CN108148433A - A kind of low warpage high temperature resistant conduction liquid crystal polyester composite and preparation method thereof - Google Patents
A kind of low warpage high temperature resistant conduction liquid crystal polyester composite and preparation method thereof Download PDFInfo
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- CN108148433A CN108148433A CN201711430967.3A CN201711430967A CN108148433A CN 108148433 A CN108148433 A CN 108148433A CN 201711430967 A CN201711430967 A CN 201711430967A CN 108148433 A CN108148433 A CN 108148433A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L101/00—Compositions of unspecified macromolecular compounds
- C08L101/12—Compositions of unspecified macromolecular compounds characterised by physical features, e.g. anisotropy, viscosity or electrical conductivity
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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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
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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
- C08K7/02—Fibres or whiskers
- C08K7/04—Fibres or whiskers inorganic
- C08K7/06—Elements
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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
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/003—Additives being defined by their diameter
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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
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/004—Additives being defined by their length
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
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- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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Abstract
The invention discloses a kind of low warpage high temperature resistant conduction liquid crystal polyester composite and preparation method thereof, composite material includes high temperature resistant liquid-crystal polyester resin, carbon fiber and sheet inorganic mineral filler, wherein, high temperature resistant liquid crystal polymer resin (LCP)：50~60 parts by weight %, carbon fiber：40~50 parts by weight % of total loading of 15~28 parts by weight %, 18~28 parts by weight % of sheet inorganic mineral, carbon fiber and sheet inorganic mineral filler.The advantages that high temperature resistant conduction liquid crystal polyester composite of the present invention has high temperature resistant, and high abrasion, high-modulus, buckling deformation is small, good stability of the dimension, conductive, high rigidity.
Description
Technical field
The invention belongs to polymer composites, specifically, are related to a kind of low warpage high temperature resistant conduction liquid crystal polyester and answer
Condensation material and preparation method thereof.It is more particularly related to liquid crystal polyester composite material be by by carbon fiber, lamella
What shape inorganic mineral was mixed with high temperature resistant liquid crystal polyester.
Background technology
Carbon fiber has many excellent performances, and the axial strength and modulus of carbon fiber are high, and density is low, higher than performance, without compacted
Become, superhigh temperature resistant under non-oxidizing atmosphere, fatigue durability is good, specific heat and electric conductivity between nonmetallic between metal, thermal expansion system
Number is small and with anisotropy, good corrosion resistance.Purposes is very extensive, such as manufacture rocket, spaceship important materials；Manufacture
Jet engine；Manufacture corrosion-resistant chemical industry equipment etc..
Liquid crystal polyester has low chemical resistance, low-expansion coefficient, shrinking percentage, high fluidity, high-fire resistance, high dielectric
The characteristics such as intensity and high-insulativity.The liquid crystal polyester used as moulding material can provide accurate mechanograph, it can be used in
Various fields including Electrical and Electronic field.In order to prevent short circuit phenomenon, Electrical and Electronic field makes under normal conditions
The requirement insulation of liquid crystal polyester composite material.But at some in special circumstances, then need electric power connector that there is good lead
Electrical property.Therefore, as a kind of material with superior electrical conductivity energy, carbon fiber is often added in liquid crystal polyester, with system
The composite material of the electric power connector of excellent, the plastic complicated shape of standby electric conductivity.
However under certain harsh applied at elevated temperature environment, common liquid crystal polyester heat resistance is insufficient, during leading to use,
Connector temperature distortion, leads to product failure.And for certain especially accurate connectors, on the one hand require connector
Heat resistance is good, and connector is on the other hand required to have low-down angularity after crossing Reflow Soldering.Patent CN1330688C is studied
The heat resistance of carbon fiber that liquid crystal polyester is modified from different surface of polyester, but its upper limit temperature of heat tolerance is 280 DEG C, is not also led
The research of electrical property.Patent CN1247703 has studied liquid crystal polyester and adds the electric conductivity after a variety of conductive fillers, but it is conductive
Ranging from 104~1011Ω does not make a search to larger range of electric conductivity, to the resistance to heat problem of carbon fiber and liquid crystal polyester
It is not directed to.More than patent does not do correlative study to the warpage performance of high temperature resistant conducing composite material.
Invention content
Technical to solve the problems, such as, the object of the present invention is to provide a kind of low warpage high temperature resistant conduction liquid crystal polyester is compound
Material has high temperature resistant, and high abrasion, high-modulus, low warpage, good stability of the dimension are conductive, and the liquid crystal polymer of high rigidity is compound
Material.
The purpose of the present invention is be achieved through the following technical solutions.
A kind of low warpage high temperature resistant conduction liquid crystal polyester composite, composite material include high temperature resistant liquid-crystal polyester resin,
Carbon fiber and sheet inorganic mineral filler, wherein, high temperature resistant liquid crystal polymer resin (LCP)：50~60 parts by weight %, carbon
Fiber：15~28 parts by weight %, 18~28 parts by weight % of sheet inorganic mineral, carbon fiber and sheet inorganic mineral filler
40~50 parts by weight % of total loading.
Carbon composition selects the works such as polyacrylonitrile, pitch, regenerated cellulose usually more than 93% in the carbon fiber
For raw material.These raw fibres carry out carbonization treatment or at 2000~3000 DEG C at graphite first at 1000~2000 DEG C
Then reason activates surface is by such as anodic oxidation the methods of, finally obtains workable carbon fiber.
The number average fiber length of carbon fiber is preferably 30-1000 μm.When number average fiber length is less than 30 μm, the effect of enhancing
Fruit will reduce.When number average fiber length is more than 1000 μm, during granulation, discharging can become unstable, product
Surface is also more crude.Carbon fiber used is high conductivity carbon fiber in the present invention, 1~100*10 of volume resistivity-4Ω·
cm。
The sheet inorganic filler includes talcum, mica, kaolin, clay, calcium silicates, alumina silicate, feldspar powder, acid
The silicates such as property carclazyte, talc clay, sericite, sillimanite, bentonite, sheet glass, slate powder, silane, calcium carbonate, chalk,
The carbonate such as barium carbonate, magnesium carbonate, dolomite, the sulfate such as blanc fixe, settleability calcium sulfate, the plaster of paris, barium sulfate, water and
The hydroxide of aluminium oxide etc., aluminium oxide, antimony oxide, magnesia, titanium dioxide, zinc white, silica, silica sand, quartz, white carbon,
The materials such as the oxides such as diatomite, molybdenum disulfide sulfides, the wollastonite of plate, metal powder plastochondria.
The sheet inorganic filler preferably talc, mica, kaolin, graphite, sheet glass, particularly preferred talcum,
Average particle diameter size is 0.5~200 μm.
In this patent, the ratio of carbon fiber and sheet inorganic mineral filler is very crucial, the carbon in composition
Total loading of fiber and sheet inorganic mineral filler is 40~50 parts by weight %.When total loading is less than 40 parts by weight %
When, no matter how carbon fiber and sheet inorganic mineral filler are combined, low warpage properties, mechanical strength, mobility, electric conductivity are difficult
To meet simultaneously.In addition, when total loading is more than 50 parts by weight %, material becomes too crisp.The content of carbon fiber is 15~30 weights
Part % is measured, the content of sheet inorganic mineral filler is 15~30 parts by weight %.
When the content of fibrous filler in the carbon fibers is higher than 30 parts by weight %, the mobility of material is deteriorated, reflux
Warpage increase during weldering.On the other hand, when the content is less than 15 parts by weight %, the content of carbon fiber is very little, and conductive effect is too
Difference..
In addition, though sheet inorganic mineral filler is effective for improving low warpage properties, but it is more than 30 in content
During parts by weight %, material becomes too crisp.On the other hand, when content is less than 15 parts by weight %, the improvement very little of low warpage properties.
Can one or more general additives, example be added in the liquid crystal polyester composite material of the present invention as required
Such as：Colorant such as dyestuff, pigment etc.；Antioxidant；Heat stabilizer；Ultraviolet absorber；Antistatic agent；Surfactant etc..
295~315 DEG C of HDT (1.82MPa) temperature range of the low warpage high temperature resistant conduction liquid crystal polyester composite,
Surface resistivity ranging from 101~1012Ohms, the addition of sheet inorganic mineral can significantly reduce angularity.
The preparation method of above-mentioned low warpage high temperature resistant conduction liquid crystal polyester composite, includes the following steps：All raw materials
By Weightlessness balance metering feeding, through double screw extruder, it is granulated through double-screw extruding pelletizing machine at a temperature of 340~380 DEG C to obtain the final product
High temperature resistant conduction liquid crystal polyester composite.The liquid crystal that isotropic melt is formed at 340-380 DEG C of preferred molten temperature gathers
Ester, the temperature range of HDT (under the conditions of 1.82MPa) is 260~295 DEG C.
High temperature resistant conduction liquid crystal polyester composite of the present invention has high temperature resistant, and high abrasion, high-modulus, buckling deformation is small,
The advantages that good stability of the dimension, conduction, high rigidity.
Specific embodiment
The invention is further illustrated by the following examples.The embodiment of the present invention includes but not limited to following embodiment party
Case.In these embodiments, parameter measures as follows.
1) tensile strength uses ASTM Type I dumbbells, and tensile strength is measured according to ASTM D638.
2) izod impact strength (notch) batten size is 64 × 12.7 × 3.2mm, and Yi Zuo is measured according to ASTM D256
Moral impact strength.
3) flexing resistance uses the bend test item of 127 × 12.7 × 3.2mm.Flexing resistance is tested according to ASTM D790.
4) deflection temperature of liquid crystal polyester uses the sample of 127 × 12.7 × 6.4mm, according to ASTM D648 in 1.82MPa
Load under measure deflection under load temperature.
5) the deflection under load temperature of composite material uses the sample of 127 × 12.7 × 6.4mm, is existed according to ASTM D648
Deflection under load temperature is measured under the load of 1.82MPa.
6) fusing point test uses differential scanning calorimeter DSC 8000 (PerkinElmer Inc, USA).With 20 DEG C/min
Rate heating sample and record endothermic peak (Tm 1).Thereafter, by liquid-crystal polyester resin sample in 20 DEG C of the temperature higher than Tm 1
Degree is lower to be kept for 5 minutes.Then sample is cooled to 200 DEG C with 10 DEG C/min of rate, then added again at the same rate
Heat.The endothermic peak found in final step is recorded as fusing point Tm.
7) melt viscosity is measured using RH2200 (Malvern Instruments Ltd., Britain), it uses spray
The a diameter of 0.5mm of mouth and the mold that nozzle length is 10mm.At a temperature of Tm+20 DEG C and shear rate be 1000S-1 item
Melt viscosity is measured under part.
8) sheet resistance is using the digital four probe assays instrument of the double electrical measurements of ST2263 types, the test of 4990 sheet resistances of QUICK
Instrument is measured.
9) composite material is molded into 1.0mm thickness, length of side 100*100mm square exemplars are stuck up according to national standard measurement
Curvature.
Liquid crystal polyester raw material selects our company volume production product, according to the method system described in US2011233462A1 patents
It is standby.The fusing point and viscosity number of resin are as shown in the table.
Table 1
| LCP | |
| Tm/℃ | 351 |
| Viscosity/PaS | 23 |
| HDT/℃ | 293 |
Embodiment 1
By the carbon fiber of 60 parts by weight LCP, 15 parts by weight, (CT70P006-PUY is manufactured by Toho, number average fiber length：
6mm, number average fiber diameter：6 μm, similarly hereinafter), 25 parts by weight talcum powder (HM4, Imifabi are manufactured, 1250 mesh) in the mixed machine of rolling into
Row mixing, then, which is granulated to obtain being gathered by liquid crystal with double screw extruder under 355 DEG C of barrel zone temperature
The pellet of ester resin composition composition.Obtained pellet is by NEX110T types injection (mo(u)lding) machine (by Nissei Plastic
Industrial Co., ltd manufacture) it is injection moulded under 365 DEG C of barrel zone temperatures and 120 DEG C of mold temperature.As a result
It is listed in Table 2 below.
Embodiment 2
By the carbon fiber of 60 parts by weight LCP, 20 parts by weight, (CT70P006-PUY is manufactured by Toho, number average fiber length：
6mm, number average fiber diameter：6 μm, similarly hereinafter), 20 parts by weight talcum powder (HM4, Imifabi are manufactured, 1250 mesh) in the mixed machine of rolling into
Row mixing, then, which is granulated to obtain being gathered by liquid crystal with double screw extruder under 355 DEG C of barrel zone temperature
The pellet of ester resin composition composition.Obtained pellet is by NEX110T types injection (mo(u)lding) machine (by Nissei Plastic
Industrial Co., ltd manufacture) it is injection moulded under 365 DEG C of barrel zone temperatures and 120 DEG C of mold temperature.As a result
It is listed in Table 2 below.
Embodiment 3
By the carbon fiber of 55 parts by weight LCP, 20 parts by weight, (CT70P006-PUY is manufactured by Toho, number average fiber length：
6mm, number average fiber diameter：6 μm, similarly hereinafter), 25 parts by weight talcum powder (HM4, Imifabi are manufactured, 1250 mesh) in the mixed machine of rolling into
Row mixing, then, which is granulated to obtain being gathered by liquid crystal with double screw extruder under 355 DEG C of barrel zone temperature
The pellet of ester resin composition composition.Obtained pellet is by NEX110T types injection (mo(u)lding) machine (by Nissei Plastic
Industrial Co., ltd manufacture) it is injection moulded under 365 DEG C of barrel zone temperatures and 120 DEG C of mold temperature.As a result
It is listed in Table 2 below.
Embodiment 4
By 55 parts by weight LCP, the carbon fiber CT70P006-PUY of 25 parts by weight, manufactured by Toho, number average fiber length：
6mm, number average fiber diameter：6 μm, similarly hereinafter), 20 parts by weight talcum powder (HM4, Imifabi are manufactured, 1250 mesh) in the mixed machine of rolling into
Row mixing, then, which is granulated to obtain being gathered by liquid crystal with double screw extruder under 355 DEG C of barrel zone temperature
The pellet of ester resin composition composition.Obtained pellet is by NEX110T types injection (mo(u)lding) machine (by Nissei Plastic
Industrial Co., ltd manufacture) it is injection moulded under 365 DEG C of barrel zone temperatures and 120 DEG C of mold temperature.As a result
It is listed in Table 2 below.
Comparative example 1
By 60 parts by weight LCP, the carbon fiber CT70P006-PUY of 10 parts by weight, manufactured by Toho, number average fiber length：
6mm, number average fiber diameter：6 μm, similarly hereinafter), 30 parts by weight talcum powder (HM4, Imifabi are manufactured, 1250 mesh) in the mixed machine of rolling into
Row mixing, then, the mixture are granulated with double screw extruder under 355 DEG C of barrel zone temperature to obtain one by liquid crystal
The pellet of polyester and resin composition composition.Obtained pellet is by NEX110T types injection (mo(u)lding) machine (by Nissei Plastic
Industrial Co., ltd manufacture) it is injection moulded under 365 DEG C of barrel zone temperatures and 120 DEG C of mold temperature.As a result
It is listed in Table 2 below.
Comparative example 2
By 65 parts by weight LCP, the carbon fiber CT70P006-PUY of 10 parts by weight, manufactured by Toho, number average fiber length：
6mm, number average fiber diameter：6 μm, similarly hereinafter), 25 parts by weight talcum powder (HM4, Imifabi are manufactured, 1250 mesh) in the mixed machine of rolling into
Row mixing, then, the mixture are granulated with double screw extruder under 355 DEG C of barrel zone temperature to obtain one by liquid crystal
The pellet of polyester and resin composition composition.Obtained pellet is by NEX110T types injection (mo(u)lding) machine (by Nissei Plastic
Industrial Co., ltd manufacture) it is injection moulded under 365 DEG C of barrel zone temperatures and 120 DEG C of mold temperature.As a result
It is listed in Table 2 below.
Comparative example 3
By 45 parts by weight LCP, the carbon fiber CT70P006-PUY of 15 parts by weight, manufactured by Toho, number average fiber length：
6mm, number average fiber diameter：6 μm, similarly hereinafter), 30 parts by weight talcum powder (HM4, Imifabi are manufactured, 1250 mesh) in the mixed machine of rolling into
Row mixing, then, the mixture are granulated with double screw extruder under 355 DEG C of barrel zone temperature to obtain one by liquid crystal
The pellet of polyester and resin composition composition.Obtained pellet is by NEX110T types injection (mo(u)lding) machine (by Nissei Plastic
Industrial Co., ltd manufacture) it is injection moulded under 365 DEG C of barrel zone temperatures and 120 DEG C of mold temperature.As a result
It is listed in Table 2 below.
Table 2
As shown in table 2, embodiment all has good electric conductivity, low angularity, high mechanical strength and high heat
Deformation temperature.In comparative example, when carbon fiber content is less than 15% parts by weight, conductivity of composite material can be poor；When component carbon fibre
When the total content of peacekeeping sheet inorganic mineral filler is less than 40%, the angularity of composite material is not low enough, and total content is higher than
During 50% parts by weight, the impact property of composite material is poor.
Claims (10)
1. a kind of low warpage high temperature resistant conduction liquid crystal polyester composite, it is characterised in that：Composite material includes high temperature resistant liquid crystal
Polyester resin, carbon fiber and sheet inorganic mineral filler, wherein, high temperature resistant liquid crystal polymer resin (LCP)：50~60 weights
Measure part %, carbon fiber：15~28 parts by weight %, 18~28 parts by weight % of sheet inorganic mineral, carbon fiber and sheet are inorganic
40~50 parts by weight % of total loading of mineral filler.
2. a kind of low warpage high temperature resistant conduction liquid crystal polyester composite according to claim 1, it is characterised in that：It is described
Carbon composition selects polyacrylonitrile, pitch, regenerated cellulose is as raw material more than 93% in carbon fiber.
3. a kind of low warpage high temperature resistant conduction liquid crystal polyester composite according to claim 1, it is characterised in that：It is described
Carbon fiber carries out carbonization treatment or the graphite treatment at 2000~3000 DEG C first at 1000~2000 DEG C, then leads on surface
The methods of crossing such as anodic oxidation activates, and finally obtains workable carbon fiber.
4. a kind of low warpage high temperature resistant conduction liquid crystal polyester composite according to claim 1, it is characterised in that：It is described
The number average fiber length of carbon fiber is 30-1000 μm；Its volume resistivity 1~100 × 10-4Ω·cm。
5. a kind of low warpage high temperature resistant conduction liquid crystal polyester composite according to claim 1, it is characterised in that：It is described
Sheet inorganic filler include silicate, carbonate, sulfate, hydroxide, oxide, sulfide, plate wollastonite
At least one of with metal powder plastochondria.
6. a kind of low warpage high temperature resistant conduction liquid crystal polyester composite according to claim 5, it is characterised in that：It is described
Silicate be selected from talcum, mica, kaolin, clay, calcium silicates, alumina silicate, feldspar powder, Emathlite, talc clay, thin,tough silk cloud
Mother, sillimanite, bentonite, sheet glass, slate powder, silane；The carbonate is selected from calcium carbonate, chalk, barium carbonate, carbonic acid
Magnesium, dolomite；The sulfate is selected from blanc fixe, settleability calcium sulfate, the plaster of paris, barium sulfate；The hydroxide
Selected from water and aluminium oxide；The oxide be selected from aluminium oxide, antimony oxide, magnesia, titanium dioxide, zinc white, silica, silica sand,
Quartz, white carbon, diatomite；The sulfide is selected from molybdenum disulfide.
7. a kind of low warpage high temperature resistant conduction liquid crystal polyester composite according to claim 6, it is characterised in that：It is described
Sheet inorganic filler be selected from talcum, mica, kaolin, graphite, sheet glass, average particle diameter size be 0.5~200 μm.
8. a kind of low warpage high temperature resistant conduction liquid crystal polyester composite according to claim 1, it is characterised in that：May be used also
Including one or more additives, the additive is selected from colorant；Antioxidant；Heat stabilizer；Ultraviolet absorber；It is antistatic
Agent；Surfactant.
9. a kind of low warpage high temperature resistant conduction liquid crystal polyester composite according to claim 1, it is characterised in that：It is described
295~315 DEG C of the HDT temperature ranges of low warpage high temperature resistant conduction liquid crystal polyester composite, surface resistivity ranging from 101~
1012Ohms, the addition of sheet inorganic mineral can significantly reduce angularity.
10. the preparation method of one of the arbitrary low warpage high temperature resistant conduction liquid crystal polyester composites of claim 1-9, special
Sign is：Include the following steps：All raw materials are by Weightlessness balance metering feeding, through double screw extruder, in 340~380 DEG C of temperature
It is lower to be granulated through double-screw extruding pelletizing machine up to high temperature resistant conduction liquid crystal polyester composite.
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