JPH0616924A - Resin composition improved in weld characteristic - Google Patents

Abstract

PURPOSE:To obtain a resin composition improved in weld characteristic, composed of a polyolefinic resin, a polyphenylene ether resin, etc., and a vinyl aromatic compound-conjugated diene block copolymer, etc., having high oil, chemical, heat and impact resistances and useful as industrial parts, etc. CONSTITUTION:The resin composition is obtained by blending (A) a polyolefinic resin (e.g. isotactic polypropylene) with (B) a polyphenylene ether resin or the polyphenylene ether resin containing polystyrene resin or a rubber-reinforced polystyrene resin and (C) a vinyl aromatic compound-conjugated diene compound block copolymer (e.g. styrene/butadiene block copolymer) or a cross-linked substance of its partially hydrogenated copolymer. When this resin composition is extracted with a mixed xylene in a Soxhlet extractor for 24 hr, it has >=80wt.% amount of a get remaining as an insoluble content on a No.84 filter paper thimble based on the amount of the component (C) in the composition before the extraction. Furthermore, this resin composition is improved in weld characteristics.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a PPE alloy having excellent oil resistance, chemical resistance, heat resistance and impact resistance, and excellent weld characteristics of injection molded articles, in the electric and electronic fields, automobiles. The present invention provides a resin composition that can be used in various fields including various industrial materials.

[0002]

2. Description of the Related Art Polyphenylene ether has excellent mechanical properties, electrical properties, heat resistance, low water absorption and excellent dimensional stability, but has the disadvantage of poor moldability and impact resistance. By blending with high-impact polystyrene to improve molding processability and impact resistance, it is widely used as resin moldings for industrial parts, electric / electronic parts, office equipment housings, automobile parts, precision parts, etc. . However, a classical polyphenylene ether resin composition composed of this polyphenylene ether and high-impact polystyrene (disclosed in US Pat. No. 3,383,435).
Has improved impact resistance, but has a drawback of poor chemical resistance.

For this reason, for example, US Pat.
No. 1 and Japanese Examined Patent Publication No. 42-7069 propose to improve chemical resistance and impact resistance by blending polyphenylene ether with polyolefin, but the delamination phenomenon is not so practical. is the current situation. Further, US Pat. No. 3,994,856 describes improvement of impact resistance and chemical resistance by blending a polyphenylene ether and a styrene resin with a hydrogenated block copolymer, and US Pat.
No. 145377 discloses polyphenylene ether,
Or impact resistance by blending a polyphenylene ether and a styrene resin with a premixture of polyolefin / hydrogenated block copolymer = 20 to 80 parts by weight / 80 to 20 parts by weight and a hydrogenated block copolymer,
There is a description regarding the improvement of chemical resistance, and further, U.S. Pat. Nos. 4,166,055, 4,239,673 and 42422.
No. 63 describes improving impact resistance by blending polyphenylene ether with a block or hydrogenated block copolymer and a polyolefin. And US Pat. No. 4,383,032, European Patent No. 115712 and Dutch Patent No. 7410.
No. 861 describes improving the impact resistance by blending polyphenylene ether with a polyolefin and a hydrogenated block copolymer.

[0004]

In the resin composition obtained from the polyolefin / polyphenylene ether / hydrogenated block copolymer obtained in the above-mentioned prior art, the hydrogenated block used as the admixture of polyolefin and polyphenylene ether. Since the conjugated diene block of the copolymer is saturated by hydrogenation, the dispersed particles of the hydrogenated block copolymer are uncrosslinked uncrosslinked particles. A molded article obtained by injection molding of the resin composition containing the uncrosslinked dispersed particles is observed by observing the resin flow direction with an electron microscope, and it is observed that the dispersed particles are stretched in the flow direction and oriented in an elongated shape. .

The shape of the dispersed particles in the weld portion of this injection-molded article observed by an electron microscope is peculiar. That is, since the weld portion of the injection-molded product is a portion where the flow of the resin collides, it is observed that the dispersed particles in this portion have a strong orientation of 90 ° with the flow direction, that is, parallel to the weld line. These welded portions have extremely small tensile elongation and low tensile strength. Also, the impact strength of IZOD in this weld portion tends to be extremely lower than that in the non-weld portion. From these facts, the resin composition having a disperse phase having a strong orientation has a defect that the weld portion is brittle.

Further, since a molded product obtained by injection molding a resin composition having a strong orientation of the dispersed phase is frozen at room temperature with the dispersed phase being stretched, a heat shock test at, for example, -40 ° C to 130 ° C is performed. When it is carried out, the dispersed phase tries to relax the stress, so that it has a drawback that cracks easily occur. For this reason, if you use a molded product molded at a high injection speed that tends to cause a shear rate or a molded product molded with a mold with a small gate diameter for a long period of time in an environment where heating and cooling are repeated, countless fine cracks will appear on the surface. And cracks grow and cracks occur.

[0007]

The present invention provides (a) a polyolefin resin, (b) a polyphenylene ether resin,
Or a polyphenylene ether resin containing a polystyrene resin or a rubber-reinforced polystyrene resin, and (c)
A resin composition comprising a crosslinked product of a vinyl aromatic compound-conjugated diene compound block copolymer or a partially hydrogenated product thereof, wherein the composition was No. 1 when soxhlet extracted with mixed xylene for 24 hours. The resin having improved weld characteristics, characterized in that the amount of gel remaining as an insoluble component on the cylindrical paper of No. 84 is 80% by weight or more of the amount of the component (c) contained in the composition before extraction. It relates to a composition.

The resin composition of the present invention comprises a vinyl aromatic compound-conjugated diene compound block copolymer constituting the dispersed particles or a partially hydrogenated product thereof (hereinafter referred to as rubber particles).
Are crosslinked, as compared with the case of a resin composition using the above-mentioned completely hydrogenated block copolymer as an admixture,
When the injection-molded piece is observed by a TEM photograph, the dispersed particles have a small orientation, and are characterized by retaining a relatively round particle shape. As a result, the welded part of the injection-molded article made of the composition of the present invention has a feature that the welded line is difficult to visually recognize. In addition, when the weld part is evaluated by a tensile test, it has a feature of being stretched by 1% or more.
Further, the tensile strength is maintained at 70% or more of the non-weld strength of the non-weld portion, and if it is good, the tensile strength is improved to the extent that it does not break at the weld line. Even in the IZOD impact test of the welded portion, it has 70% or more of the non-welded portion, and the composition according to the present invention eliminates the drawback that the welded portion of the injection-molded article is brittle.

The polyolefin used in the present invention has a number average molecular weight of 3000 which is used as a usual molding material.
0 or more polyolefins, for example, low density polyethylene, high density polyethylene, ultra high molecular weight high density polyethylene, linear low density polyethylene, isotactic polypropylene, ultra high molecular weight isotactic polypropylene,
Poly (4-methyl-1-pentene), polybutene-1,
Ultra low density polyethylene having a density of less than 0.90, a copolymer of two or more compounds selected from ethylene, propylene, other α-olefins, unsaturated carboxylic acids or their derivatives, for example, ethylene / butene-1. Copolymer, ethylene- (meth) acrylic acid copolymer, ethylene- (meth) acrylic acid ester copolymer, propylene / ethylene (random, block) copolymer, propylene / 1-
Examples include hexene copolymers and propylene / 4-methyl-1-pentene copolymers. These polyolefins may be used alone or in combination of two or more. Of these polyolefins, low density polyethylene, high density polyethylene, isotactic polypropylene, propylene / ethylene block copolymer and the like are preferable.

The polyolefin used in the present invention is
In addition to the above-mentioned polyolefin, the polyolefin and α, β-unsaturated carboxylic acid or its derivative are melted or in solution in the presence or absence of a radical generator at a temperature of 30 to 350 ° C. A known modified (0.01 to 10% by weight of the α, β-unsaturated carboxylic acid or its derivative is grafted or added) polyolefin obtained by the reaction may be used, and further, the above-mentioned polyolefin and the modified polyolefin may be used. It may be a mixture in any proportion.

Next, the polyphenylene ether (hereinafter simply referred to as PPE) used in the present invention has a bonding unit:

[0012]

[Chemical 1]

Here, R ₁ , R ₂ , R ₃ and R ₄ are each hydrogen, halogen, a primary or secondary lower alkyl group having 1 to 7 carbon atoms, a phenyl group, a haloalkyl group, an aminoalkyl. A group, a hydrocarbonoxy group or a halohydrocarbonoxy group in which at least two carbon atoms separate a halogen atom and an oxygen atom, and they may be the same or different. And reduced viscosity (0.5 g / dl, chloroform solution,
A homopolymer and / or a copolymer having a measurement temperature of 30 ° C.) of 0.15 to 0.70, more preferably 0.20 to 0.60.

Specific examples of these PPEs include, for example, poly (2,6-dimethyl-1,4-phenylene ether), poly (2-methyl-6-ethyl-1,4-phenylene ether), and poly (2-methyl-6-ethyl-1,4-phenylene ether). (2-methyl-6-phenyl-
1,4-phenylene ether), poly (2,6-dichloro-1,4-phenylene ether), and the like, and further 2,6-dimethylphenol and other phenols (for example, 2,3,6-trimethyl). Also included are polyphenylene ether copolymers such as copolymers with phenol and 2-methyl-6-butylphenol). Among them, poly (2,6-dimethyl-1,4-phenylene ether),
A copolymer of 2,6-dimethylphenol and 2,3,6-trimethylphenol is preferable, and poly (2,6-diphenylphenol)
6-dimethyl-1,4-phenylene ether) is preferred. The PPE is not particularly limited as long as it can be obtained by a known method. For example, US Pat.
Using the complex of cuprous chloride and amine by Hay described in No. 06874 as a catalyst, for example, 2,6
-It can be easily produced by oxidative polymerization of xylenol. In addition to these, U.S. Pat. Nos. 3,306,685, 3,257,357 and 3,257,358, JP-B-52-7880, JP-A-50- 5
It can be easily produced by the methods described in JP 1197 and JP 63-152628.

The PPE used in the present invention is, in addition to the above-mentioned PPE, the PPE and the α, β unsaturated carboxylic acid or its derivative in a molten state or in a solution in the presence or absence of a radical generator. 8 in the state or slurry state
Known modification (0.01 to 10% by weight of the α, β-unsaturated carboxylic acid or its derivative grafted or added) obtained by reacting at a temperature of 0 to 350 ° C P
It may be PE, and further, the above PPE and the modified PPE.
The mixture may be in any proportion.

In addition to the above-mentioned PPE, those obtained by adding polystyrene to these PPE in an amount not exceeding 50% by weight can be preferably used. The partially hydrogenated product of vinyl aromatic compound-conjugated diene compound block copolymer or vinyl aromatic compound-conjugated diene compound block copolymer (hereinafter abbreviated as TR, partially hydrogenated TR) used in the present invention is polyolefin and PPE. It acts as an admixture (hereinafter abbreviated as "compatibilizer").

These TRs or partially hydrogenated TRs can be produced in a wide range of properties from soft elastomeric properties to hard resinous properties depending on the content ratio of aromatic compound blocks and conjugated diene compound blocks in the molecule. Also, the performance as a compatibilizer can be changed from one having a high affinity for PPE to one having a high affinity for a polyolefin resin. These TRs are obtained by copolymerizing a vinyl aromatic compound and a conjugated diene compound, and partially hydrogenated TRs are obtained by hydrogenating an olefinic double bond based on the conjugated diene compound of TR up to 90%. can get. Examples of the vinyl aromatic compound constituting this compatibilizer include styrene, α-methylstyrene, vinyltoluene, p-third
One or more of butyl styrene and diphenyl ethylene can be selected, and styrene is preferable.
Examples of the conjugated diene compound include butadiene,
Isoprene, 3-pentadiene, 2,3-dimethyl-
One or more kinds are selected from 1,3-butadiene and the like, and among them, butadiene, isoprene and a combination thereof are preferable. An example of such a compatibilizer is styrene-obtained by anionic polymerization.
A butadiene block copolymer, and further a partial water additive of this styrene-butadiene block copolymer,
These are, for example, British Patent No. 1130770, US Pat. No. 3,281,383 and No. 36.
39517 and the method described in British Patent No. 1
It can be easily produced by the method described in No. 020720, U.S. Pat. No. 3,333,024 and No. 450157.

These compatibilizers are usually 1
It is a copolymer obtained by copolymerizing 5 to 95% of the above vinyl aromatic compound. The amount of the vinyl aromatic compound in this copolymer can be arbitrarily selected in consideration of the miscibility between the polyolefin and PPE. As this compatibilizer, for example, those commercially available from Asahi Kasei Kogyo Co., Ltd. under the trade names of “Tafprene”, “Sorprene”, “Tuffden” and “Asaprene” can be used. The composition of the present invention contains the above-mentioned components, and the amount ratio of such components is determined in consideration of the heat resistance and oil resistance of the resulting composition.

The content range of the polyolefin of the present invention is usually 5 to 85% based on the resin portion of the composition. 5%
If it is less than 80%, the oil resistance of the resulting composition is insufficient, and if it exceeds 85%, the effect of improving the heat resistance due to the addition of PPE cannot be obtained. The range of the content of PPE is 15 to 85% based on the resin portion of the composition. When PPE exceeds 85%, the fluidity of the composition is deteriorated and the elongation of the weld portion also decreases, and when it is less than 15%, the heat resistance is insufficient.

TR used in the present invention or partially hydrogenated T
The amount of R added is 10 to 300%, and more preferably 50 to 200% with respect to 100, which is a small component of either the polyolefin resin or the polyphenylene ether resin. In the PPE-rich composition, the TR used or the partially hydrogenated TR is preferably one having a relatively high amount of bound vinyl aromatic compound (hereinafter abbreviated as the amount of bound styrene), and conversely, in the composition rich in polyolefin, a low vinyl aromatic compound. When TR contained or TR partially hydrogenated is used, a composition having excellent compatibility tends to be obtained.

In the present invention, the rubber particles are crosslinked by utilizing the residual olefinic double bond of TR or partially hydrogenated TR. As a method of crosslinking, a method of treating rubber particles with an organic peroxide is used. Any organic peroxide may be used as long as it can crosslink rubber particles, but since it is easiest to add and extrude at the same time as each component at the time of producing the composition, it is possible to control the decomposition temperature at a high temperature. Those that have are preferred. Specific examples of the organic peroxide include di-t-butyl peroxide, dicumyl peroxide, benzoyl peroxide, 1,1-bis (t
-Butylperoxy) 3,3,5-trimethylcyclohexane, lauroyl peroxide, cumene hydroperoxide and the like. The amount of organic peroxide added is 0.01 with respect to the amount of TR or partially hydrogenated TR used.
Is in the range of 5.0% by weight. If the added amount of the organic peroxide exceeds 5%, the crosslinking of the rubber particles will proceed too much and the impact resistance of the composition will be deteriorated, which is not preferable. Does not reach.

Further, the composition of the present invention was soxhlet-extracted from the resin composition with mixed xylene for 24 hours. On the cylindrical filter paper 84, 80% by weight or more of TR contained in the composition or partially hydrogenated TR remains as an insoluble gel. The xylene in the gel remaining on the cylindrical filter paper by Soxhlet extraction is dried under reduced pressure at 130 ° C., and the gel content is calculated by weighing. When the amount of the gel component is less than 80% by weight, the crosslinking is insufficient and the sufficient improvement of the weld physical properties, which is a feature of the present invention, cannot be achieved. In the present invention, the No. after soxhlet extraction is performed. The amount of insoluble gel remaining on the cylindrical filter paper of No. 84, the flow direction of the test piece injection-molded with the composition of the present invention, and the flow direction of the particle diameter of the dispersed rubber particles observed in the central part with an electron microscope (major axis diameter) ) And the ratio of the anti-flow direction (minor axis diameter) are observed. That is, the amount of gel in the Soxhlet extraction is outside the range of the present invention.
If it is less than wt%, the ratio of the particle diameter of the dispersed rubber particles observed in an electron microscope to the flow direction and the counter flow direction becomes large, and the particles tend to be oriented like a string. On the contrary, as the amount of the soxhlet-extracted gel exceeds 80% by weight, the dispersed rubber particles observed in the electron micrograph become closer to spherical rather than elliptical. Therefore, the ratio of the particle size of the dispersed rubber particles to the flow direction and the counter-flow direction serves as a measure of the degree of orientation, and at the same time represents the degree of gelation of the dispersed rubber particles. When the ratio of the particle size of the dispersed rubber particles to the flow direction and the counter flow direction is in the range of 1 to 5, the particles are spherical or elliptical, and the weld properties are sufficiently improved, and the composition has tensile elongation and impact resistance of the weld portion. The thing is obtained.

In the present invention, in addition to the above-mentioned components, other additional components, such as an aromatic halogen flame retardant, antimony trioxide, and triphenyl phosphate, may be used as needed, as long as the characteristics and effects of the present invention are not impaired. Such as phosphorus-based flame retardants, antioxidants, weather resistance improvers, nucleating agents for polyolefins, lubricants, inorganic and organic fillers and reinforcing materials (glass fiber, carbon fiber, whiskers, mica, calcium carbonate, titanic acid) Potassium, etc.), various colorants, release agents, etc. may be added. The composition of the present invention is produced by melt-kneading the components shown in the claims. Various melt-kneaders can be used, and specific examples thereof include a single-screw extruder, a twin-screw extruder, various kneaders, brabenders, and heating rolls. The preferable kneading temperature is 220 to 300 ° C., more preferably 230.
It is good to carry out in the range of up to 280 ° C. The molding method of the resin composition of the present invention is not particularly limited as long as it is a commonly used molding method such as injection molding, extrusion molding, compression molding and blow molding.

[0024]

The present invention will be described in more detail with reference to the following examples, but it goes without saying that the scope of the present invention is not limited thereto.

[0025]

Example 1 Polyphenylene ether resin powder (reduced viscosity ηsp / c = 0.51 0.5 g / deciliter,
Chloroform solution, measured at 30 ° C.) 45 parts by weight, isotactic polypropylene resin (Asahi Kasei Polypropylene, E1100) 20 parts by weight, styrene / butadiene /
Partially hydrogenated TR (number average molecular weight: 810,000, bound styrene content 50%) in which 80% of olefinic double bonds in the polybutadiene block were saturated by hydrogenating SBS type TR having a block structure of styrene ) 35 parts by weight, antioxidant (Irganox 1010, Ciba-Geigy, Switzerland) 0.5 parts by weight, di-t-butyl peroxide 0.05 parts by weight diluted 10 times with acetone, and blended using a Henschel mixer. Rear co-rotating twin-screw extruder (ZSK25, WEMER & PFL
L / D = 13.4, (π of all kneading blocks during screw design using ELDERER, Germany)
・ D · N / h) = 98.1, melted and kneaded at a set temperature of 250 ° C. to obtain an extruded composition. 250-26 this
Tensile dumbbell for evaluation of 1/8 inch weld (thickness 1 using a screw inline type injection molding machine set at 0 ° C)
A dumbbell for / 8 inch tensile test was used to insert resin from both gates so that a weld line would appear in the center of the test piece) and a normal dumbbell for ⅛ inch tensile test.

Weld tensile test using these test pieces
Test and non-weld tensile test
Tensile elongation 11.0%, tensile breaking strength 200.0kg
/ Cm²The tensile strength of the non-weld part is 130%.
Tensile breaking strength 230kg / cm ²Met. Also these
Weld line and weld using tensile test piece
The test piece without the line has a notch in the center.
The test piece was an IZOD evaluation test piece. Use these test pieces
Weld and non-weld IZOD impact test
Welded IZOD impact value 25.2 kg · cm
/ Cm, IZOD impact value of non-weld part 26.0kg ・
It was cm / cm.

10.0 g of pellets obtained by the above extrusion
Was precisely weighed and subjected to Soxhlet extraction for 24 hours with 300 ml of mixed xylene. No. 84 The gel on the cylindrical filter paper was dried together with the cylindrical filter paper at 130 ° C. under reduced pressure to a constant weight, and the weight of the gel was measured.
%Met. Also, using the above tensile test piece, electron microscope observation in the direction as shown in FIG. 1 (TEM by RuO ₄ staining)
Was carried out.

The ratio of major axis diameter / minor axis diameter of dispersed particles (flow direction / counterflow direction) was 1.7 / 1.

[0029]

Comparative Example 45 parts by weight of polyphenylene ether resin similar to that used in Example 1, 20 parts by weight of isotactic polypropylene resin similar to Example 1, fully hydrogenated styrene / butadiene block polymer (abbreviated as HTR, number average) Molecular weight of 80,000, bound styrene content of 45%, polybutadiene block olefinic double bond hydrogenation rate of 99.8
%) 35 parts by weight, antioxidant (Irganox 101)
0) Example 1 was prepared by treating 0.5 parts by weight in the same manner as in Example 1.
The same evaluation as was performed.

Weld tensile elongation 0.20%, weld tensile breaking strength 85 kg / cm ² , non-weld tensile elongation 120%, non-weld tensile breaking strength 320 kg / c
It was m ² . Further, the gel content in the Soxhlet extraction under the same conditions as in Example 1 was 0%. Dispersed particles observed by an electron microscope in the same direction as in Example 1 did not have a particle shape and were stretched in the direction of flow, and the measurement of the major axis diameter / minor axis diameter was impossible. .

As described above, in the composition in which the dispersed particles are not crosslinked, the orientation of the dispersed particles in the injection-molded product is extremely strong and the adhesion of the weld is poor.

[0032]

Example 2 The same polyphenylene ether resin as in Example 1 (60 parts by weight), Rhodenity polyethylene resin (Asahi Kasei Suntec LD) 12 parts by weight, styrene / butadiene block polymer (Asahi Kasei AFX810, number average molecular weight 10,000,000, bound styrene) 70%) 14 parts by weight, styrene / butadiene block polymer (Asahi Kasei Tuffprene A, number average molecular weight 50000, bound styrene amount 4)
0%) 14 parts by weight, phosphite-based antioxidant (PEP
36, ADEKA STAB, Asahi Denka Co., Ltd. 0.25 parts by weight, hindered phenolic antioxidant (Irganox 101)
(0, Ciba-Geigy, Switzerland) 0.25 parts by weight and 0.05 parts by weight of di-t-butyl peroxide diluted 10 times with acetone were mixed in a Henschel mixer and then treated in the same manner as in Example 1 to prepare a weld for evaluation. A test piece was prepared and evaluated in the same manner as in Example 1.

Weld tensile strength 18%, weld tensile strength 280 kg / cm ² , non-weld tensile strength 32%, non-weld tensile strength 320 kg / cm ^2.
And weld part IZOD impact strength 21 kg · cm /
cm, non-weld part IZOD impact strength 20 kg · cm /
It was cm. Soluble gel by Soxhlet extraction is 98.0%, long axis diameter of average dispersed particles by electron microscope /
The minor axis diameter was 1.3 / 1.

[0034]

Reference Example Using the pellets obtained in Examples 1, 2 and Comparative Example, a screw type in-line injection molding machine set at 250 ° C. to 270 ° C. was used, and the nozzle type bore diameter was 1
mm pinpoint gate with mold temperature 70 ℃ 100 × 1
A flat plate of 00 × 2 mm was molded at an injection speed of 225 mm / sec.

Using these flat plates, -40 ° C x 2 hours ~
105 ° C x 2 hours (6 hours per cycle, repeat this)
The heat shock test was conducted. After the completion of 10 cycles, the sample was taken out and visually observed. In the flat plate of the comparative example, deformation and warpage were large, and innumerable microcracks were observed in the flow direction of the flat plate surface, whereas the flat plates of Examples 1 and 2 showed no change in appearance and had no microcracks. Was not observed at all.

[0036]

EFFECT OF THE INVENTION The resin composition obtained by the present invention has a thin portion which tends to be oriented because it has a characteristic that the weld portion is stretched at the time of injection molding, the weld portion is excellent in strength, and microcracks are hard to enter. It can be preferably used for large-sized molded products and parts materials under severe operating conditions.

[Brief description of drawings]

FIG. 1 is an explanatory diagram of an electron microscope observing method of a composition according to the present invention.

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Claims (1)

[Claims] 1. A polyphenylene ether resin containing (a) a polyolefin resin, (b) a polyphenylene ether resin, or a polystyrene resin or a rubber-reinforced polystyrene resin, and (c) a vinyl aromatic compound-conjugated diene compound block copolymer or a compound thereof. A resin composition comprising a cross-linked product of a partially hydrogenated product, the composition being No. 2 when soxhlet extracted with mixed xylene for 24 hours.
The amount of the gel remaining as an insoluble component on the cylindrical paper of No. 84 is 80% by weight of the amount of the component (c) contained in the composition before extraction.
A resin composition having improved weld characteristics, characterized by the above.