KR101263986B1 - Environment-friendly, flame retardant thermoplastic polyetherester elastomer resin composition having good flexibility and reflectivity - Google Patents
Environment-friendly, flame retardant thermoplastic polyetherester elastomer resin composition having good flexibility and reflectivity Download PDFInfo
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Abstract
The present invention is an environmentally friendly flame retardant thermoplastic polyetherester elastomer resin composition having high flexibility and reflectance, and more specifically, 1) 30 to 70% by weight of polyetherester elastomer, 2) more than 0 to 30% by weight of polybutylene terephthalate. 3) 15 to 25 weight percent titanium dioxide, and 4) 10 to 20 weight percent metal salt flame retardant of phosphinate having an organic substituent as the main flame retardant; 5) A thermoplastic polyether ester elastomer resin composition containing 0.05 to 0.1 parts by weight of a fluorine-based anti-dripping agent, based on 100 parts by weight of an elastomer resin.
The present invention provides a thermoplastic resin composition having high flame retardancy and high reflectivity of a conventional engineering plastic-based resin but having flexibility comparable to a material using only a thermoplastic elastomer, and having good environmental friendliness, impact resistance, molding processability, heat resistance, and rigidity. Through the present invention it can be usefully used in parts such as a display backlight unit requiring low noise characteristics due to vibration and friction.
Description
The present invention relates to a flame retardant thermoplastic polyether ester elastomer resin composition, and to an engineering plastic having flexibility for use in parts requiring low noise characteristics.
Typically, the internal parts applied to the display back light unit are made of materials having a very high reflectance to maximize the transfer efficiency of the UV light source. Engineering plastics are high-performance resins of polymer structure that are stronger than steel, more malleable than aluminum, and more resistant to chemicals.In addition, they contain a large amount of titanium dioxide to improve reflectivity, and have a certain level of flame retardancy by general specifications of electrical and electronic products. The component which has is included and used for the display backlight unit.
In this case, in the case of a component such as a side housing, a lamp guide, etc. of the display backlight unit, it is necessary to reduce the noise due to minute vibrations during the display operation, and thus flexibility is required rather than rigidity of the material. Therefore, materials having elastomeric properties should be applied, but there is no known technique for materials having a certain degree of flexibility while maintaining a large part of the performance expressed by existing engineering plastic materials such as high reflectivity and eco-friendly flame retardant properties.
In addition, polyether ester elastomer is a thermoplastic elastic material having an ester-type chain structure, and has the advantage of being able to be recycled at the same time as it exhibits rubber-like properties generally produced by vulcanization. In recent years, polyether having flame retardant heat resistance characteristics Ester elastomeric materials have been developed. Polyetherester elastomer resins having such flame retardancy are generally halogen flame retardant systems using brominated polypentabromobenzene acrylate as the main flame retardant, antimony oxide and a small amount of silica as the secondary flame retardant, and in some cases phenolic halogen compounds Although the flame retardancy is expressed by using an environmentally friendly problem, conventionally, a melamine compound, an inorganic metal hydrate, or a phosphorus-based flame retardant is often used. However, the flame retardancy used in the display backlight unit is satisfied while satisfying the regulation according to the degree of flame retardancy. There is no environmentally friendly polyetherester thermoplastic elastomer composition having high flexibility, high reflectivity.
The present invention was derived to solve the above problems, the problem to be solved by the present invention is to use titanium dioxide to impart a high reflectance while utilizing a thermoplastic polyetherester elastomer resin composite composition having environmentally friendly flame retardance studied in the prior art The present invention provides a material required as a component for a display backlight unit that includes a large amount and at the same time maintains moldability, workability and impact resistance, and maintains low noise characteristics due to vibration and friction.
The present invention as a means for solving the above technical problem,
1) 30 to 70% by weight of polyetherester elastomer, 2) greater than 0 to 30% by weight of polybutylene terephthalate, 3) 15 to 25% by weight of titanium dioxide, and 4) a force having an organic substituent as the main flame retardant 10 to 20% by weight of a metal salt flame retardant of the pinate; 5) A thermoplastic polyether ester elastomer resin composition containing 0.05 to 0.1 parts by weight of a fluorine-based anti-dripping agent, based on 100 parts by weight of an elastomer resin.
In addition, the present invention provides a thermoplastic polyether ester elastomer resin composition, characterized in that the elastomer resin further comprises 100 parts by weight of more than 0% by weight and 15% by weight or less of a melamine-based auxiliary flame retardant.
On the other hand, the present invention, the melamine secondary flame retardant is characterized in that any one or a mixture of two or more of melamine cyanurate, triphenyl isocyanurate, melamine phosphate, melamine polyphosphate, melamine pyrophosphate, melamine borate A thermoplastic polyether ester elastomer resin composition is provided.
In addition, the present invention, the 1) the polyether ester elastomer is a) a crystalline hard segment (a) Hard Segment containing a ester group formed from an aromatic dicarboxylic acid or ester-forming derivative and aliphatic diol (b), b) The thermoplastic polyether ester elastomer resin composition may be a random block copolymer of a soft soft segment containing an ether group-containing polyalkylene oxide.
In addition, the present invention, 1) the polyether ester elastomer, 50 to 70% by weight of any one or two or more of these aromatic dicarboxylic acids or derivatives thereof; The aliphatic diols are ethylene glycol, propylene glycol, 1,2-propanediol, 1,3-propanediol, 1,4-butanediol, 1,5-pentanediol, 1,6-hexanediol, 1,4-cyclohexane 15 to 25% by weight of any one or a mixture of two or more of dimethanol; The poly alkylene oxide is 20 to 40% by weight of polypropylene glycol having a molecular weight of 2,000 ~ 3,000 and ethylene oxide terminal; It may be a thermoplastic polyether ester elastomer resin composition characterized in that the polymer is a random block copolymerization.
In addition, the present invention, the thermoplastic polyether ester resin composition is an antioxidant, UV stabilizer, lubricant, hydrolysis stabilizer, metal deactivator, lubricant, pigment, colorant, antistatic agent, conductivity imparting agent, EMI shielding agent, magnetic imparting agent It may be a thermoplastic polyether ester elastomer resin composition further comprises an additive which is any one of a crosslinking agent, an antimicrobial agent, a processing aid, a friction wear-resistant agent or a mixture of two or more thereof.
In addition, the present invention may be a thermoplastic polyether ester elastomer resin composition, characterized in that Shore D hardness of the thermoplastic polyether ester elastomer resin composition is 50 to 60.
On the other hand, the present invention provides a backlight unit prepared by kneading the thermoplastic polyether ester elastomer resin composition.
The present invention is more flexible than conventional engineering plastics, has low noise characteristics, and has high reflectance and eco-friendly flame retardant properties of V-0 grade, which can be useful and widely used in various electric and electronic components including displays.
DETAILED DESCRIPTION Hereinafter, the present invention will be described in more detail including examples so that those skilled in the art to which the present invention pertains can easily practice the present invention. Provide it.
The present invention includes a phosphinate compound containing titanium dioxide in one or their alloys of polyetherester elastomer resin and polybutylene terephthalate, and an organometallic salt as a main flame retardant, a melamine derivative as an auxiliary flame retardant, and flame drooping. To prevent the addition of fluorine-based anti-dripping agent, if necessary, antioxidant, UV stabilizer, lubricant, hydrolysis stabilizer, metal deactivator, lubricant, pigment, colorant, antistatic agent, conductivity giving agent, EMI shielding agent, magnetizing agent, crosslinking agent The present invention relates to a thermoplastic elastomer composition having reflectance properties and environmentally friendly flame retardant performance, comprising an additive which is one of an antibacterial agent, a processing aid, and an anti-friction wear agent or a mixture of two or more thereof.
Specifically, the present invention is 30 to 70% by weight of polyether ester elastomer, more than 0 to 30% by weight of polybutylene terephthalate, 15 to 25% by weight of titanium dioxide in the resin composition mainly containing polyether ester elastomer %, And a thermoplastic polyether ester elastomer resin composition containing 0.05 to 0.1 parts by weight of a fluorine-based anti-drip agent based on 100 parts by weight of an elastomer resin composed of 10 to 20% by weight of a phosphinate metal salt flame retardant having an organic substituent as the main flame retardant. To provide.
On the other hand, the present invention provides a thermoplastic polyether ester elastomer resin composition, characterized in that the elastomer resin further comprises 100 parts by weight of more than 0% by weight and 15% by weight or less of the melamine-based auxiliary flame retardant.
First, the polyether ester elastomer (hereinafter referred to as TPEE) used as the main component of the present invention is a crystalline hard segment containing an ester group formed from an aromatic dicarboxylic acid or its ester forming derivative and aliphatic diol (Diol) It is a thermoplastic polymer with random block copolymerization of soft soft segments composed mainly of hard segments and polyalkylene oxides containing ether groups.
The aromatic dicarboxylic acid is terephthalic acid (Terephthalic acid, TPA), isophthalic acid (Isophthalic acid, IPA), 2,6-naphthalene dicarboxylic acid, 1,5-naphthalene dicarboxylic acid, 1,4-cyclohexane dica Dimethyl terephthalate (DMT), dimethyl isophthalate, 2,6-dimethyl naphthalene dicarboxylate, dimethyl 1,4-cyclohexane dicarboxyl, which is an aromatic dicarboxylate in which diacid is substituted with a dimethyl group Any one or a mixture of two or more thereof may be used, preferably dimethyl terephthalate (DMT) is used. In preparing the TPEE used in the present invention, the aromatic dicarboxylic acid is used in an amount of 30 to 90% by weight, preferably 50 to 70% by weight.
The aliphatic diols are ethylene glycol, propylene glycol, 1,2-propanediol, 1,3-propanediol, 1,4-butanediol, 1,5-pentanediol, 1,6-hexanediol, 1,4-cyclohexane Any one or a mixture of two or more of dimethanols is used, preferably 1,4-butanediol is used. The aliphatic diol is used 10 to 30% by weight, preferably 15 to 25% by weight. If the content of aliphatic diol is less than 10% by weight or more than 30% by weight, the reaction balance is not suitable, which makes it difficult to proceed with the reaction. On the other hand, the polyalkylene oxide used in the present invention is an aliphatic polyether as a component of the soft soft segment. Specific examples include polyoxyethylene glycol, polyoxypropylene glycol, polyoxytetramethylene glycol (hereinafter referred to as PTMEG), polyoxyhexamethylene glycol, copolymers of ethylene oxide and propylene oxide, and polypropylene oxide glycol. Ethylene oxide addition polymer, copolymer of ethylene oxide and tetrahydrofuran is mentioned. Among these, it is preferable to use PTMEG, It is preferable to use PTMEG whose number average molecular weights are 600-3,000 especially, More preferably, the number average molecular weight 1,000 is used.
In general, the hardness of TPEE is expressed as Shore hardness-D (shore D), and the hardness is determined by the content of polyalkylene oxide. In the present invention, 10 to 70% by weight, preferably 20 to 40% by weight of polyalkylene oxide is used.
TPEE used in the present invention is obtained by primary melt condensation polymerization, and is about 140 using titanium butoxide (TBT), which is a catalyst based on aromatic dicarboxylic acid, aliphatic diol, and polyalkylene oxide. BHBT (Bis (4-hydroxy Butyl) Terephthalate) oligomer was produced by transesterification at 215 ° C. for 120 minutes, and then TBT, which is a catalyst, was added to the oligomer to carry out condensation polymerization at 215 ° C. to 245 ° C. for 120 minutes. do. At this time, the condensation polymerization reaction proceeds to the step of reducing the pressure in steps from 760 torr to 0.3 torr. The reaction is terminated by melt polymerization until the flow index (MFI) is 10-50, preferably 10-30, according to ASTM D-1238.
After completion of the reaction, the reactor was discharged in a reactor under nitrogen pressure to pelletize the pellets through pelletizing. The final TPEE has a melting point of 150 to 220 ° C, preferably 180 to 220 ° C, and a melt index of 10 to 40 g / 10 min at 230 ° C and a 2.16 kg load.
In the present invention, titanium dioxide used a general-purpose powder product.
In the present invention, with respect to 100% by weight of the elastomer resin composed of polyetherester elastomer, polybutylene terephthalate, and main flame retardant, auxiliary flame retardant if necessary, the composition of the titanium dioxide is preferably 15 to 25% by weight. When the composition of the titanium dioxide is less than 15% by weight, there is a decrease in reflectance, and in the case of more than 25% by weight, the problem of lowering the impact strength is significant.
In the present invention, using the phosphinate compound containing an organometallic salt as shown in the following <Formula 1> as the main flame retardant is the most suitable non-halogen flame retardant in terms of excellent flame retardancy and tensile properties of TPEE.
On the other hand, melamine complex is used as an auxiliary flame retardant used in the present invention, which is less toxic than halogen flame retardant, is easy to handle, and hardly generates toxic gas during thermal decomposition and is known as a flame retardant that does not affect human health and the environment. have. In addition, when the melamine complex is used together with the main flame retardant, it exhibits optimal synergy and has excellent flame retardancy, and as the melamine secondary flame retardant used in the present invention, melamine cyanurate, triphenyl isocyanurate, melamine phosphate, melamine Any one of polyphosphate, melamine pyrophosphate, melamine borate or mixtures of two or more thereof may be used. Of these, the use of melamine cyanurate <Formula 2> is preferred.
The particle size of the flame retardant used to increase the flame retardancy of TPEE resin has a great influence on the physical properties of the final flame retardant resin, so the particle size of the flame retardant is also very important. In general, it is known that the use of a flame retardant having a small particle size is excellent in physical properties and flame retardancy, but in the case of too small particles, a bulk density is low and a large amount of flame retardant has to be added, and at the time of feeding Separation between the layer and the flame retardant layer may not be desired, and mixing between the flame retardant and the resin may not be efficient, and thus, flame retardancy may be difficult to be expressed stably. In this example, a hybrid of a flame retardant having a particle size distribution was used. Usually it is preferable to use a flame retardant having a particle size of 1 to 100 micrometers, more preferably a flame retardant having a particle size of 1 to 50 micrometers.
Eco-friendly flame retardant thermoplastic polyether ester elastomer resin composition of the present invention, in addition to the flame retardant mentioned above, antioxidants, UV stabilizers, lubricants, hydrolysis stabilizers, metal inerts, lubricants, pigments, colorants, antistatic agents, conductivity giving agents, EMI shielding agents, Magnetic additives, crosslinking agents, antimicrobial agents, processing aids, frictional wear and the like may include an additive, characterized in that made of any one or a mixture of two or more thereof. The additives may be optionally used within the scope of not having a significant adverse effect on the physical properties in the practice of the present invention.
Environment-friendly flame retardant thermoplastic polyetherester elastomer resin composition having high flexibility and high reflectance according to the present invention may be made using a device that can effectively disperse various flame retardants at a temperature above the melting point of the TPEE resin. In general, the melting point of the TPEE resin according to an embodiment of the present invention has a temperature of 180 ~ 220 ℃, after mixing the components of the present invention in a super mixer in a conventional twin-screw extruder, a twin screw compressor (Single-screw extruder, Roll-mills, Kneader or Banbury mixer) Any one of a variety of compounding machines, such as a non-halogen-based flame retardant is used in this embodiment using a twin screw extruder The melt was kneaded, and the melt from the extruder die was stranded through a cooling bath, cooled, and prepared in pellet form.
The flexible and highly reflective eco-friendly flame retardant thermoplastic polyether ester elastomer resin composition thus prepared was sufficiently dried in a dehumidifying dryer or a hot air dryer, and then injection molded using an injection machine to sufficiently stabilize at room temperature, and then evaluated various mechanical properties and flame retardancy.
(Example 1)
Hereinafter, embodiments of the present invention will be described so that those skilled in the art can easily carry out the present invention, and the test results and the like will be described in detail with reference to the accompanying table. However, it will be apparent to those skilled in the art that the present invention may be embodied in many different forms and should not be limited to the embodiments set forth below.
(Exolit OP-1240, Clariant)
(Melamine cyanurate, particle size less than 2 micro)
Example (1) to (4) and Comparative example (1) to (4)
Using the TPEE resin and additives used in the present invention was carried out an embodiment with a composition ratio as shown in Table 1, was tested for the result.
Referring to Example 1 as an example, 12 wt% of organometallic salt phosphinate flame retardant as a main flame retardant, 5 wt% melamine cyanurate as auxiliary flame retardant, using Keyflex BT 1063D, a TPEE resin manufactured by LG Chemical, as a main raw material, by mixing a total amount of 1% by weight, such as flame drip agent is PTFE, other antioxidants, sodium phosphate, UV stabilizers in a tumbler using a mixing, a main feeder (main feeder) and, TiO 2 20 wt% was introduced into a 40? Twin screw extruder using a side feeder and melt kneaded to prepare a resin composition. At this time, the temperature of the extruder was set by giving a temperature gradient for the temperature range of 200 ~ 240 ℃ from the first inlet to the die (Die) and the rotation speed of the screw was kneaded under the conditions of 200 ~ 250 RPM. The melt from the extruder die was cooled by stranding through a cooling bath and prepared in pellet form. In other examples, using TPEE resin and PBT resin having different Shore hardness or changing only the content of other components, the same procedure as in Example 1 was carried out according to the conventional method.
Test Example
The composition prepared in Examples and Comparative Examples was dried for 3 to 4 hours at 80 to 100 ° C. using a dehumidifying hot air dryer to remove moisture, and to prepare a physical specimen and a flame retardant specimen using an injection molding machine as follows. The test was carried out according to the method and the physical properties were confirmed.
(1) Flammability
Flame retardancy was measured using a 1.6 mm thick, 12.7 mm wide, 127.0 mm long specimen in accordance with the UL (Underwriter's Laboratory) 94 bar vertical combustion test method.
(2) Reflectance
Reflectance at 550 nm wavelength was measured using a colorimeter.
(3) Hardness
Hardness was measured by Shore D type according to ASTM D 2240.
(4) tensile strength and elongation
Specimens molded according to DIN 53504-85 STAB 2 were measured at room temperature, and tensile strength (kg / cm 2 ) and tensile elongation (%) at break were measured.
(5) Flexural modulus
According to ASTM D 790 it was measured with a specimen of thickness 6.4mm.
(6) Izod impact strength
According to ASTM D 256 was measured with a 3.2mm thickness, notched specimens.
(7) heat deflection temperature
It was measured at low load (4.6 kg / cm 2 ) according to ASTM D 648.
(8) Noise characteristics
After the backlight unit module was installed in the soundproof dustproof room and operated for 30 minutes, the noise generated for a total of 1 hour was evaluated for 30 hours.
Evaluation standard: 25 to 40 decibels 15 times or less, 31 to 40 decibels 3 times or less, 40 decibels or more 0 times
Furtherance
PC = TiO 2 20% Flame Retardant
Properties
In Comparative Example 4, 'PC = TiO 2 20% flame retardant' is LG Chemical LUPOY GN 3208F as a flame retardant material, and is a material applied as a back light unit component.
According to the component ratio of each embodiment in Table 1, in the case of the present invention, using an organic metal salt-based phosphinate flame retardant 12 to 15% by weight, and a nitrogen-based flame retardant adjuvant melamine cyanurate greater than 0 to 5 or less When used in the% range, it exhibited flame retardancy of V-0 level. In the test by the component ratio according to the above embodiment, the reflectance is 95% or more, the flexural modulus is maintained at 1300 MPa or less and at the same time passes the test below the standard value of noise generated when the display backlight unit is operated. The effect of the high reflectance eco-friendly flame-retardant thermoplastic polyetherester elastomer resin desired in the present invention was confirmed.
On the other hand, in the case of the composition of the same components as Comparative Examples 1 and 4, it corresponds to a high reflectance eco-friendly flame-retardant engineering plastics, the noise occurs more than the reference value as the rigidity of the flexural modulus is higher than 2000 MPa, the comparative example 2 As a result of using the main flame retardant content of 10% by weight, the flame retardancy of the V-0 level was satisfied only 60%, in the case of Comparative Example 3 the reflectance is reduced to 94% by using 15% by weight of titanium dioxide Both of them were found to be unsuitable for the desired properties desired in the present invention. That is, it was confirmed that the polyetherester elastomer thermoplastic resin compositions according to Examples 1 to 4 satisfy all of high reflectance, flame retardant characteristics of V-0 level, etc., along with low noise characteristics due to a certain level of flexibility.
While the present invention has been particularly shown and described with reference to exemplary embodiments thereof, it is to be understood that the invention is not limited to the disclosed exemplary embodiments, Of the right.
Claims (7)
2) greater than 0 to 30 weight percent of polybutylene terephthalate,
3) 15-25 weight percent titanium dioxide, and
4) 10 to 20% by weight of the metal flame retardant of phosphinate having an organic substituent as the main flame retardant; With respect to 100 parts by weight of elastomer resin,
5) A thermoplastic polyether ester elastomer resin composition containing 0.05 to 0.1 parts by weight of a fluorine-based anti-dripping agent.
The elastomer resin, the thermoplastic polyether ester elastomer resin composition comprising more than 0% by weight of 15% by weight or less of the melamine-based auxiliary flame retardant to form 100 parts by weight.
1) The polyether ester elastomer is a) a polycrystalline crystalline hard segment (a hard segment containing an ester group formed from an aromatic dicarboxylic acid or ester forming derivative and an aliphatic diol, b) a poly containing an ether group The thermoplastic polyether ester elastomer resin composition, characterized in that the random block copolymer of the soft soft segment containing the alkylene oxide.
50 to 70 wt% of the aromatic dicarboxylic acid or ester forming derivative; 10 to 30% by weight of the aliphatic diol; And 20 to 40% by weight of polyalkylene oxide containing the ether group.
Wherein the aliphatic diol is ethylene glycol, propylene glycol, 1,2-propanediol, 1,3-propanediol, 1,4-butanediol, 1,5-pentanediol, 1,6-hexanediol, and 1,4- At least one member selected from cyclohexanedimethanol, and the polyalkylene oxide containing the ether group has a molecular weight of 2,000 to 3,000, and a thermoplastic polyether ester elastomer resin composition, characterized in that the terminal is polypropylene glycol of ethylene oxide.
The thermoplastic polyether ester resin composition may be an antioxidant, a UV stabilizer, a lubricant, a hydrolysis stabilizer, a metal deactivator, a lubricant, a pigment, a colorant, an antistatic agent, a conductivity imparting agent, an EMI shielding agent, a magnetizing agent, a crosslinking agent, an antimicrobial agent, a processing agent. The thermoplastic polyether ester elastomer resin composition, further comprising an additive which is any one of a preparation, a friction wear-resistant agent or a mixture of two or more thereof.
The thermoplastic polyether ester elastomer resin composition has a Shore D hardness of 50 to 60, characterized in that the thermoplastic polyether ester elastomer resin composition.
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| KR101425285B1 (en) * | 2012-12-14 | 2014-08-01 | 삼성토탈 주식회사 | Flame Retarding Polypropylene Resin Composition |
| KR101990407B1 (en) * | 2015-12-03 | 2019-06-18 | 주식회사 엘지화학 | Halogen-free thermoplastic resin composition and cable comprising the same |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002512645A (en) | 1997-03-18 | 2002-04-23 | デー エス エム エヌ．ヴェー． | Laser sinterable thermoplastic powder |
| KR100423233B1 (en) | 2001-03-21 | 2004-03-18 | 엘지전선 주식회사 | High strength insulation materials with flame retardant |
| KR100767956B1 (en) | 2005-08-31 | 2007-10-18 | 주식회사 엘지화학 | Backlight unit using thermal conductive resin for liquid crystal display |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002512645A (en) | 1997-03-18 | 2002-04-23 | デー エス エム エヌ．ヴェー． | Laser sinterable thermoplastic powder |
| KR100423233B1 (en) | 2001-03-21 | 2004-03-18 | 엘지전선 주식회사 | High strength insulation materials with flame retardant |
| KR100767956B1 (en) | 2005-08-31 | 2007-10-18 | 주식회사 엘지화학 | Backlight unit using thermal conductive resin for liquid crystal display |
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