Synthetic resins or natural rubbers -- part of the class 520 ser – Synthetic resins – Processes of preparing a desired or intentional composition...
Reexamination Certificate
1999-04-19
2001-05-29
Mulcahy, Peter D. (Department: 1713)
Synthetic resins or natural rubbers -- part of the class 520 ser
Synthetic resins
Processes of preparing a desired or intentional composition...
C524S265000, C524S267000, C524S269000
Reexamination Certificate
active
06239195
ABSTRACT:
TECHNICAL FIELD
The present invention relates to a thermoplastic resin composition containing a thermoplastic resin and a silane-treated foliated phyllosilicate, and a method for producing the same.
BACKGROUND ART
In order to improved the mechanical properties, the heat resistance, and the like of a thermoplastic resin, a layered clay mineral such as talk and mica have been conventionally used as a filler (see Japanese Publication for Opposition No. 49-18615, Japanese Laid-Open Publication No. 55-16049, and Japanese Publication for Opposition No. 63-53222, for example). By adding a large amount of such layered clay mineral to a thermoplastic resin, the elastic modulus and the heat resistance of the resultant resin composition improves. However, a molded product obtained from the resin composition has the disadvantages of poor appearance, increased specific gravity, and poor color tone. Moreover, the strength, the tenacity, and the like of the resin composition are reduced due to insufficient dispersion of the layered clay mineral or insufficient adhesion between the layered clay mineral and the resin.
A surface treatment agent has generally been used for improving the adhesion between a filler and a resin to prevent the reduction of strength, impact strength, and the like of a resin composition. For example, a composite of a layered clay mineral treated with a silane coupling agent and a polyester resin is disclosed (see Japanese Laid-Open Publication No. 51-24653 and Japanese Laid-Open Publication No. 51-24654, for example). However, the conventional surface treatment method has not yet provided a sufficient effect of improving the strength and the like of the resin composition. Further, even if the surface of the layered clay was treated, the layered clay mineral itself still has an aggregate structure. Therefore, the problems of poor appearance, increase in the specific gravity, and poor color tone of the resultant molded product remained unsolved.
The layered clay mineral normally has an aggregate structure where about a hundred to several thousands of unit layers each having a thickness of about 1 nm are stratified. Therefore, in the above prior art technique, the layered clay mineral dispersed in the thermoplastic resin exists, not as foliated layers, but in the state of the aggregate structure.
If such an aggregate structure of the layered clay mineral could be exfoliated to allow unit layers to be dispersed separately in the thermoplastic resin, the resultant resin would be strengthened by the addition of only a small amount of the layered clay mineral , and the problems of the poor appearance, the increase in the specific gravity, and the poor color tone of the resultant molded product would be overcome. However, no technique that can exfoliated the layered clay mineral to the state of foliated unit layers to disperse the unit layers in the thermoplastic resin uniformly by use of a silane-coupling agent so as to obtain a resin composition having excellent properties has yet been provided.
DISCLOSURE OF THE INVENTION
The object of the present invention is to intend to solve the above-described conventional problems and provide a thermoplastic resin composition excellent in mechanical properties (elastic modulus, strength, impact strength, and the like), heat resistance, and appearance of a molded product by exfoliating an aggregate structure of a layered clay mineral to disperse the layered clay mineral as a number of separate thin layers each having a size of the order of nanometers independently.
As a result of intense examination for attaining the above object, the inventors of the present invention have completed the present invention.
The thermoplastic resin composition of the present invention contains a thermoplastic resin (A) and a silane-treated foliated phyllosilicate (B), wherein the silane-treated foliated phyllosilicate (B) is prepared by introducing a organosilane compound (B
2
) represented by general formula (I):
Y
n
SiX
4-n
(I)
wherein n denotes an integer of 0 to 3, Y denotes independently a substituted or non-substituted hydrocarbon group having 1 to 25 carbon(s), and X denotes independently a hydrolyzable group or a hydroxyl group, into a swellable layered silicate (B
1
), and a value [R
B300
] is 20% or more when the value [R
B300
] is defined as a rate of layers of the silane-treated foliated phyllosilicate (B) of which equivalent area circle diameter [D] is 300 nm or less.
In one embodiment, the thermoplastic resin (A) is at least one type selected from the group consisting of a thermoplastic polyester resin and a polycarbonate resin.
In another embodiment, the swellable layered silicate (B
1
) is at least one type selected from the group consisting of smectite clay and swellable mica.
In still another embodiment, the silane-treated foliated phyllosilicate (B) is prepared by introducing the organosilane compound (B
2
) after the basal spacing of the swellable layered silicate (B
1
) has been expanded.
In still another embodiment, the content of the silane-treated foliated phyllosilicate (B) is 0.1 to 100 parts by weight with respect to 100 parts by weight of the thermoplastic resin (A).
In still another embodiment. the ash content originated from the silane-treated foliated phyllosilicate (B) is 0.1 to 50% by weight.
In a preferred embodiment, the value [R
B300
] is 500 nm or less when the [D
B
] is defined as an average value of the equivalent area circle diameters of the silane-treated foliated phyllosilicate (B).
In still another embodiment, a value [D
B
]/[D
B1
] is 0.010 or less when the value [D
B
] is defined as an average value of the equivalent area circle diameters of the silane-treated foliated phyllosilicate (B) and the value [D
B1
] is defined as an average value of the equivalent area circle diameters of the swellable layered silicate (B
1
).
In still another embodiment, a value [N
B
]/[N
B1
] is 300 or more when the value [N
B
] is defined as the number of foliated layers of the silane-treated foliated phyllosilicate (B) per unit ash content and per unit area, and the value of [N
B1
] is defined as the number of the swellable layered silicate (B
1
) per unit ash content and per unit area.
In still another embodiment, an average thickness of the foliated layers of the silane-treated foliated phyllosilicate (B) dispersed in the thermoplastic resin composition is 20 nm or less.
In still another embodiment, 20% or more of layers of the silane-treated foliated phyllosilicate (B) dispersed in the thermoplastic resin composition have a layer thickness of 5 nm or less.
In still another embodiment, a value [I
B
]/[I
B
] is 0.25 or less when the value [I
B
] is defined as a diffraction intensity of the small angle X-ray diffraction originated from the silane-treated foliated phyllosilicate (B), and the value [I
B
] is defined as a diffraction intensity of small angle X-ray diffraction originated from an aggregate structure of the swellable layered silicate (B
1
).
In still another embodiment, the basal spacing of the silane-treated foliated phyllosilicate (B) in the thermoplastic resin composition is three times or more as large as an initial basal spacing of the swellable layered silicate (B
1
).
According to another aspect of the present invention, the thermoplastic resin composition of the present invention contains a thermoplastic resin (A) and a silane-treated foliated phyllosilicate (B), wherein the silane-treated foliated phyllosilicate (B) is prepared by introducing a organosilane compound (B
2
) represented by general formula (I);
Y
n
SiX
4-n
(I)
wherein n denotes an integer of 0 to 3, Y denotes independently a substituted or non-substituted hydrocarbon group having 1 to 25 carbon(s), and X denotes independently a hydrolyzable group or a hydroxyl group, into a swellable layered silicate (B
1
) after the basal spacing of the swellable lay
Oohara Youichi
Suzuki Noriyuki
Baker & Botts L.L.P.
Kaneka Corporation
Mulcahy Peter D.
LandOfFree
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