KR101743301B1 - Wholly Aromatic Liquid Crystalline Polyester Resin Composition with Excellent Blister Resistant - Google Patents
Wholly Aromatic Liquid Crystalline Polyester Resin Composition with Excellent Blister Resistant Download PDFInfo
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- KR101743301B1 KR101743301B1 KR1020110112179A KR20110112179A KR101743301B1 KR 101743301 B1 KR101743301 B1 KR 101743301B1 KR 1020110112179 A KR1020110112179 A KR 1020110112179A KR 20110112179 A KR20110112179 A KR 20110112179A KR 101743301 B1 KR101743301 B1 KR 101743301B1
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- wholly aromatic
- polyester resin
- aromatic liquid
- crystalline polyester
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K19/00—Liquid crystal materials
- C09K19/04—Liquid crystal materials characterised by the chemical structure of the liquid crystal components, e.g. by a specific unit
- C09K19/38—Polymers
- C09K19/3804—Polymers with mesogenic groups in the main chain
- C09K19/3809—Polyesters; Polyester derivatives, e.g. polyamides
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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
- C08K3/01—Use of inorganic substances as compounding ingredients characterized by their specific function
- C08K3/013—Fillers, pigments or reinforcing additives
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- Organic Chemistry (AREA)
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- Chemical Kinetics & Catalysis (AREA)
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- Crystallography & Structural Chemistry (AREA)
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Abstract
The present invention relates to a wholly aromatic liquid-crystalline polyester resin composition improved in blister resistance, said composition comprising a wholly aromatic liquid-crystalline polyester resin having a melting point of 300 to 450 ° C; Fillers for reinforcing physical properties; And an inorganic filler in the form of a powder, to have excellent blister resistance without deteriorating heat resistance and mechanical properties.
Description
The present invention relates to a wholly aromatic liquid-crystalline polyester resin composition improved in blister resistance. More specifically, the present invention relates to a wholly aromatic liquid-crystalline polyester resin composition improved in blister resistance without deteriorating heat resistance and mechanical properties.
The wholly aromatic liquid-crystalline polyester resin is excellent in heat resistance and dimensional stability and has excellent fluidity in melting, and is widely used as a precision injection molding material mainly in the field of electronic parts.
In particular, the wholly aromatic liquid-crystal polyester reinforced with various fillers has high heat resistance and excellent dimensional stability, electrical insulation and mechanical properties, so that it can be used as a material for electronic parts, connectors and other memory card sockets requiring high heat resistance. The use thereof has been expanded.
The wholly aromatic liquid-crystalline polyester resin is a kind of thermoplastic polymer produced by condensation polymerization, which is kneaded with an inorganic filler such as glass fiber or talc and extruded to produce a resin compound. The resin compound thus produced is injection- And can be processed into a product through a process.
In recent years, there has been a growing demand for wholly aromatic polyester resin compounds having improved heat resistance and blister resistance according to the tendency of thinning, miniaturization and weight reduction of electronic parts.
In addition, complex properties are required for the development of connectors for electronic products and memory card socket products to which the resin compound is applied. Therefore, the wholly aromatic liquid crystal polyester resin compound used as the material of the parts should also have high heat resistance while maintaining the existing properties.
However, in the case of a resin compound prepared by filling only glass fiber for high heat resistance among the wholly aromatic liquid crystalline polyester resin compound, moisture or volatile substance contained in the resin compound during high temperature processing such as heat treatment or soldering near the melting point A blister phenomenon occurs which expands and ejects through the surface. If such a blister phenomenon occurs, there is a problem that the appearance defects and mechanical properties of the molded article are deteriorated, making them unsuitable as parts materials for electronic products.
Accordingly, an object of the present invention is to provide a wholly aromatic liquid-crystalline polyester resin composition improved in blister resistance without deteriorating heat resistance and mechanical properties so as to be usable as a component material for connectors and memory card sockets.
In order to solve the above problems, the present invention relates to a wholly aromatic liquid-crystalline polyester resin having a melting point of 300 to 450 캜, a reinforcing filler for physical properties, and an inorganic filler in powder form, Lt; / RTI >
Specifically, as the filler for reinforcing physical properties, one or more kinds of fillers are preferably selected from the group consisting of glass fibers and carbon fibers.
The powdery inorganic filler may be selected from the group consisting of calcium carbonate, quartz, tridymite, cristobalite, coesite, stishovite, talc, talc, mica, and carbon black. It is preferable that the carbon black is at least one selected from the group consisting of talc, mica, and carbon black.
The content of the physical property reinforcing filler is preferably in the range of 5 to 90 parts by weight based on 100 parts by weight of the wholly aromatic liquid-crystalline polyester resin.
The content of the powdery inorganic filler is preferably in the range of 0.1 to 5 parts by weight based on 100 parts by weight of the wholly aromatic liquid-crystalline polyester resin.
The wholly aromatic liquid-crystalline polyester resin composition according to the present invention contains a small amount of a powdery inorganic filler in a wholly aromatic liquid-crystalline polyester resin having a solid content of a solid content and a filler for physical property reinforcement, Because of its excellent resistance to blistering, it can be used as an electronic component, connector, and memory card socket component material.
Hereinafter, the wholly aromatic liquid-crystalline polyester resin composition according to one embodiment of the present invention will be described in detail.
According to one embodiment of the present invention, the wholly aromatic liquid-crystalline polyester resin composition comprises a wholly aromatic liquid-crystalline polyester resin having a melting point of 300 to 450 ° C, a physical property reinforcing filler, and a powder type inorganic filler.
The wholly aromatic liquid-crystalline polyester resin, which is the first component constituting the wholly aromatic liquid-crystalline polyester resin composition according to this embodiment, is preferably selected to have a melting point of 300 to 450 ° C for realizing high heat resistance and mechanical properties .
Since the wholly aromatic liquid-crystalline polyester resin has a high melting point, it has high heat resistance. Such a wholly aromatic liquid-crystalline polyester resin can be produced through two steps as described below.
(a) synthesizing a wholly aromatic liquid-crystalline polyester prepolymer by condensation polymerization of at least two kinds of monomers; And
(b) synthesizing the wholly aromatic liquid-crystalline polyester resin by solid-phase polycondensing the prepolymer.
The monomer used in the step (a) includes at least one kind of compound selected from the group consisting of aromatic diols, aromatic diamines and aromatic hydroxyamines, and aromatic dicarboxylic acids. In addition, the monomer may further comprise an aromatic hydroxycarboxylic acid and / or an aromatic aminocarboxylic acid.
As the synthesis method of step (a), a solution condensation polymerization method or a bulk condensation polymerization method may be used. In order to accelerate the condensation reaction in the step (a), a monomer having increased reactivity and pretreated with a chemical substance such as an acylating agent, for example, an acetylating agent, for example, an acylated monomer may be used.
For the solid-phase polycondensation reaction in the step (b), suitable heat should be provided to the prepolymer. As the method of providing the heat, a method using a hot plate, a method using hot air, or a method using a high temperature fluid may be used. In order to remove the byproducts generated during the solid-phase condensation polymerization, it is possible to purge or remove by vacuum using an inert gas.
The wholly aromatic liquid-crystalline polyester resin can be produced by the method described above, but is not limited thereto, and it is preferable that the wholly aromatic liquid-crystalline polyester resin is selected from those having a melting point of 300 to 450 ° C.
The wholly aromatic liquid-crystalline polyester resins each contain various repeating units in the chain, and may include, for example, the following repeating units:
(1) a repeating unit derived from an aromatic diol:
-O-Ar-O-
(2) a repeating unit derived from an aromatic diamine:
-HN-Ar-NH-
(3) repeating unit derived from aromatic hydroxyamine:
-HN-Ar-O-
(4) repeating unit derived from an aromatic dicarboxylic acid:
-OC-Ar-CO-
(5) repeating unit derived from an aromatic hydroxycarboxylic acid:
-O-Ar-CO-
(6) a repeating unit derived from an aromatic aminocarboxylic acid:
-HN-Ar-CO-
In the above recurring units, Ar is an aromatic compound in which phenylene, biphenylene, naphthalene or two phenylene are bonded with carbon or a non-carbon element, or phenylene, biphenylene, naphthalene or two phenylene An aromatic compound in which at least one hydrogen of an aromatic compound bonded with a carbon or non-carbon element is substituted with another element may be used.
The wholly aromatic liquid-crystalline polyester resin composition according to the present embodiment includes a filler for imparting mechanical properties, and the physical property-enhancing filler preferably includes at least one selected from glass fibers or carbon fibers, But is not limited to.
The content of the physical property reinforcing filler may be in the range of 5 to 90 parts by weight based on 100 parts by weight of the wholly aromatic liquid crystal polyester resin. When the content of the filler is less than 5 parts by weight based on 100 parts by weight of the wholly aromatic liquid-crystalline polyester resin, it is difficult for the wholly aromatic liquid-crystalline polyester resin composition to achieve sufficient mechanical strength. When the content is more than 90 parts by weight, The moldability of the liquid crystal polyester resin composition is lowered.
On the other hand, since a blister phenomenon occurs at a high temperature in the case of a resin compound using only an all-aromatic liquid crystal polyester resin and a material-reinforcing filler, a small amount of a powdery inorganic filler is used to prevent this.
Since the wholly aromatic liquid-crystalline polyester resin has a high melting point of 300 ° C or higher, most of the wholly aromatic liquid-crystalline polyester resins are decomposed when the powdery organic filler is contained, and thus, are unusable. Therefore, the powdery inorganic filler to be used should have thermal stability.
Examples of the powdery inorganic filler include calcium carbonate, quartz, tridymite, cristobalite, coesite, stishovite, talc, , Mica (mica), and carbon black (carbon black).
The powdery inorganic filler may be used singly or in the form of a mixture of two or more thereof.
The content of the powdery inorganic filler is preferably in the range of 0.1 to 5 parts by weight based on 100 parts by weight of the wholly aromatic liquid-crystalline polyester resin. When the amount of the powdery inorganic filler is less than 0.1 part by weight, it is difficult to expect improvement in blister resistance of the wholly aromatic liquid-crystalline polyester resin composition. When the amount exceeds 5 parts by weight, the mechanical properties of the wholly aromatic liquid- It is not preferable because it can be changed.
Herein, the inorganic filler included for improvement of blister resistance is preferably in the form of a powder because the inorganic particles of the powder form functions as a radical trapping agent and also contributes to thermal stability.
The inorganic filler of the powder type contains a small amount in the wholly aromatic liquid crystal polyester resin compound to improve the blister resistance without deteriorating the heat resistance and the mechanical properties, and the molded product of the connector and memory card socket of the electronic product requiring high heat resistance and soldering .
The wholly aromatic liquid-crystalline polyester resin composition according to the present invention is obtained by mixing a wholly aromatic liquid-crystalline polyester resin having a melting point of 300 to 450 ° C with a physical property-enhancing filler and a powdery inorganic filler, Compound. ≪ / RTI >
For the melt kneading, a twin-screw extruder, a batch kneader or a mixing roll may be used, but the present invention is not limited thereto. In particular, when the melt-kneading is performed using a twin-screw extruder, the barrel temperature of the extruder can be maintained at 330 to 450 ° C. Here, the barrel of an extruder is also referred to as a cylinder as a portion for melting, kneading, and transporting an extruded material (i.e., a resin composition). A screw is mounted in the barrel so that the extruded raw material is transported forward in accordance with the rotation of the screw, and at the same time, the extruded raw material is melted due to heat conducted from the barrel wall surface. Further, for the purpose of smooth melt-kneading, an activator may be used for melt-kneading.
Since the resin compound prepared by mixing and melt-kneading the powder type inorganic filler with the wholly aromatic liquid-crystalline polyester resin having a high melting point has excellent blister resistance without deteriorating fluidity, heat resistance and mechanical properties, And connectors and memory card socket products.
Hereinafter, the present invention will be described in more detail with reference to examples, but the present invention is not limited to the examples.
Manufacturing example One
Wholly aromatic Production of liquid crystal polyester resin
24.4 kg of parahydroxybenzoic acid, 10.8 kg of biphenol, 7.3 kg of terephthalic acid and 2.4 kg of isophthalic acid were charged into a 100 liter batch reactor capable of controlling the temperature, and nitrogen gas was injected to render the internal space of the reactor inactive Next, 33 kg of acetic anhydride was further added to the reactor. The reactor temperature was then raised to 150 ° C over 30 minutes and the alcohol functionality of the monomers was acetylated at this temperature for 3 hours. Then, the acetic acid generated in the acetylation reaction was removed and the temperature of the reactor was elevated to 330 ° C over 6 hours to prepare a wholly aromatic liquid-crystalline polyester prepolymer by condensation polymerization of monomers. In addition, acetic acid was further produced as a by-product in the preparation of the prepolymer. The acetic acid was also continuously removed during the preparation of the prepolymer together with the acetic acid generated in the acetylation reaction. The prepolymer was then recovered from the reactor and cooled and solidified.
Thereafter, the above wholly aromatic liquid-crystalline polyester prepolymer was pulverized to an average particle size of 1 mm, 20 kg of the pulverized wholly aromatic liquid-crystalline polyester prepolymer was charged into a 100-liter capacity rotary kiln reactor, nitrogen was continuously supplied at a flow rate of 1 Nm 3 / The temperature was raised to 200 deg. C, which is the weight loss starting temperature, over 1 hour, and then the temperature was raised to 280 deg. C over 10 hours and maintained for 3 hours to prepare a wholly aromatic liquid crystal polyester resin. Then, the reactor was cooled to room temperature over 1 hour, and the wholly aromatic liquid-crystalline polyester resin was recovered from the reactor.
The melting point of the resin measured using a differential scanning calorimeter was 320 ° C.
Example One
The wholly aromatic liquid-crystalline polyester resin prepared in Preparation Example 1 was mixed with glass fibers (KCC, CS371) and carbon black (Evonik, HIBLACK 30L) at a ratio of 69.9: 30: 0.1 by weight, / D: 40, diameter: 20 mm). During the melt kneading, the barrel temperature of the extruder was 350 ° C. During the melt kneading, a by-product was removed by applying a vacuum to the twin screw extruder. Then, the melt-kneaded product was mixed with an automatic mixer (product of Cheil Industries Co., Ltd.) for 10 minutes and dried at 130 ° C for 2 hours by a hot-air dryer (manufactured by Shing PLANT) to prepare a wholly aromatic liquid-crystalline polyester resin compound.
Example 2
Except that the wholly aromatic liquid-crystalline polyester resin prepared in Preparation Example 1 was mixed with glass fibers (KCC, CS371) and talc (Dongyang Material Chemistry, ETA # 400) at a ratio of 68.5: 30: 1.5 by weight , A wholly aromatic liquid-crystalline polyester resin compound was prepared in the same manner as in Example 1 above.
Example 3
Except that the wholly aromatic liquid-crystalline polyester resin prepared in Preparation Example 1 was mixed with glass fibers (KCC, CS371) and calcium carbonate (V-JAD # 300, Orient Chemical Material) at a ratio of 69: 30: 1 by weight , A wholly aromatic liquid-crystalline polyester resin compound was prepared in the same manner as in Example 1 above.
Example 4
(KCC, CS371), talc (TYOYAN MATERIALS, ETA # 400) and carbon black (Evonik, HIBLACK 30L) in a weight ratio of 67: 30: 1.5 based on the weight of the wholly aromatic liquid- : 1.5, a wholly aromatic liquid-crystalline polyester resin compound was prepared in the same manner as in Example 1 above.
Example 5
Except that glass fiber (KCC, CS371) and quartz powder (QT # 1250, Orientate material) were mixed in the ratio of 67: 30: 3 by weight to the wholly aromatic liquid crystal polyester resin prepared in Production Example 1 , A wholly aromatic liquid-crystalline polyester resin compound was prepared in the same manner as in Example 1 above.
Example 6
Except that glass fiber (KCC, CS371) and cristobalite (HOBEN international LTD, C325) were mixed in the ratio of 67: 30: 3 on the weight basis of the wholly aromatic liquid crystal polyester resin produced in Production Example 1, A wholly aromatic liquid-crystalline polyester resin compound was prepared in the same manner as in Example 1.
Comparative Example One
Except that the wholly aromatic liquid-crystalline polyester resin and glass fiber (KCC, CS371) prepared in Preparation Example 1 were mixed at a ratio of 70:30 on the basis of weight, To prepare an ester resin compound.
Comparative Example 2
(KCC, CS371), calcium carbonate (V-JAD # 300) and carbon black (Evonik, HIBLACK 30L) and 65.5: 30 by weight of the wholly aromatic liquid crystal polyester resin prepared in Preparation Example 1 : 3: 1.5, the wholly aromatic liquid-crystalline polyester resin compound was prepared.
Evaluation example
The physical properties of the wholly aromatic liquid-crystalline polyester resin compounds prepared in Examples 1 to 6 and Comparative Examples 1 and 2 were measured by the following methods.
(1) Measurement of melt viscosity
The viscosity of each compound was measured under the conditions of 330 캜 and 1/1000 s using a capillary viscometer to compare the fluidity of the molten state.
(2) The tensile strength And Tensile Measure
The tensile strength and tensile elongation of each of the wholly aromatic liquid-crystalline polyester resin compounds were measured according to ASTM D638.
(3) Flexural strength And Flexor Measure
The flexural strength and flexural elongation of each of the wholly aromatic liquid crystalline polyester resin compounds were measured according to ASTM D790.
(4) The heat resistance (heat distortion temperature) Measure
The heat resistance of each of the wholly aromatic liquid-crystalline polyester resin compounds was measured according to ASTM D648. At this time, the applied pressure was 18.5 kgf / cm 2.
(5) My blister castle Measure
The blister resistance of each of the wholly aromatic liquid-crystalline polyester resin compounds was tested at 250 ° C to 5 ° C intervals using a reflow oven (Samsung, RF30102), and the temperature at which the blisters began to occur was measured.
Occurrence temperature (℃)
Referring to Table 1 above, The results are shown in Fig.
First, the wholly aromatic liquid-crystalline polyester resin compounds prepared in Examples 1 to 6 are superior in tensile strength, elongation at break, elongation at break, and elongation at break, as compared with the wholly aromatic liquid-crystalline polyester resin compound prepared in Comparative Example 1, Bending strength, flexural elongation and heat resistance, and the blister resistance was improved.
Second, in the case of Examples 1 to 4, as the amount of the powdery inorganic filler to be added is less than 5 parts by weight based on 100 parts by weight of the wholly aromatic liquid-crystalline polyester resin, the blister resistance .
And Comparative Example 2 is a case where the powder type inorganic filler is contained in an amount exceeding 5 parts by weight based on 100 parts by weight of the wholly aromatic liquid-crystalline polyester resin. In this case, the physical properties are deteriorated due to tensile strength, tensile elongation, .
While the invention has been described with reference to exemplary embodiments, it is to be understood that the invention is not limited to the disclosed embodiments, but, on the contrary, is intended to cover various modifications and equivalent arrangements included within the spirit and scope of the appended claims. Accordingly, the true scope of the present invention should be determined by the technical idea of the appended claims.
Claims (5)
Fillers for reinforcing physical properties; And
A powdery inorganic filler,
The content of the powdery inorganic filler is 0.1 to 3 parts by weight based on 100 parts by weight of the wholly aromatic liquid crystal polyester resin, the physical property reinforcing filler and the powder type inorganic filler, the wholly aromatic liquid- Resin composition.
Wherein the filler for reinforcing physical properties is at least one selected from the group consisting of glass fibers and carbon fibers.
The powdery inorganic filler may be selected from the group consisting of calcium carbonate, quartz, tridymite, cristobalite, coesite, stishovite, talc, Mica, and carbon black. The blister-modified wholly aromatic liquid-crystalline polyester resin composition according to claim 1,
Wherein the content of the physical property-reinforcing filler is in the range of 5 to 90 parts by weight based on 100 parts by weight of the wholly aromatic liquid-crystalline polyester resin.
Priority Applications (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| KR1020110112179A KR101743301B1 (en) | 2011-10-31 | 2011-10-31 | Wholly Aromatic Liquid Crystalline Polyester Resin Composition with Excellent Blister Resistant |
| TW101139656A TWI591120B (en) | 2011-10-31 | 2012-10-26 | Wholly aromatic liquid crystalline polyester resin composition with excellent blister resistance |
| PCT/KR2012/008899 WO2013066008A1 (en) | 2011-10-31 | 2012-10-26 | Wholly aromatic liquid crystal polyester resin composition having improved blister resistance |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| KR1020110112179A KR101743301B1 (en) | 2011-10-31 | 2011-10-31 | Wholly Aromatic Liquid Crystalline Polyester Resin Composition with Excellent Blister Resistant |
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| Publication Number | Publication Date |
|---|---|
| KR20130047261A KR20130047261A (en) | 2013-05-08 |
| KR101743301B1 true KR101743301B1 (en) | 2017-06-02 |
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| Application Number | Title | Priority Date | Filing Date |
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| KR1020110112179A KR101743301B1 (en) | 2011-10-31 | 2011-10-31 | Wholly Aromatic Liquid Crystalline Polyester Resin Composition with Excellent Blister Resistant |
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| Country | Link |
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| KR (1) | KR101743301B1 (en) |
| TW (1) | TWI591120B (en) |
| WO (1) | WO2013066008A1 (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR101488307B1 (en) | 2013-04-29 | 2015-01-30 | 현대자동차주식회사 | Smart Touch Type Electronic Auto Shift Lever |
| CN111073258A (en) * | 2019-12-24 | 2020-04-28 | 江苏沃特特种材料制造有限公司 | Polyphenyl ether composite material and preparation method thereof |
Family Cites Families (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002294038A (en) * | 2001-03-28 | 2002-10-09 | Sumitomo Chem Co Ltd | Liquid crystal ester resin composition |
| JP4999285B2 (en) * | 2005-05-24 | 2012-08-15 | 上野製薬株式会社 | Liquid crystalline polyester resin composition |
| JP2007119673A (en) * | 2005-10-31 | 2007-05-17 | Polyplastics Co | Thermoplastic resin composition |
| KR100722949B1 (en) * | 2005-11-17 | 2007-05-30 | 삼성정밀화학 주식회사 | High Heat-resistance Wholly Aromatic Polyester Composition and Manufacturing Method thereof |
| KR101708927B1 (en) * | 2009-10-09 | 2017-02-21 | 심천 워트 어드밴스드 머티리얼즈 주식회사 | Wholly aromatic liquid crystalline polyester resin compound with enhanced thermal resistance and method for preparing the same |
| KR101783477B1 (en) * | 2009-10-21 | 2017-09-29 | 심천 워트 어드밴스드 머티리얼즈 주식회사 | Wholly aromatic liquid crystalline polyester resin compound, method of preparing the resin compound, parts for optical pick-up, and method of preparing the parts |
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2011
- 2011-10-31 KR KR1020110112179A patent/KR101743301B1/en active IP Right Review Request
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2012
- 2012-10-26 WO PCT/KR2012/008899 patent/WO2013066008A1/en active Application Filing
- 2012-10-26 TW TW101139656A patent/TWI591120B/en active
Also Published As
| Publication number | Publication date |
|---|---|
| KR20130047261A (en) | 2013-05-08 |
| TW201317296A (en) | 2013-05-01 |
| TWI591120B (en) | 2017-07-11 |
| WO2013066008A1 (en) | 2013-05-10 |
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