length is controlled at 190-220 μm, so that the advantage of low dielectric constant can be achieved. Also, it can be seen that the higher the cell density, the lower the dielectric constant.
Table 2: comparative example
| Comparative example 1 | Comparative example 2 | Comparative example 3 | Comparative example 4 | Comparative example 5 | Comparative example 6 | |
| Polyphenylene sulfide resin A | 65 | 65 | 65 | 65 | 65 | 65 |
| Low dielectric glass fiber | 30 | 30 | 30 | 30 | 30 | |
| Ordinary glass fiber | 30 | |||||
| Type of blowing agent | Physics of physics | Physics of physics | Physics of physics | Physics of physics | Physics of physics | Physics of physics |
| Lubricant agent | 0.3 | 0.3 | 0.3 | 0.3 | 0.3 | 0.3 |
| Screw speed, rpm | 350 | 350 | 350 | 500 | 310 | 260 |
| Carbon dioxide saturation pressure (MPa) | 23.5 | 24.0 | 23.5 | 24.2 | 24.5 | 22.7 |
| Cell average pore diameter, microns | 75.7 | 259.0 | 32.5 | 28.7 | 27.4 | 640.7 |
| Whether more than 98% of the cell pores have a diameter in the range of 1-100 μm | Whether or not | Whether or not | Is that | Is that | Is that | Whether or not |
| Cell density, cell/cm3 | 108 | 107 | 1010 | 1010 | 1011 | 107 |
| Average retention length of glass fiber, micron | 206.4 | 210.2 | 197.1 | 156.4 | 243.7 | 284.6 |
| Tensile strength, MPa | 139 | 137 | 158 | 145 | 155 | 134 |
| Density, g/cm3 | 1.47 | 1.50 | 1.41 | 1.41 | 1.4 | 1.45 |
| Dielectric constant | 4.4 | 4.8 | 5.5 | 3.9 | 4.5 | 4.9 |
It can be seen from the comparative example 1/2/6 that the conventional foaming technique has a low cell density and a large cell diameter, and it is impossible to achieve the feature that 98% or more of the cell diameter is in the range of 1-100. mu.m, and the advantage of low dielectric constant is not achieved even when the glass fiber retention length is in the range of 190-220. mu.m.
As can be seen from comparative example 3, the conventional glass fiber cannot achieve the advantage of low dielectric constant.
From comparative example 4/5, it is clear that the technical effect of low dielectric is achieved only if both the microfoaming technique and the average retention length of the glass fibers are within the range of the present invention.
Claims (9)
1. The foaming polyphenylene sulfide composition is characterized by comprising the following components in parts by weight:
65 parts of polyphenylene sulfide resin;
20-40 parts of low-dielectric glass fiber;
in the foaming polyphenylene sulfide composition, more than 98 percent of the pore diameters are in the range of 1-100 microns, the average pore diameter is 20-40 microns, and the cell density is 109-1015Per cm3；
The average retention length of the low dielectric glass fiber in the resin matrix is 190-220 microns.
2. The foamed polyphenylene sulfide composition of claim 1, wherein the polyphenylene sulfide resin is a linear polyphenylene sulfide resin.
3. The foamed polyphenylene sulfide composition of claim 1, wherein the polyphenylene sulfide resin has a melt flow rate of 1800g/10min at 316 ℃ under 5 kg.
4. The foamed polyphenylene sulfide composition of claim 1, wherein the low dielectric glass fiber has a dielectric constant Dk of less than 4.5, as measured under test condition 1GHZ。
5. The foamed polyphenylene sulfide composition of claim 1, further comprising 0-2 parts by weight of an auxiliary agent, wherein the auxiliary agent comprises at least one of an antioxidant and a lubricant.
6. The foamed polyphenylene sulfide composition of claim 1, wherein the foamed polyphenylene sulfide composition is obtained by foaming with a physical blowing agent and/or foaming with a chemical blowing agent; the physical foaming agent is selected from at least one of compressed gas, soluble solid and volatile liquid with the boiling point lower than 110 ℃; the chemical foaming agent is selected from inorganic foaming agents and organic foaming agents, wherein the inorganic foaming agents are selected from at least one of carbonates, nitrites, potassium borohydride and sodium borohydride; the organic foaming agent is at least one selected from azo compounds, nitrite compounds and sulfonyl hydrazide compounds.
7. The foamed polyphenylene sulfide composition of claim 1, wherein the foamed polyphenylene sulfide composition has a dielectric constant Dk of 3.2 or less, as measured under test condition 1GHZ。
8. The preparation method of the foaming polyphenylene sulfide composition is characterized by comprising the following steps: according to the proportion, the polyphenylene sulfide resin is extruded by a double-screw extruder, the screw is divided into 10 sections, wherein low-dielectric glass fiber is fed from the side of 6 sections, foaming agent is fed from the side of 8 sections, the temperature range of a screw cylinder is 1-4 sections 285-295 ℃, 5-7 sections 290-300 ℃, 8-10 sections 275-285 ℃ and the rotating speed range is 300-500 rpm.
9. Use of the foamed polyphenylene sulfide composition according to any of claims 1-7 for the preparation of articles for high frequency electromagnetic wave applications.
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| JP2017088690A (en) * | 2015-11-06 | 2017-05-25 | 東ソー株式会社 | Polyarylene sulfide-based composition |
| US20200224030A1 (en) * | 2017-04-27 | 2020-07-16 | Byd Company Limited | Low-dielectric resin composition, low-dielectric resin/metal composite material and preparation method thereof, and electronic equipment |
| CN108250751A (en) * | 2018-02-07 | 2018-07-06 | 深圳华力兴新材料股份有限公司 | The NMT technologies polyphenyl thioether resin composition and preparation method of a kind of low-k |
| CN111423723A (en) * | 2020-04-14 | 2020-07-17 | 广东圆融新材料有限公司 | Reinforced polyphenylene sulfide composition for 5G and preparation method thereof |
| CN112552684A (en) * | 2020-11-16 | 2021-03-26 | 中广核俊尔(浙江)新材料有限公司 | Low-linear expansion coefficient polyphenylene sulfide composite material special for micro-arc oxidation and preparation and application thereof |
| CN112646297A (en) * | 2020-12-25 | 2021-04-13 | 深圳市兴东泰电子有限公司 | Low-dielectric-constant modified plastic casing pipe and preparation method thereof |
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