KR20170025917A - Polyethyleneterephthalate resin composition and injection molding product - Google Patents

Polyethyleneterephthalate resin composition and injection molding product Download PDF

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KR20170025917A
KR20170025917A KR1020150123036A KR20150123036A KR20170025917A KR 20170025917 A KR20170025917 A KR 20170025917A KR 1020150123036 A KR1020150123036 A KR 1020150123036A KR 20150123036 A KR20150123036 A KR 20150123036A KR 20170025917 A KR20170025917 A KR 20170025917A
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polyethylene terephthalate
resin composition
terephthalate resin
weight
parts
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KR1020150123036A
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Korean (ko)
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KR102012953B1 (en
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김중원
조해철
이수민
주현진
박준기
이경환
김경문
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주식회사 엘지화학
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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
    • C08L67/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
    • C08L67/03—Polyesters derived from dicarboxylic acids and dihydroxy compounds the dicarboxylic acids and dihydroxy compounds having the carboxyl- and the hydroxy groups directly linked to aromatic rings
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
    • C08K3/0033—
    • 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
    • C08K5/00—Use of organic ingredients
    • C08K5/04—Oxygen-containing compounds
    • C08K5/09—Carboxylic acids; Metal salts thereof; Anhydrides thereof
    • 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
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L19/00—Compositions of rubbers not provided for in groups C08L7/00 - C08L17/00
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L91/00—Compositions of oils, fats or waxes; Compositions of derivatives thereof
    • C08L91/06—Waxes

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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)
  • Oil, Petroleum & Natural Gas (AREA)
  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

The present invention relates to a polyethylene terephthalate resin composition and articles of manufacture, and more particularly to a polyethylene terephthalate resin composition comprising (A) a polyethylene terephthalate resin; (B) a (meth) acrylate rubber; (C) at least one nucleating agent selected from the group consisting of a neutralized unsaturated acid polymer, a neutralized saturated fatty acid wax and an ionomer; And (D) a lubricant; The present invention relates to a polyethylene terephthalate resin composition.
According to the present invention, the HDT value is improved by maintaining the deviation of the Left value and the Right value of HDT to 0 through appropriate crystallization control at the time of extrusion, thereby securing the heat resistance stability and reducing the specific gravity, The present invention provides a polyethylene terephthalate resin composition excellent in flowability and mechanical properties and an article of manufacture containing the same.

Description

TECHNICAL FIELD [0001] The present invention relates to a poly (ethylene terephthalate) resin composition,

The present invention relates to a polyethylene terephthalate resin composition and articles of manufacture, and more particularly to a polyethylene terephthalate resin composition containing a specific rubber and a specific nucleating agent, which enables the HDT (4.6 kgf) of Left The HDT value is also improved by maintaining the deviation of the value from 0 and the value of 0 is maintained to secure the heat resistance stability and the specific gravity can be reduced and the polyethylene terephthalate resin composition excellent in the flowability of the resin flow and the mechanical properties can be obtained, It is about exhibition.

In general, polyester resins have excellent mechanical and electrical properties, physical and chemical properties and are applied to a wide range of fields such as automobiles, electric and electronic devices, and office equipment.

Examples of the polyester resin used for the exterior of automobiles and electrical and electronic parts include polybutylene terephthalate (PBT) and polyethylene terephthalate (PET). Here, PET is being used at a low price and easy to recycle, and its usage is increasing due to the development of a technique of controlling the crystallization speed and increasing the crystallization degree. The PET is used not only in water bottles but also in a variety of fields such as building structural materials, office furniture, automobile engine room covers and housings. This is generally due to the low cost and easy recycling, but from the viewpoint of the material, the development of a technology capable of controlling the crystallization by the addition of a nucleating agent has become possible.

However, the increase in crystallization rate and the increase in crystallinity due to the addition of a nucleating agent and the like increase the heat stability. However, when the nucleating agent is used more than a certain amount, the resin which is most important in injection molding due to the cluster formed in the compounding process The flow index associated with the flow of the resin decreases, which adversely affects the injection conditions of the molded article and causes problems such as an increase in the weight of the molded article and a change in mechanical properties.

Therefore, in order to overcome such a problem, it is necessary to develop a technique which can increase the crystallization rate and crystallinity by using a nucleating agent and at the same time prevent the decrease of resin flow.

Japanese Patent Laid-Open No. 2008-506012

In order to solve the problems of the prior art as described above, the present invention relates to a method for controlling the crystallization of polyethylene terephthalate, which is capable of preventing the deterioration of fluidity due to clusters formed by the nucleating agent added for controlling crystallization of polyethylene terephthalate, It is an object of the present invention to provide a resin composition and a product obtained therefrom.

These and other objects of the present disclosure can be achieved by all of the present invention described below.

In order to achieve the above object, the present invention relates to (A) a polyethylene terephthalate resin; (B) a (meth) acrylate rubber; (C) at least one nucleating agent selected from the group consisting of a neutralized unsaturated acid polymer, a neutralized saturated fatty acid wax and an ionomer; And (D) a lubricant. The present invention also provides a polyethylene terephthalate resin composition.

The present invention also provides an injection molded article comprising the above polyethylene terephthalate resin composition.

According to the present invention, the HDT value is improved while keeping the deviation of the Left value and the Right value of HDT (4.6 kgf) from 0 through the proper crystallization control at the time of extrusion, thereby securing the heat resistance stability and reducing the specific gravity. There is provided an effect of providing a polyethylene terephthalate resin composition excellent in resin flow property and mechanical properties and a product containing the same.

Hereinafter, the present invention will be described in detail.

The polyethylene terephthalate resin composition of the present invention comprises (A) a polyethylene terephthalate resin; (B) a (meth) acrylate rubber; (C) at least one nucleating agent selected from the group consisting of a neutralized unsaturated acid polymer, a neutralized saturated fatty acid wax and an ionomer; And (D) a lubricant; And a control unit.

The (B) (meth) acrylate rubber has an effect of a nucleating agent which controls the crystallization speed while acting as an impact modifier in the polyethylene terephthalate resin, and examples thereof include an ethylene-methacrylate copolymer, an ethylene- Glycidyl methacrylate copolymer or mixtures thereof.

The (B) (meth) acrylate rubber may be, for example, (A) 5 to 20 parts by weight, 7 to 17 parts by weight or 10 to 15 parts by weight based on 100 parts by weight of the polyethylene terephthalate resin, The deviation between the left value and the right value of the HDT can be maintained at 0, and the effect of reducing the specific gravity and minimizing the deterioration of the melt index is obtained.

The term "deviation of the Left value and the Right value of the HDT value" unless otherwise specified refers to the difference between the measured values for the left and right sides of the HDT (4.6 kgf) measured in accordance with ASTM D648.

For reference, a high HDT value means that the heat resistance is excellent at high temperature, but the specimen for measuring HDT has a trapezoidal shape, one of the two is measured at the left side and the other at the right side. , It means that the crystallization of the measured polyethylene terephthalate material is uniform and quick and there is no deviation between the qualities.

The (C) nucleating agent is at least one selected from the group consisting of a neutralized unsaturated acid polymer, a neutralized saturated fatty acid wax, and an ionomer.

The neutralized unsaturated acid polymer may be, for example, a neutralized ethylene-methacrylic acid copolymer, and the neutralized saturated fatty acid may be, for example, a neutralized montanic acid wax.

The nucleating agent may be, for example, (A) 1 to 7 parts by weight, 1.5 to 5 parts by weight, 2 to 4.5 parts by weight, or 2 to 3 parts by weight based on 100 parts by weight of the polyethylene terephthalate resin, When used together with the above (meth) acrylate rubber, the HDT value itself can be increased while keeping the deviation of the Left value and the Right value of HDT to 0, thereby securing the heat stability and reducing the specific gravity and the melt index have. If the amount of the nucleating agent exceeds 7 parts by weight based on 100 parts by weight of the (A) polyethylene terephthalate resin, the melt index rapidly decreases and a problem arises in molding.

The weight ratio of the (B) (meth) acrylate rubber and the (N) nucleating agent may be, for example, 6 to 8: 3 to 1 or 6.5 to 7.5: 2.5 to 1.5. In this case, There is an effect that the deviation between the value and the Right value is close to 0, and there is also an effect of excellent heat resistance.

Examples of the lubricant (D) include at least one selected from the group consisting of high density polyethylene (HDPE), montanic acid and pentaerythritol tetrastearate, and preferably montanic acid .

The high density polyethylene (HDPE) is, for example, polyethylene having a density of 0.93 to 0.97 g / cm 3 .

The lubricant may be, for example, (A) 0.1 to 2.0 parts by weight, 0.5 to 1.5 parts by weight, or 0.7 to 1.2 parts by weight based on 100 parts by weight of the polyethylene terephthalate resin, and the fluidity It has a similar flowability as the case of not using the nucleating agent and also has excellent injection moldability.

The polyethylene terephthalate resin has, for example, a crystallization temperature (Tc) of 190 to 220 ° C, 195 to 215 ° C, or 195 to 205 ° C, and an effect of generating a crystalline region which is a specific portion of the crystalline polymer within this range have.

The polyethylene terephthalate resin composition may include, for example, glass fiber, inorganic filler, or both.

The glass fiber, the inorganic filler, or both of them may be contained in an amount of 45 to 75 parts by weight, 50 to 70 parts by weight, or 55 to 65 parts by weight based on 100 parts by weight of the polyethylene terephthalate resin composition, and the fluidity and mechanical properties This has an excellent effect.

The glass fibers may be, for example, chop glass fibers having an average cross section of 3 to 5 mm or 3.5 to 4.5 mm and an average particle diameter of 9 to 15 μm or 12 to 15 μm.

The inorganic filler is at least one selected from the group consisting of talc, calcium carbonate, calcium sulfate, magnesium oxide, calcium stearate, mica, silica, calcium silicate and clay.

The polyethylene terephthalate resin composition may further include a heat stabilizer. The heat stabilizer may be a hindered phenol type having a crystallization temperature (Tm) of 110 to 130 ° C, a phosphite type having a crystallization temperature (Tm) of 180 to 190 ° C, or a mixture thereof.

The heat stabilizer (A) may be 0.1 to 2 parts by weight, 0.5 to 1.5 parts by weight, or 0.7 to 1.2 parts by weight based on 100 parts by weight of the polyethylene terephthalate resin, and has excellent balance of physical properties within this range.

The polyethylene terephthalate resin composition may further include a black master batch.

The black master batch may be, for example, a carbon black master batch, in which case the layer separation of the composition does not occur and the dispersibility is improved.

The carbon black masterbatch is not particularly limited in the case of a carbon black masterbatch which is usually applicable to polyethylene terephthalate resin.

The black master batch may be 0.1 to 2.0 parts by weight, 0.5 to 1.5 parts by weight, or 0.7 to 1.2 parts by weight based on 100 parts by weight of (A) polyethylene terephthalate resin, and the effect of excellent balance of physical properties within this range have.

The polyethylene terephthalate resin composition further includes at least one selected from the group consisting of a colorant, a releasing agent, a pigment, a dye, a charge control agent, an antibacterial agent, a processing aid, a metal deactivator, a flame retardant, .

For example, the polyethylene terephthalate resin composition has a deviation of Left value and Right value of HDT (4.6 kgf) of 4 ° C or less, 3 ° C or less, 2 ° C or 1 ° C or less, The effect is excellent.

The polyethylene terephthalate resin composition may have an MI (265 DEG C) of 28 to 40 g / 10 min., Or 28 to 38 g / 10 min., And has an excellent moldability within this range.

The present invention is characterized by a molded article comprising a polyethylene terephthalate resin composition.

The injection-molded article may be, for example, a structural material for construction, office furniture, an automobile engine room cover, a housing or an architectural apparatus.

It will be apparent to those skilled in the art that various modifications and variations can be made in the present invention without departing from the spirit or scope of the present invention. Such variations and modifications are intended to be within the scope of the appended claims.

[Example]

The compounds used in the following Table 1 are as follows.

- PET: JSB598 from Huvis

- Heat stabilizers: Irganox 1010, Irgafos 168

- Glass fiber: Owens Corning G / F 183F

- Lactic A: Montanic acid (Licowax E from Clariant)

- Lubricant B: High density polyethylene (LC206N manufactured by Lion Chemtech)

- Lubricant C: EP184 (Hanyang Hwaseong)

- Lubricant D: PETS-AHS (FACI)

- Rubber: ethylene methacrylate rubber (Evaloy 1330AC from DuPont)

- Nucleating agent: ionomer (Surlyn 8920 from DuPont)

- Inorganic filler: Mica (200DX from Nippon Rika)

- M / B (carbon black master batch): NB9082 of Woosung Chemical Co.

Example  1 to 2 and Comparative Example  1 to 8

The ingredients and the contents of Table 1 were uniformly mixed with a super mixer, and then melt-kneaded at 200 to 280 ° C using a twin-screw extruder to produce pellets through extrusion. It was dried at 120 DEG C for 8 hours or more and molded at an injection temperature range of 200 to 280 DEG C and a mold temperature range of 60 to 100 DEG C using an 80MT ENGEL injection machine.

 [Test Example]

The properties of the specimens prepared in Examples 1 to 2 and Comparative Examples 1 to 8 were measured by the following methods, and the results are shown in Tables 1 and 2 below.

* Crystallization temperature (Tc): Measured by DSC (differential scanning calorimeter) at 20 ° C / min.

* HDT (° C, 4.6 kgf): Two trapezoidal specimens were measured with one left and one right according to ASTM D648.

* Specific gravity: measured according to ASTM D792.

* Flowability (g / 10 min., 265 캜, 5.0 kg): Measured according to ASTM D1238.

Tensile strength (kgf / cm 2 ): Measured according to ASTM D638.

Flexural Strength: Measured according to ASTM D790.

Impact strength (kgf · cm / cm): Measured according to ASTM D256.

Example 1 Example 2 Comparative Example 1 Comparative Example 2 Comparative Example 3 Comparative Example 4 PET (parts by weight) 100 100 100 100 100 100 Lubricant
(Parts by weight) A 0.91 B 0.92 Rubber (parts by weight) 12.7 12.8 0 9.1 9.1 12.7 Nucleating agent (parts by weight) 3.6 3.7 0 7.3 7.3 3.6 Glass fiber (parts by weight) 18.2 18.3 31.2 36.4 18.2 18.2 Inorganic filler (parts by weight) 45.5 45.8 23.4 27.3 45.5 45.5 Heat stabilizer (parts by weight) 0.91 0.92 0.78 0.91 0.91 0.91 M / B (parts by weight) 0.91 0.92 0.78 0.91 0.91 0.91 Properties HDT
(4.6 kgf) Left 235 238 243 237 236 237 Right 236 237 234 236 235 236 importance 1.57 1.57 1.61 1.57 1.57 1.57 Flowability (MI) 33 34 36 19 24 23 The tensile strength 800 820 1,070 920 830 810 Flexural strength 81,000 75,000 109,000 84,000 79,000 81,500 Impact strength 5.6 5.4 4.0 5.2 5.1 5.5

Comparative Example 5 Comparative Example 6 Comparative Example 7 Comparative Example 8 PET (parts by weight) 100 100 100 100 Lubricant
(Parts by weight) A 0.88 B 0.88 C 0.92 D 0.92 Rubber (parts by weight) 12.8 12.8 12.4 12.4 Nucleating agent (parts by weight) 3.7 3.7 0 0 Glass fiber (parts by weight) 18.3 18.3 17.7 17.7 Inorganic filler (parts by weight) 45.3 45.8 44.2 44.2 Heat stabilizer (parts by weight) 0.92 0.92 0.88 0.88 M / B (parts by weight) 0.91 0.91 0.91 0.91 Properties HDT
(4.6 kgf) Left 238.7 237.6 240 239 Right 237.2 236.4 231 232 importance 1.55 1.55 1.56 1.56 Flowability (MI) 13 12 37 35 The tensile strength 860 850 930 940 Flexural strength 83,000 83,000 93,000 93,000 Impact strength 6.0 6.0 5.8 5.7

As shown in Table 1, in Examples 1 and 2 including the rubber and lubricant of the present invention, the deviation between the Left value and the Right value of HDT was 1 占 폚 or less and the heat stability was excellent and the specific gravity And the flowability was improved. In Comparative Example 1 in which the nucleating agent, lubricant and rubber were not included, the deviation between the Left value and the Right value of the HDT rapidly increased and the impact strength was lowered. In Comparative Examples 2 to 6 in which the lubricant of the present invention was not used, In Comparative Examples 7 and 8 in which the lubricant of the present invention was included but the nucleating agent was not included, the deviation between the Left value and Right value of the HDT rapidly increased.

Claims (16)

(A) a polyethylene terephthalate resin;
(B) a (meth) acrylate rubber;
(C) at least one nucleating agent selected from the group consisting of a neutralized unsaturated acid polymer, a neutralized saturated fatty acid wax and an ionomer; And
(D) a lubricant;
Wherein the poly (ethylene terephthalate) resin composition is a polyethylene terephthalate resin composition.
The method according to claim 1,
Wherein the (B) (meth) acrylate-based rubber is an ethylene-methacrylate copolymer, an ethylene-butyl acrylate-glycidyl methacrylate copolymer, or a mixture thereof.
The method according to claim 1,
Wherein the neutralized unsaturated acid polymer is a neutralized ethylene-methacrylic acid copolymer.
The method according to claim 1,
Wherein the neutralized saturated fatty acid is a neutralized montanic acid wax.
The method according to claim 1,
Wherein the lubricant comprises at least one selected from the group consisting of high density polyethylene (HDPE), montanic acid, and pentaerythritol tetrastearate.
The method according to claim 1,
Wherein the polyethylene terephthalate resin has a crystallization temperature (Tc) of 190 to 220 占 폚.
The method according to claim 1,
Wherein the polyethylene terephthalate resin composition comprises glass fiber, an inorganic filler, or both.
8. The method of claim 7,
Wherein the glass fiber, the inorganic filler, or both are contained in an amount of 45 to 75 parts by weight based on 100 parts by weight of the polyethylene terephthalate resin composition.
The method according to claim 1,
Wherein the weight ratio of the (meth) acrylate-based rubber and the nucleating agent is 6 to 8: 3 to 1. The poly (ethylene terephthalate) resin composition according to claim 1,
The method according to claim 1,
Wherein the polyethylene terephthalate resin composition has a deviation of Left value and Right value of HDT (4.6 kgf) of 4 占 폚 or less.
The method according to claim 1,
Wherein the polyethylene terephthalate resin composition has a fluidity (265 DEG C) of 28 to 40 g / 10 min.
The method according to claim 1,
Wherein the polyethylene terephthalate resin composition further comprises a black master batch.
The method according to claim 1,
The polyethylene terephthalate resin composition may contain,
(A) 100 parts by weight of a polyethylene terephthalate resin;
(B) 5 to 20 parts by weight of a (meth) acrylate rubber;
(C) 1 to 7 parts by weight of at least one nucleating agent selected from the group consisting of a neutralized unsaturated acid polymer, a saturated fatty acid wax and an ionomer; And
(D) 0.1 to 2 parts by weight of a lubricant;
Wherein the poly (ethylene terephthalate) resin composition is a polyethylene terephthalate resin composition.
The method according to claim 1,
The polyethylene terephthalate resin composition may include at least one selected from the group consisting of a colorant, a releasing agent, a pigment, a dye, an antistatic agent, an antibacterial agent, a processing aid, a metal deactivator, a flame retardant, Wherein the polyethylene terephthalate resin composition is a polyethylene terephthalate resin composition.
An injection-molded article comprising the polyethylene terephthalate resin composition according to any one of claims 1 to 14.
16. The method of claim 15,
Wherein the injection-molded article is a structural member for construction, office furniture, an automobile engine room cover, a housing or a construction machine.
KR1020150123036A 2015-08-31 2015-08-31 Polyethyleneterephthalate resin composition and injection molding product KR102012953B1 (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20180117936A (en) * 2017-04-20 2018-10-30 주식회사 엘지생활건강 Beverage container and method of fabricating the same
CN109233220A (en) * 2018-08-27 2019-01-18 华润化学材料科技有限公司 A kind of master batch and its Preparation Method that PET melt mobility can be improved

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR840001450B1 (en) * 1980-06-04 1984-09-27 데이진 가부시끼가이샤 Glass fiber-reinforced thermoplastic polyester compositions
JP2008506012A (en) 2004-07-08 2008-02-28 ティコナ・エルエルシー High gloss PET molding composition and articles made therefrom
KR20100045695A (en) * 2008-10-24 2010-05-04 현대자동차주식회사 Recycling polyethyleneterephthalate composite and manufacturing method of thereof

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR840001450B1 (en) * 1980-06-04 1984-09-27 데이진 가부시끼가이샤 Glass fiber-reinforced thermoplastic polyester compositions
JP2008506012A (en) 2004-07-08 2008-02-28 ティコナ・エルエルシー High gloss PET molding composition and articles made therefrom
KR20100045695A (en) * 2008-10-24 2010-05-04 현대자동차주식회사 Recycling polyethyleneterephthalate composite and manufacturing method of thereof

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20180117936A (en) * 2017-04-20 2018-10-30 주식회사 엘지생활건강 Beverage container and method of fabricating the same
CN109233220A (en) * 2018-08-27 2019-01-18 华润化学材料科技有限公司 A kind of master batch and its Preparation Method that PET melt mobility can be improved

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