CN107022171A - Liquid-crystal polyester resin compound and preparation method and application - Google Patents
Liquid-crystal polyester resin compound and preparation method and application Download PDFInfo
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- CN107022171A CN107022171A CN201611253546.3A CN201611253546A CN107022171A CN 107022171 A CN107022171 A CN 107022171A CN 201611253546 A CN201611253546 A CN 201611253546A CN 107022171 A CN107022171 A CN 107022171A
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- 229920001225 polyester resin Polymers 0.000 title claims abstract description 125
- 239000004645 polyester resin Substances 0.000 title claims abstract description 125
- 239000004973 liquid crystal related substance Substances 0.000 title claims abstract description 121
- 150000001875 compounds Chemical class 0.000 title claims abstract description 58
- 238000002360 preparation method Methods 0.000 title claims abstract description 28
- 229920000049 Carbon (fiber) Polymers 0.000 claims abstract description 30
- 239000004917 carbon fiber Substances 0.000 claims abstract description 30
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000002041 carbon nanotube Substances 0.000 claims abstract description 23
- 238000000034 method Methods 0.000 claims abstract description 16
- 238000004519 manufacturing process Methods 0.000 claims abstract description 9
- 239000000945 filler Substances 0.000 claims abstract description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 31
- 239000002131 composite material Substances 0.000 claims description 30
- 125000003118 aryl group Chemical group 0.000 claims description 28
- 229910021393 carbon nanotube Inorganic materials 0.000 claims description 22
- 239000000178 monomer Substances 0.000 claims description 17
- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical compound O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 claims description 13
- 238000001125 extrusion Methods 0.000 claims description 13
- 238000006068 polycondensation reaction Methods 0.000 claims description 13
- 238000002156 mixing Methods 0.000 claims description 10
- 239000002994 raw material Substances 0.000 claims description 10
- UFWIBTONFRDIAS-UHFFFAOYSA-N Naphthalene Chemical compound C1=CC=CC2=CC=CC=C21 UFWIBTONFRDIAS-UHFFFAOYSA-N 0.000 claims description 8
- 229910052799 carbon Inorganic materials 0.000 claims description 8
- 125000000843 phenylene group Chemical group C1(=C(C=CC=C1)*)* 0.000 claims description 8
- 239000012345 acetylating agent Substances 0.000 claims description 7
- -1 aromatic diol Chemical class 0.000 claims description 7
- 229920000728 polyester Polymers 0.000 claims description 7
- 239000007790 solid phase Substances 0.000 claims description 7
- 150000001491 aromatic compounds Chemical class 0.000 claims description 6
- 239000003795 chemical substances by application Substances 0.000 claims description 5
- AVXURJPOCDRRFD-UHFFFAOYSA-N Hydroxylamine Chemical compound ON AVXURJPOCDRRFD-UHFFFAOYSA-N 0.000 claims description 4
- 150000004984 aromatic diamines Chemical class 0.000 claims description 4
- 125000002529 biphenylenyl group Chemical group C1(=CC=CC=2C3=CC=CC=C3C12)* 0.000 claims description 4
- KXDHJXZQYSOELW-UHFFFAOYSA-N Carbamic acid Chemical compound NC(O)=O KXDHJXZQYSOELW-UHFFFAOYSA-N 0.000 claims description 3
- OFOBLEOULBTSOW-UHFFFAOYSA-N Malonic acid Chemical compound OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 claims description 3
- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical compound OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 3
- 239000012856 weighed raw material Substances 0.000 claims description 3
- 238000005303 weighing Methods 0.000 claims description 3
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims 1
- 239000011324 bead Substances 0.000 claims 1
- 229910000019 calcium carbonate Inorganic materials 0.000 claims 1
- 239000004927 clay Substances 0.000 claims 1
- 229910052570 clay Inorganic materials 0.000 claims 1
- 239000011521 glass Substances 0.000 claims 1
- 239000003365 glass fiber Substances 0.000 claims 1
- 229910052739 hydrogen Inorganic materials 0.000 claims 1
- 239000001257 hydrogen Substances 0.000 claims 1
- 239000000155 melt Substances 0.000 claims 1
- 239000010445 mica Substances 0.000 claims 1
- 229910052618 mica group Inorganic materials 0.000 claims 1
- 239000000203 mixture Substances 0.000 claims 1
- 239000010456 wollastonite Substances 0.000 claims 1
- 229910052882 wollastonite Inorganic materials 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 11
- 239000011342 resin composition Substances 0.000 abstract 1
- WFDIJRYMOXRFFG-UHFFFAOYSA-N Acetic anhydride Chemical group CC(=O)OC(C)=O WFDIJRYMOXRFFG-UHFFFAOYSA-N 0.000 description 12
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 description 8
- QQVIHTHCMHWDBS-UHFFFAOYSA-N isophthalic acid Chemical compound OC(=O)C1=CC=CC(C(O)=O)=C1 QQVIHTHCMHWDBS-UHFFFAOYSA-N 0.000 description 8
- 239000000047 product Substances 0.000 description 8
- 229920005989 resin Polymers 0.000 description 8
- 239000011347 resin Substances 0.000 description 8
- 238000004898 kneading Methods 0.000 description 6
- 238000001816 cooling Methods 0.000 description 5
- 230000008569 process Effects 0.000 description 5
- 208000016261 weight loss Diseases 0.000 description 5
- 230000004580 weight loss Effects 0.000 description 5
- 229940090248 4-hydroxybenzoic acid Drugs 0.000 description 4
- 125000005274 4-hydroxybenzoic acid group Chemical group 0.000 description 4
- KAUQJMHLAFIZDU-UHFFFAOYSA-N 6-Hydroxy-2-naphthoic acid Chemical compound C1=C(O)C=CC2=CC(C(=O)O)=CC=C21 KAUQJMHLAFIZDU-UHFFFAOYSA-N 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- FJKROLUGYXJWQN-UHFFFAOYSA-N papa-hydroxy-benzoic acid Natural products OC(=O)C1=CC=C(O)C=C1 FJKROLUGYXJWQN-UHFFFAOYSA-N 0.000 description 4
- 238000012545 processing Methods 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 239000011159 matrix material Substances 0.000 description 3
- 229920000106 Liquid crystal polymer Polymers 0.000 description 2
- 239000004977 Liquid-crystal polymers (LCPs) Substances 0.000 description 2
- 230000000875 corresponding effect Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 239000000428 dust Substances 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000001746 injection moulding Methods 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000010926 purge Methods 0.000 description 2
- 230000009257 reactivity Effects 0.000 description 2
- 230000002195 synergetic effect Effects 0.000 description 2
- 230000021736 acetylation Effects 0.000 description 1
- 238000006640 acetylation reaction Methods 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000010292 electrical insulation Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 238000005469 granulation Methods 0.000 description 1
- 230000003179 granulation Effects 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000010137 moulding (plastic) Methods 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000000523 sample Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/22—Expanded, porous or hollow particles
- C08K7/24—Expanded, porous or hollow particles inorganic
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/02—Fibres or whiskers
- C08K7/04—Fibres or whiskers inorganic
- C08K7/06—Elements
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/20—Applications use in electrical or conductive gadgets
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses a kind of liquid-crystal polyester resin compound and its manufacture method and application.Liquid-crystal polyester resin compound of the present invention includes the component of following parts by weight：60 80 parts of liquid-crystal polyester resin, 15 35 parts of filler, 0 20 parts of carbon fiber, 05 parts of CNT.Liquid-crystal polyester resin compound of the present invention resin Composition based on liquid-crystal polyester resin is modified by components such as contained carbon fiber, CNTs to it, so as to which the surface resistivity for assigning liquid-crystal polyester resin compound of the present invention is low, there is excellent mechanical strength and processability simultaneously, its preparation method technique is easily-controllable, the material property of preparation is stable, effectively reduces its production cost.
Description
Technical Field
The invention belongs to the technical field of polymer composite materials, and particularly relates to a liquid crystal polyester resin compound and a preparation method and application thereof.
Background
Liquid Crystal Polyester (LCP) is widely used in the fields of electronics, electrical, automotive, aerospace, and the like because of its excellent flow properties, electrical insulation properties, heat resistance, dimensional stability, and the like. It can also be used for printed circuit boards, food packaging, electronic parts for artificial satellites, electronic electric and automobile parts, and even as materials for aerospace parts. In many fields of application of LCP, one of the most important and most widely used fields is as electronic and electrical parts, and LCP material can be used to make precision electronic parts due to its excellent flow property, heat resistance and dimensional stability, but liquid crystal polymer composite material has very high surface resistivity and is very easy to generate electric charge, and during plastic molding, foreign matters such as dust, powder and even fiber are adsorbed on the product due to electric charge to cause product appearance defects and surface smoothness to be reduced, thereby also causing mechanical strength and insulation performance of the product to be reduced.
Due to the above characteristics of the current liquid crystal polymer composite materials, in the electronic industry, electronic products made of the polyester composite material are very easy to accumulate charges during use and difficult to eliminate, and the charges of electronic parts are accumulated continuously, so that the charges not only attract dust, powder and other foreign matters in the air during use to reduce the performance of the parts, but also can cause circuit breakdown, damage of integrated circuits and component damage. Intermediate to the above drawbacks and problems.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a liquid crystal polyester resin compound, a preparation method and application thereof, so as to solve the technical problem that the performance of a prepared product, such as an electronic element, is reduced or even damaged due to the fact that the prior liquid crystal polyester resin is easy to accumulate charges due to high surface resistivity.
In order to achieve the above object, according to one aspect of the present invention, there is provided a liquid crystal polyester resin composite. The liquid crystal polyester resin compound comprises the following components in parts by weight:
wherein, the content of the carbon fiber and the carbon nano tube is not 0 at the same time.
In another aspect of the invention, a method for preparing the liquid crystal polyester resin compound is provided. The preparation method comprises the following steps:
weighing raw materials of the components according to the types and the contents of the components contained in the liquid crystal polyester resin compound;
and carrying out melt mixing extrusion treatment on the weighed raw materials of the components.
In another aspect of the embodiments of the present invention, there is provided an application of the liquid crystal polyester resin composite of the present invention or the liquid crystal polyester resin composite prepared by the preparation method of the present invention in an electronic component, an automobile part or an industrial structural member.
Compared with the prior art, the liquid crystal polyester resin compound takes the liquid crystal polyester resin as a basic resin component, and is modified by the contained components such as carbon fibers, carbon nanotubes and the like, so that the liquid crystal polyester resin compound has low surface resistivity, and simultaneously has excellent mechanical strength and processability.
According to the preparation method of the liquid crystal polyester resin compound, the components are directly subjected to melt mixing extrusion treatment according to the types and the proportions of the components contained in the liquid crystal polyester resin compound, so that the components can be fully dispersed and act with each other, the surface resistance of the extruded liquid crystal polyester resin compound is low, and the liquid crystal polyester resin compound is excellent in mechanical strength and processability. In addition, the preparation method has easily controlled process, the prepared material has stable performance, and the production cost is effectively reduced.
The liquid crystal polyester resin compound has the characteristics of low surface resistance, excellent mechanical strength, excellent processability and the like, so that the application range of the liquid crystal polyester resin compound is effectively expanded, and the liquid crystal polyester resin compound is particularly suitable for electronic element materials, and the quality and the working stability of corresponding products such as electronic elements are effectively improved.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The weight of the related components mentioned in the description of the embodiments of the present invention may not only refer to the specific content of each component, but also represent the proportional relationship of the weight among the components, and therefore, the content of the related components is scaled up or down within the scope disclosed in the description of the embodiments of the present invention as long as it is in accordance with the description of the embodiments of the present invention. Specifically, the weight described in the description of the embodiment of the present invention may be a unit of mass known in the chemical industry field, such as μ g, mg, g, and kg.
In one aspect, embodiments of the present invention provide a liquid crystal polyester resin composite. The liquid crystal polyester resin compound comprises the following components in parts by weight:
in this way, the liquid crystal polyester resin composite of the present embodiment uses the liquid crystal polyester resin as a base resin component, and is modified by the components such as the carbon fiber and the carbon nanotube contained therein, thereby providing the liquid crystal polyester resin composite of the present invention with low surface resistivity and excellent mechanical strength and processability.
Specifically, in the embodiment of the liquid crystal polyester resin composite, the liquid crystal polyester resin is a wholly aromatic liquid crystal polyester resin. In one embodiment, the wholly aromatic liquid crystal polyester resin has a number average molecular weight of 10000-. The resin molecular weight in this range can impart excellent flowability and processability to the composite. In one embodiment of the present invention, the wholly aromatic liquid crystalline polyester resin contains at least one of the following repeating units:
(1) repeating units derived from an aromatic diol: -O-Ar-O-;
(2) repeating units derived from an aromatic diamine: -HN-Ar-NH-;
(3) repeating units from aromatic hydroxylamine: -HN-Ar-O-;
(4) repeating units derived from aromatic dicarboxylic acids: -OC-Ar-CO-;
(5) repeating units derived from aromatic hydroxycarboxylic acids: -O-Ar-CO-;
(6) repeating units from aromatic aminocarboxylic acids: -HN-Ar-CO-.
Wherein the Ar group in the repeating units represented by (1) to (6) is any of phenylene, biphenylene, naphthalene, and an aromatic compound in which two phenylenes are bonded by an element other than carbon, or an aromatic compound in which one or more hydrogens of phenylene, biphenylene, naphthalene, and an aromatic compound in which two phenylenes are bonded by an element other than carbon are substituted with another element. The wholly aromatic liquid crystalline polyester resin produced from the structural unit monomer has excellent high temperature resistance, flowability and processability.
The liquid crystal polyester resin can be prepared by the following method:
the preparation method comprises the steps of firstly carrying out polycondensation reaction on a first monomer and a second monomer, and then carrying out solid-phase polycondensation reaction on a wholly aromatic liquid crystal polyester prepolymer synthesized by the polycondensation reaction.
Wherein the first monomer is at least one of a free aromatic diol, an aromatic diamine and an aromatic hydroxylamine, and the second monomer is at least one of an aromatic dicarboxylic acid, an aromatic hydroxycarboxylic acid and an aromatic aminocarboxylic acid. Specifically, the aromatic diol, aromatic diamine, aromatic hydroxylamine, aromatic dicarboxylic acid, aromatic hydroxycarboxylic acid, and aromatic aminocarboxylic acid may be, but are not limited to, those conventionally used.
In a further embodiment, the first monomer and/or the second monomer are pretreated with an acylating agent to improve reactivity before the polycondensation reaction. Specifically, the acylating agent is at least one of acetylating agents. Specifically, for example, when the acylating agent is an acetylating agent, the first monomer and/or the second monomer is pretreated to increase the reactivity of the first monomer and/or the second monomer for acetylation.
In the process of carrying out solid phase polycondensation on the wholly aromatic liquid crystal polyester prepolymer synthesized by the polycondensation, the molecular weight of the product is extracted by the solid phase polycondensation, and the liquid crystal polyester resin with proper molecular weight is obtained. The solid phase polycondensation reaction process requires heating treatment, and for example, heating plates, hot air, high temperature fluid, etc. can be used to provide heat energy for the solid phase polycondensation reaction. To remove the by-products of the solid phase polycondensation reaction, purging with an inert gas or purging with a vacuum may be used.
The filler contained in the liquid crystal polyester resin compound can exert a synergistic effect with the carbon fibers and the carbon nanotubes, acts on the matrix liquid crystal polyester resin, and effectively improves the mechanical property and the processing property of the liquid crystal polyester resin, so that the liquid crystal polyester resin compound is endowed with excellent mechanical property and functional performance.
The carbon fiber and the carbon nanotube are not contained in the same amount of 0. In one embodiment, the preferred content of the carbon fibers is 5-10 parts. In another embodiment, the carbon nanotubes are present in an amount of 1 to 5 parts, preferably 1 to 3 parts.
More preferably, the content of the carbon fiber and the content of the carbon nanotube are both not 0, so that the carbon fiber and the carbon nanotube are compounded, that is, the carbon material with the one-dimensional structure and the two-dimensional carbon structure are compounded, so that the carbon with the two structures are mutually interpenetrated, and a conductive network is formed on the matrix liquid crystal polyester resin, thereby obviously reducing the surface resistance of the liquid crystal polyester resin compound. Meanwhile, the carbon component and the filler are respectively in the matrix liquid crystal polyester resin, so that the mechanical property and the processing property of the liquid crystal polyester resin are effectively improved, and the liquid crystal polyester resin compound is endowed with excellent mechanical property and functional property.
In one embodiment, the carbon fiber of the carbon fiber preferably has the size of 7-10 μm of monofilament diameter, 2-5mm of length and volume resistivity less than or equal to 1.0 × 10-2Omega cm. in another embodiment, the carbon nano-tube preferably has a tube diameter of 5-30nm, a tube length of 10-100 μm, and a volume resistivity of 1.5 × 10-1Omega cm. Through the synergistic effect between the carbon fibers and the carbon nanotubes, the stability of the conductive network structure constructed by the carbon fibers and the carbon nanotubes is improved, and the surface resistivity of the liquid crystal polyester resin compound is reduced.
Therefore, the liquid crystal polyester resin composite of the present invention has low surface resistivity and excellent mechanical strength and processability due to the effect of the carbon fibers, the carbon nanotubes and the filler on the liquid crystal polyester resin as a base resin component.
In another aspect, embodiments of the present invention provide a method for preparing a liquid crystal polyester resin composite in the above embodiments. In one embodiment, the method for preparing the liquid crystal polyester resin compound comprises the following steps:
step S01: weighing the raw materials of the components according to the types and the contents of the components contained in the liquid crystal polyester resin compound;
step S02: and carrying out melt mixing extrusion treatment on the weighed raw materials of the components.
The contents and selected components of the components weighed in the step S01 are as described in the liquid crystal polyester resin composite, and are not repeated herein for the sake of brevity.
In the step S02, the raw materials of the components are sufficiently dispersed and acted upon each other by the high pressure and high heat of melt-kneading extrusion, so as to act upon the liquid crystal polyester resin, so that the liquid crystal polyester resin compound of the target product is obtained by melt-kneading extrusion, and the liquid crystal polyester resin compound has low surface resistivity and excellent mechanical and work-adding properties. In one embodiment, the melt-kneading extrusion temperature is 330-365 ℃, so that the components are fully and uniformly mixed and fully acted in a molten state, the surface resistivity of the liquid crystal polyester resin compound is reduced, and the mechanical property and the processing property of the liquid crystal polyester resin compound are improved.
In one embodiment, the melt-kneading extrusion may be performed by melt-kneading and extrusion processing using a twin-screw extruder, in which the raw materials are fed in a certain proportion, but not exclusively, using a weight-loss automatic feeder.
In addition, before the step S02, drying treatment is further included, such as drying at 160 ℃ for 4 hours at 130-.
After step S02, the method may further include the subsequent steps of drawing, cooling, and granulating the liquid crystal polyester resin composite produced by the melt-kneading extrusion process.
Therefore, in the method for preparing the liquid crystal polyester resin composite according to the embodiment of the invention, the components are directly subjected to melt mixing extrusion treatment according to the types and the proportions of the components contained in the liquid crystal polyester resin composite, so that the components can be fully dispersed and act with each other, the surface resistance of the extruded liquid crystal polyester resin composite is low, and the mechanical strength and the processability are excellent. In addition, the preparation method has easily controlled process, the prepared material has stable performance, and the production cost is effectively reduced.
Based on the liquid crystal polyester resin compound and the preparation method thereof, the liquid crystal polyester resin compound has the characteristics of low surface resistance, excellent mechanical strength, excellent processability and the like, so that the application range of the liquid crystal polyester resin compound is effectively expanded, and the liquid crystal polyester resin compound is particularly suitable for electronic element materials.
The liquid crystal polyester resin composite and the preparation method thereof will be described in detail with reference to specific examples.
Example 1
The embodiment provides a liquid crystal polyester resin compound and a preparation method thereof. The liquid crystal polyester resin compound comprises the following components in parts by weight and contents in table 1. Wherein,
the average molecular weight of the liquid crystal polyester resin is 50000, the size of the talcum powder is 300 meshes, the size of the carbon fiber is 4mm, and the volume resistivity is 1.0 × 10-3Omega cm, the size of the carbon nano tube is 5-15nm, the length of the tube is 30-0 μm, and the volume resistivity is (1.0-1.5) × 10-1Ω·cm。
The preparation method of the liquid crystal polyester resin compound comprises the following steps:
s11, preparation of liquid crystal polyester resin: the resin structural unit is p-hydroxybenzoic acid, terephthalic acid, biphenol, 6-hydroxy-2-naphthoic acid and isophthalic acid, and the acetylating agent is acetic anhydride;
s12, according to the weight parts in the example 1 in the table 1, 70 parts of selected liquid crystal polyester resin (wholly aromatic liquid crystal polyester resin, Jiangsu Wott special material manufacturing company, Ltd.), 20 parts of talcum powder, 10 parts of carbon fiber and 0 part of carbon nano tube are dried for 4 hours at 130 ℃;
s13, putting the liquid crystal polyester resin, the talcum powder and the carbon fiber dried in the step S12 into a weight-loss type feeder, and putting the raw materials into a double-screw extruder according to the formula ratio through the feeder? And (3) carrying out melt mixing at the temperature, and then carrying out extrusion, drawing, cooling and granulation to obtain the liquid crystal polyester resin compound.
Example 2
The embodiment provides a liquid crystal polyester resin compound and a preparation method thereof. The liquid crystal polyester resin compound comprises the following components in parts by weight and contents in table 1. Wherein,
the average molecular weight of the liquid crystal polyester resin is 50000, the size of the talcum powder is 300 meshes, the size of the carbon fiber is 4mm, and the volume resistivity is 1.0 × 10-3Ω·cm。
The preparation method of the liquid crystal polyester resin compound comprises the following steps:
s21, preparing liquid crystal polyester resin: the resin structural unit is p-hydroxybenzoic acid, terephthalic acid, biphenol, 6-hydroxy-2-naphthoic acid and isophthalic acid, and the acetylating agent is acetic anhydride;
s22, according to the weight parts in the example 2 in the table 1, 70 parts of selected liquid crystal polyester resin (wholly aromatic liquid crystal polyester resin, Jiangsu Wott special material manufacturing company, Ltd.), 25 parts of talcum powder, 5 parts of carbon fiber and 0 part of carbon nano tube are dried for 4 hours at 130 ℃;
s23, feeding the liquid crystal polyester resin, the talcum powder and the carbon fiber dried in the step S22 into a weight-loss type feeder, feeding the raw materials into a double-screw extruder according to the formula proportion through the feeder, carrying out melt mixing at 355 ℃, then extruding, bracing, cooling and granulating to obtain the liquid crystal polyester resin compound.
Example 3
The embodiment provides a liquid crystal polyester resin compound and a preparation method thereof. The liquid crystal polyester resin compound comprises the following components in parts by weight and contents in table 1. Wherein,
the average molecular weight of the liquid crystal polyester resin is 50000, the size of the talcum powder is 300 meshes, the size of the carbon fiber is 4mm, and the volume resistivity is 1.0 × 10-3Omega cm, the size of the carbon nano tube is 5-15nm, the length of the tube is 30-0 μm, and the volume resistivity is (1.0-1.5) × 10-1Ω·cm。
The preparation method of the liquid crystal polyester resin compound comprises the following steps:
s31, preparation of liquid crystal polyester resin: the resin structural unit is p-hydroxybenzoic acid, terephthalic acid, biphenol, 6-hydroxy-2-naphthoic acid and isophthalic acid, and the acetylating agent is acetic anhydride;
s32, according to the weight parts in the example 3 in the table 1, 69 parts of selected liquid crystal polyester resin (wholly aromatic liquid crystal polyester resin, JiangsuWott special material manufacturing company, Ltd.), 25 parts of talcum powder, 5 parts of carbon fiber and 1 part of carbon nano tube are dried for 4 hours at 130 ℃;
s33, putting the liquid crystal polyester resin, the talcum powder and the carbon fiber dried in the step S32 into a weight-loss type feeder, putting the raw materials into a double-screw extruder according to the formula proportion through the feeder, carrying out melt mixing at 355 ℃, then extruding, bracing, cooling and granulating to obtain the liquid crystal polyester resin compound.
Example 4
The embodiment provides a liquid crystal polyester resin compound and a preparation method thereof. The liquid crystal polyester resin compound comprises the following components in parts by weight and contents in table 1. Wherein,
the average molecular weight of the liquid crystal polyester resin is 50000, the size of the talcum powder is 300 meshes, the size of the carbon fiber is 4mm, and the volume resistivity is 1.0 × 10-3Omega cm, the size of the carbon nano tube is 5-15nm, the length of the tube is 30-0 μm, and the volume resistivity is (1.0-1.5) × 10-1Ω·cm。
The preparation method of the liquid crystal polyester resin compound comprises the following steps:
s41, preparation of liquid crystal polyester resin: the resin structural unit is p-hydroxybenzoic acid, terephthalic acid, biphenol, 6-hydroxy-2-naphthoic acid and isophthalic acid, and the acetylating agent is acetic anhydride;
s42, according to the weight parts in the example 4 in the table 1, 68 parts of selected liquid crystal polyester resin (wholly aromatic liquid crystal polyester resin, JiangsuWott special material manufacturing company, Ltd.), 25 parts of talcum powder, 5 parts of carbon fiber and 2 parts of carbon nano tube are dried for 4 hours at 130 ℃;
s43, feeding the liquid crystal polyester resin, the talcum powder and the carbon fiber dried in the step S42 into a weight-loss type feeder, feeding the raw materials into a double-screw extruder according to the formula proportion through the feeder, carrying out melt mixing at 355 ℃, then extruding, bracing, cooling and granulating to obtain the liquid crystal polyester resin compound.
Comparative example 1
Provided is a liquid crystal polyester resin composite, which comprises the following components in parts by weight and contents in Table 1. The preparation method refers to the preparation method of example 1.
Testing of corresponding Properties
The liquid crystal polyester resin compounds provided in examples 1 to 4 and the liquid crystal polyester resin compound provided in comparative example 1 were respectively used as injection molding raw materials, injection-molded using an injection molding machine, and then subjected to performance tests by the following test standards, respectively, and the test results are shown in the following table 2:
(1) bending strength: testing was performed according to ASTM D-790.
(2) Surface resistivity: the surface resistivity of the liquid crystal polyester compound is measured by adopting a four-probe method, wherein the environmental temperature is 20 ℃, and the humidity is 40%.
TABLE 1
TABLE 2
| Performance index | Comparative example 1 | Example 1 | Example 2 | Example 3 | Example 4 |
| Surface resistivity (omega) | 1×1020 | 3×109 | 5×1012 | 1×109 | 4×106 |
| Flexural Strength (MPa) | 120 | 183 | 165 | 166 | 123 |
Referring to table 2 above, examples 1 to 4 have excellent characteristics of low apparent resistivity and high mechanical strength as compared with the liquid crystal polyester resin composite manufactured in comparative example 1.
The principle and embodiments of the present invention are explained herein by using specific embodiments, the description of the embodiments is only for the purpose of facilitating understanding of the method and the core concept of the present invention, the above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. The liquid crystal polyester resin compound is characterized by comprising the following components in parts by weight:
wherein, the content of the carbon fiber and the carbon nano tube is not 0 at the same time.
2. The liquid-crystalline polyester resin composite according to claim 1, wherein: the diameter of the carbon fiber monofilament is 7-10 mu m, and the length of the carbon fiber monofilament is 2-5 mm; and/or
The diameter of the carbon nano tube is 5-30nm, and the length of the carbon nano tube is 10-100 mu m; and/or
The filler is one or a mixture of more than two of glass fiber, talcum powder, mica, wollastonite, calcium carbonate, clay and glass beads.
3. The liquid-crystalline polyester resin composite according to claim 1 or 2, wherein: the liquid crystal polyester resin is wholly aromatic liquid crystal polyester resin, and the number average molecular weight of the wholly aromatic liquid crystal polyester resin is 10000-100000.
4. The liquid crystalline polyester resin composite of claim 3, wherein: the wholly aromatic liquid crystal polyester resin contains at least one of the following repeating units:
-O-Ar-O-、-HN-Ar-NH-、-HN-Ar-O-、-OC-Ar-CO-、-O-Ar-CO-、-HN-Ar-CO-；
and the Ar group in the repeating unit is any one of phenylene, biphenylene, naphthalene and aromatic compounds in which two phenylenes are bonded by carbon or non-carbon elements, or aromatic compounds in which more than one hydrogen in the phenylene, biphenylene, naphthalene and aromatic compounds in which two phenylenes are bonded by carbon or non-carbon elements is replaced by other elements.
5. The liquid-crystalline polyester resin composite according to any one of claims 3 to 4, wherein: the wholly aromatic liquid crystal polyester prepolymer is prepared by carrying out polycondensation reaction on a first monomer and a second monomer, and then carrying out solid-phase polycondensation reaction on the wholly aromatic liquid crystal polyester prepolymer synthesized by the polycondensation reaction; wherein the first monomer is at least one of a free aromatic diol, an aromatic diamine and an aromatic hydroxylamine, and the second monomer is at least one of an aromatic dicarboxylic acid, an aromatic hydroxycarboxylic acid and an aromatic aminocarboxylic acid.
6. The liquid-crystalline polyester resin composite according to claim 5, wherein: the first monomer and/or the second monomer are pre-treated with an acylating agent.
7. The liquid-crystalline polyester resin composite of claim 6, wherein: the acylating agent is at least one of acetylating agents.
8. A preparation method of a liquid crystal polyester resin compound comprises the following steps:
weighing the raw materials of the components according to the component types and contents contained in the liquid crystal polyester resin compound of any one of claims 1 to 7;
and carrying out melt mixing extrusion treatment on the weighed raw materials of the components.
9. The method of claim 8, wherein: the temperature of the melt mixing extrusion treatment is 330-365 ℃.
10. Use of the liquid-crystalline polyester resin composite according to any one of claims 1 to 7 or the liquid-crystalline polyester resin composite produced by the production method according to any one of claims 8 to 9 in electronic components, automobile parts or industrial members.
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