KR20120136434A - Wholly aromatic liquid crystalline polyester resin compound having high stiffness - Google Patents
Wholly aromatic liquid crystalline polyester resin compound having high stiffness Download PDFInfo
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- KR20120136434A KR20120136434A KR1020110055269A KR20110055269A KR20120136434A KR 20120136434 A KR20120136434 A KR 20120136434A KR 1020110055269 A KR1020110055269 A KR 1020110055269A KR 20110055269 A KR20110055269 A KR 20110055269A KR 20120136434 A KR20120136434 A KR 20120136434A
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- polyester resin
- aromatic liquid
- wholly aromatic
- liquid crystal
- crystal polyester
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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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/36—Silica
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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
- C08K7/14—Glass
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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
- C08L67/00—Compositions of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Compositions of derivatives of such polymers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G2261/00—Macromolecular compounds obtained by reactions forming a carbon-to-carbon link in the main chain of the macromolecule
- C08G2261/50—Physical properties
- C08G2261/53—Physical properties liquid-crystalline
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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)
- Polyesters Or Polycarbonates (AREA)
Abstract
Description
A wholly aromatic liquid crystalline polyester resin compound is disclosed. More specifically, a wholly aromatic liquid crystal polyester resin compound comprising a wholly aromatic liquid crystal polyester resin having a high melting point and a silicone-based reinforcing agent is disclosed.
The wholly aromatic liquid crystal polyester resin is excellent in heat resistance and dimensional stability, and excellent in fluidity during melting, and is widely used in the field of electronic parts as a precision injection molding material. In particular, such an wholly aromatic liquid crystal polyester resin has excellent dimensional stability and electrical insulation, and its use is expanding as a connector for electronic products and sockets for other memory cards. In addition, the wholly aromatic liquid crystal polyester resin is a kind of thermoplastic polymer produced by condensation polymerization, and the resin compound may be prepared by kneading with an inorganic filler such as glass fiber and / or talc and extruding. In addition, the resin compound prepared as described above may be processed into a product through an injection process.
Meanwhile, connectors and memory card socket products of electronic products manufactured by using the resin compound tend to be developed as products having a thin thickness and a wide width or a thin thickness and long length. Accordingly, even when applied to a product having a thin and wide thin film form or a thin and long form, a high rigid resin compound that can sufficiently satisfy the mechanical requirements of the product is required. However, when the degree of polymerization of the wholly aromatic liquid crystal polyester resin, which is the main raw material of the resin compound, is increased in the polymerization step in order to improve the rigidity of the resin compound, in general, the flowability and elasticity of the resin and the resin compound are lowered and molding becomes difficult. Even if the product is hardly molded, there is a problem that it can not maintain its shape and is broken.
One embodiment of the present invention provides a wholly aromatic liquid crystal polyester resin compound comprising a wholly aromatic liquid crystal polyester resin having a high melting point and a silicone-based reinforcing agent.
According to an aspect of the present invention,
100 parts by weight of the wholly aromatic liquid-crystalline polyester resin having a melting point of 300 to 450 ℃; And
It provides a wholly aromatic liquid crystal polyester resin compound containing 2 to 50 parts by weight of a silicone-based reinforcing agent.
The silicone-based reinforcing agent may have an average particle diameter of 1000 μm or less.
The silicone-based reinforcing agent may include silica, silicate or a mixture thereof.
The wholly aromatic liquid crystal polyester resin compound may further include an inorganic filler.
The inorganic filler may include glass fiber, talc, calcium carbonate, clay or a mixture of two or more thereof.
The content of the inorganic filler may be 5 to 90 parts by weight based on 100 parts by weight of the wholly aromatic liquid crystal polyester resin.
According to one embodiment of the present invention, by including a wholly aromatic liquid crystal polyester resin having a high melting point and a silicone-based reinforcing agent, the rigidity is improved, the wholly aromatic liquid crystal polyester resin compound excellent in mechanical properties, heat resistance and dimensional stability can be provided Can be.
Hereinafter, the wholly aromatic liquid crystal polyester resin compound according to one embodiment of the present invention will be described in detail.
The wholly aromatic liquid crystal polyester resin compound according to the embodiment of the present invention includes 100 parts by weight of the wholly aromatic liquid crystal polyester resin having a melting point of 300 to 450 ° C. and 2 to 50 parts by weight of the silicone-based reinforcing agent.
As such, by including the wholly aromatic liquid crystal polyester resin having a high melting point and the silicone-based reinforcing agent, the rigidity of the wholly aromatic liquid crystal polyester resin compound can be improved.
If the melting point of the wholly aromatic liquid-crystalline polyester resin is less than 300 ° C, the fluidity is too high in the high-temperature processing region of 330 ° C or more, and processing is difficult.
Since the wholly aromatic liquid-crystalline polyester resin has a high melting point, heat resistance is also high. Such wholly aromatic liquid crystalline polyester resin can be prepared by the following steps:
(a) synthesizing the wholly aromatic liquid crystalline polyester prepolymer by polycondensing at least one monomer; And
(b) synthesizing the wholly aromatic liquid crystal polyester resin by solid-phase polymerization of the prepolymer.
The monomer used in step (a) may include an aromatic diol, aromatic diamine, aromatic hydroxylamine, aromatic dicarboxylic acid, aromatic hydroxy carboxylic acid, aromatic amino carboxylic acid, or a combination thereof.
As the synthesis method of step (a), solution condensation polymerization, bulk condensation polymerization may be used. In addition, in order to promote the condensation reaction in the step (a), it is possible to use an acylated (particularly, acetylated) monomer as the monomer of the step (a). To this end, before the step (a) may further comprise the step of acylating the monomer in advance.
Appropriate heat should be provided to the prepolymer for the solid phase polymerization reaction of step (b), and the heat providing method includes a method using a heating plate, a method using a hot air, a method using a high temperature fluid, and the like. In order to remove by-products generated during the solid-phase condensation polymerization reaction, purging using an inert gas or vacuum removal may be performed.
Each of the wholly aromatic liquid crystal polyester resins may include various repeating units in a chain, and may include, for example, the following repeating units:
(1) repeating units derived from aromatic diols:
-O-Ar-O-
(2) repeating units derived from aromatic diamines:
-HN-Ar-NH-
(3) repeating units derived from aromatic hydroxylamines:
-HN-Ar-O-
(4) repeating units derived from aromatic dicarboxylic acids:
-OC-Ar-CO-
(5) repeating units derived from aromatic hydroxy carboxylic acids:
-O-Ar-CO-
(6) repeating units derived from aromatic amino carboxylic acids:
-HN-Ar-CO-
In the above formulas, Ar is an aromatic compound in which phenylene, biphenylene, naphthalene or two phenylenes are bonded to elements other than carbon or carbon, or phenylene, biphenylene, naphthalene or two phenylene is carbon Or an aromatic compound in which at least one hydrogen is substituted with another element among aromatic compounds bonded with an element other than carbon.
The silicone-based reinforcing agent imparts high rigidity to the resin compound without degrading the mechanical properties and heat resistance properties of the wholly aromatic liquid crystal polyester resin compound, so that the resin compound is thin and wide, or thin and long It can be used to manufacture connectors and memory card sockets.
The silicone-based reinforcing agent may have an average particle diameter of 1000 μm or less (eg, 5-100 μm). When the average particle diameter of the embodiment cone-based reinforcing agent is 1000 μm or less, the fluidity of the wholly aromatic liquid crystal polyester resin compound may be maintained high.
The silicone-based reinforcing agent may include silica, silicate or a mixture thereof. The silica may include crystalline silica, amorphous silica, fumed silica, or a mixture of two or more thereof. The silicate may include sodium silicate, magnesium silicate, aluminum silicate, potassium silicate, lithium silicate or a mixture of two or more thereof.
When the content of the silicone-based reinforcing agent is less than 2 parts by weight based on 100 parts by weight of the wholly aromatic liquid crystal polyester resin, it is difficult for the wholly aromatic liquid crystal polyester resin compound to express sufficient rigidity. The fluidity of the aromatic liquid crystal polyester resin compound may decrease.
The wholly aromatic liquid crystal polyester resin compound may further include an inorganic filler. These inorganic fillers serve to further increase the mechanical strength and heat resistance of the wholly aromatic liquid crystal polyester resin compound comprising the same.
The inorganic filler may include at least one selected from the group consisting of glass fibers, talc, calcium carbonate and clay.
The content of the inorganic filler may be 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 inorganic filler is within the above range, it is possible to impart sufficient mechanical strength to the resin compound without lowering the fluidity of the resin compound.
The wholly aromatic liquid crystal polyester resin compound may be prepared by mixing a wholly aromatic liquid crystal polyester resin having a melting point of 300 to 450 ° C. with a silicone-based reinforcing agent to prepare a resin composition, and melt kneading the resin composition. Thus, the resin composition comprising a wholly aromatic liquid crystal polyester resin having a high melting point and a silicone-based reinforcing agent is improved in rigidity without deterioration in fluidity and heat resistance, and improved in dimensional stability, thereby making a thin molded article such as a connector and a memory. Suitable for the manufacture of sockets for cards.
In addition, a twin screw extruder, a batch kneader or a mixing roll may be used for the melt kneading. In particular, when performing the melt kneading using a twin screw extruder it is possible to maintain the barrel temperature of the extruder to 330 to 450 ℃. Here, the barrel of the extruder is also referred to as a cylinder as a part for melting, kneading and transporting the extruded raw material (that is, the resin composition). The inside of the barrel is equipped with a screw so that the extrusion raw material is forwarded as the screw rotates, and at the same time the extrusion raw material is melted due to the heat conducted through the barrel wall. Further, for the purpose of smooth melt-kneading, an activator may be used for melt-kneading.
Hereinafter, the present invention will be described in more detail with reference to examples, but the present invention is not limited to these embodiments.
Example
Example One
(1) Preparation of wholly aromatic liquid crystalline polyester resin
Into a 100-liter batch reactor capable of temperature control, 24.4 kg of para hydroxy benzoic acid, 10.8 kg of 4,4′-biphenol, 7.3 kg of terephthalic acid and 2.4 kg of isophthalic acid were added and nitrogen gas was injected to the internal space of the reactor. After making the inert state, 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 hydroxyl groups of the monomers were acetylated for 3 hours at this temperature . Subsequently, the reactor temperature was raised to 330 ° C. over 6 hours while removing the acetic acid produced in the acetylation reaction to prepare a wholly aromatic liquid crystal polyester prepolymer by a condensation polymerization reaction of the monomers. In addition, acetic acid is further produced as a by-product in the preparation of the prepolymer, which was also removed continuously during the prepolymer preparation together with the acetic acid produced in the acetylation reaction. Next, the prepolymer was recovered from the reactor and cooled and solidified.
Thereafter, the wholly aromatic liquid crystalline polyester prepolymer was pulverized to an average particle diameter of 1 mm, 20 kg of the crushed wholly aromatic liquid crystalline polyester prepolymer was introduced into a rotary kiln reactor having a capacity of 100 liters, and nitrogen was continued at a flow rate of 1 Nm 3 / hour. The whole aromatic liquid crystal polyester resin was prepared by heating up to 200 degreeC which is a weight loss start temperature while flowing over 1 hour, then heating up to 280 degreeC over 10 hours, and maintaining for 3 hours. Subsequently, the reactor was cooled to room temperature over 1 hour, and then the wholly aromatic liquid crystal polyester resin was recovered from the reactor.
The melting point of the resin measured using a differential scanning calorimeter was 320 ° C.
(2) Preparation of wholly aromatic liquid crystalline polyester resin compound (1)
The wholly aromatic liquid crystal polyester resin prepared in (1), silica (21st century silica, KorSil® KS-300, average particle diameter 9㎛), glass fiber (Sungjin fiber, MF150W-NT) and talc (Dongyang Materials Chemistry, ETA # 400 and an average particle diameter of 11 μm were mixed at a ratio of 80: 5: 5: 10 by weight and melt kneaded using a twin screw extruder (L / D: 40, diameter: 20 mm). In the melt kneading, the barrel temperature of the extruder was 350 ° C. In addition, during the melt kneading, a vacuum was applied to the twin screw extruder to remove by-products.
Subsequently, the melt-kneaded product was mixed for 10 minutes with an automatic mixer (product of the first industrial equipment), and dried at 130 ° C. for 2 hours using a hot air dryer (product made by Azant Plant) to prepare a wholly aromatic liquid crystal polyester resin compound (1). .
Example 2
The wholly aromatic liquid crystal polyester resin prepared in (1), silica (21st century silica, KorSil® KS-300, average particle diameter 9㎛), glass fiber (Sungjin fiber, MF150W-NT) and talc (Dongyang Materials Chemistry, ETA Compound (2) of the wholly aromatic liquid-crystalline polyester resin was prepared in the same manner as in Example 1, except that the mixing ratio of # 400, average particle diameter of 11 μm) was changed to 70: 15: 5: 10 by weight. It was.
Example 3
The wholly aromatic liquid crystal polyester resin prepared in (1), silica (21st century silica, KorSil® KS-300, average particle diameter 9㎛), glass fiber (Sungjin fiber, MF150W-NT) and talc (Dongyang Materials Chemistry, ETA Compound (3) of the wholly aromatic liquid-crystalline polyester resin was prepared in the same manner as in Example 1, except that the mixing ratio of # 400, average particle diameter of 11 μm) was changed to 60: 25: 5: 10 by weight. It was.
Comparative example One
Based on the weight of the wholly aromatic liquid crystal polyester resin, glass fiber (Sungjin fiber, MF150W-NT) and talc (Dongyang Materials Chemistry, ETA # 400, average particle diameter 11㎛) prepared in Example 1 (1) A wholly aromatic liquid crystalline polyester resin compound 4 was prepared in the same manner as in Example 1, except that the mixture was mixed at 5:10 (ie, no silica was used).
Comparative example 2
The wholly aromatic liquid crystal polyester resin prepared in (1), silica (21st century silica, KorSil® KS-300, average particle diameter 9㎛), glass fiber (Sungjin fiber, MF150W-NT) and talc (Dongyang Materials Chemistry, ETA Compound (5) of the wholly aromatic liquid-crystalline polyester resin was prepared in the same manner as in Example 1, except that the mixing ratio of # 400, average particle diameter of 11 μm) was changed to 55: 30: 5: 10 by weight. It was.
Evaluation example
The physical properties of the wholly aromatic liquid crystal polyester resin compounds (1) to (5) prepared in Examples 1 to 3 and Comparative Examples 1 to 2 were measured by the following method.
(Measurement of Melt Viscosity (Liquidity))
Using a melt viscosity measuring apparatus (Rosand, RH2000), the viscosity of each wholly aromatic liquid crystal polyester resin compound was measured under a 1.0 mm × 32 mm capillary tube at a temperature of 330 ° C. and a shear rate of 1000 / s. It was said. Lower melt viscosity means higher fluidity.
(Measurement of tensile modulus and tensile strength)
Tensile modulus and tensile strength of each of the wholly aromatic liquid crystal polyester resin compound were measured according to ASTM D638.
(Measurement of Flexural Modulus and Flexural Strength)
Flexural modulus and flexural strength of each of the wholly aromatic liquid crystal polyester resin compounds were measured according to ASTM D790.
(Measurement of heat resistance (heat deformation temperature))
The heat resistance of each of the wholly aromatic liquid crystal polyester resin compound was measured according to ASTM D648. At this time, the given pressure was 18.5 kgf / cm 2.
(Measurement of Linear Thermal Expansion Coefficient)
The linear thermal expansion coefficient of each of the wholly aromatic liquid crystal polyester resin compounds was measured according to ASTM E831. At this time, the measurement direction was a direction perpendicular to the flow direction of the resin during molding.
(Μm / mm / ℃)
Referring to Table 1, the wholly aromatic liquid crystal polyester resin compound prepared in Examples 1 to 3, the flowability is similar, compared to the wholly aromatic liquid crystal polyester resin compound prepared in Comparative Example 1, the tensile modulus and flexural modulus It has high stiffness, excellent mechanical properties such as tensile strength and flexural strength, high heat resistance and low linear thermal expansion coefficient. Meanwhile, the wholly aromatic liquid crystal polyester resin compound prepared in Comparative Example 2 was found to have excellent physical properties except fluidity as compared to the wholly aromatic liquid crystal polyester resin compound prepared in Examples 1 to 3, but the fluidity was very low ( That is, the melt viscosity is very high) molding is impossible.
Although the present invention has been described with reference to the examples, these are merely exemplary, and those skilled in the art will understand that various modifications and equivalent other embodiments are possible therefrom. Accordingly, the true scope of the present invention should be determined by the technical idea of the appended claims.
Claims (6)
The wholly aromatic liquid crystal polyester resin compound containing 2-50 weight part of silicone type reinforcing agents.
The silicone-based reinforcing agent is a wholly aromatic liquid crystal polyester resin compound having an average particle diameter of less than 1000㎛.
The silicone-based reinforcing agent is a wholly aromatic liquid crystal polyester resin compound comprising silica, silicate or a mixture thereof.
The wholly aromatic liquid crystal polyester resin compound is an wholly aromatic liquid crystal polyester resin compound further comprises an inorganic filler.
The inorganic filler is a wholly aromatic liquid crystal polyester resin compound containing glass fiber, talc, calcium carbonate, clay or a mixture of two or more thereof.
The content of the inorganic filler is a wholly aromatic liquid crystal polyester resin compound is 5 to 90 parts by weight based on 100 parts by weight of the wholly aromatic liquid crystal polyester resin.
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| Application Number | Priority Date | Filing Date | Title |
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| KR1020110055269A KR20120136434A (en) | 2011-06-08 | 2011-06-08 | Wholly aromatic liquid crystalline polyester resin compound having high stiffness |
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| KR1020110055269A KR20120136434A (en) | 2011-06-08 | 2011-06-08 | Wholly aromatic liquid crystalline polyester resin compound having high stiffness |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US10829634B2 (en) | 2017-12-05 | 2020-11-10 | Ticona Llc | Aromatic polymer composition for use in a camera module |
| US11086200B2 (en) | 2019-03-20 | 2021-08-10 | Ticona Llc | Polymer composition for use in a camera module |
| US11722759B2 (en) | 2019-03-20 | 2023-08-08 | Ticona Llc | Actuator assembly for a camera module |
-
2011
- 2011-06-08 KR KR1020110055269A patent/KR20120136434A/en active Search and Examination
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US10829634B2 (en) | 2017-12-05 | 2020-11-10 | Ticona Llc | Aromatic polymer composition for use in a camera module |
| US11725106B2 (en) | 2017-12-05 | 2023-08-15 | Ticona Llc | Aromatic polymer composition for use in a camera module |
| US11086200B2 (en) | 2019-03-20 | 2021-08-10 | Ticona Llc | Polymer composition for use in a camera module |
| US11722759B2 (en) | 2019-03-20 | 2023-08-08 | Ticona Llc | Actuator assembly for a camera module |
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