Synthetic resins or natural rubbers -- part of the class 520 ser – Synthetic resins – From silicon reactant having at least one...
Reexamination Certificate
2000-10-11
2002-06-04
Dawson, Robert (Department: 1712)
Synthetic resins or natural rubbers -- part of the class 520 ser
Synthetic resins
From silicon reactant having at least one...
C528S010000, C528S031000, C528S033000, C528S039000, C556S466000, C556S467000, C556S484000, C525S474000
Reexamination Certificate
active
06399733
ABSTRACT:
BACKGROUND OF THE INVENTION
The present invention relates to a process for preparing a highly pure silicone ladder polymer. More particularly, the invention relates to a process for preparing a highly pure silicone ladder polymer capable of being employed preferably as a protective film and an interlaminar insulating film of a semiconductor.
A silicone ladder polymer has been employed as a protective film and an interlaminar insulating film of an electronic part or a semiconductor device because of its excellence in terms of the heat resistance, the electric insulating capability and the chemical resistance which is attributable to its molecular structure. A conventional process for preparing such silicone ladder polymer is proposed in a reference (Japanese Unexamined Patent Publication No. 1985-124943). In a conventional process, triethoxysilane is first hydrolyzed in a solution of an organic solvent and then allowed to polymerize under reduced pressure to modify terminals with dimethylchlorosilane and then purified with an organic solvent, whereby yielding a silicone ladder polymer.
However, even if such conventional process can produce a silicone ladder polymer, the resulting silicone ladder polymer contains a large amount of impurities and by-products. This is because of an insufficient purification after the modification of terminals or because of a manufacturing condition making it difficult to remove the impurities and the by-products, such as a temperature as high as 35° C. at which a reaction after the hydrolysis is conducted. In addition, the molecular weight of the resultant silicone ladder polymer is limited to at the highest 100000, resulting in a difficulty in forming a thick film.
SUMMARY OF THE INVENTION
Thus, the present invention relates to:
a process for preparing a highly pure silicone ladder polymer comprising sodium, potassium, iron, copper, lead, magnesium, maganese and chlorine, each in amount of at most 1 ppm, and uranium and thorium, each in an amount of at most 1 ppb, and represented by the general formula (1):
wherein R
1
and R
2
are the same or different and are selected from the group consisting of a fluorine atom, a hydrogen atom, a lower alkyl group, an alkenyl group, an aryl group, a lower alkyl group in which a part or all of hydrogen atoms are substituted with a fluorine atom, an alkenyl group in which a part or all of hydrogen atoms are substituted with a fluorine atom and an aryl group in which a part or all of hydrogen atoms are substituted with a fluorine atom; R
3
, R
4
, R
5
, and R
6
are the same or different and are selected from the group consisting of a hydrogen atom, a lower alkyl group and a lower alkyl group in which a part or all of hydrogen atoms are substituted with a fluorine atom; and n represents an integer of 5 to 10000, which comprises:
(a) obtaining a prepolymer in which at least one organosilane compound is dissolved in an organic solvent and hydrolyzed with ultrapure water;
(b) washing the obtained prepolymer with ultrapure water; and,
(c) dissolving the washed prepolymer in an organic solvent and heating without a catalyst;
a process as described above, wherein the organosilane compound is represented by the general formula (2):
R
7
SiOR
8
OR
9
OR
10
wherein R
7
is selected from the group consisting of a fluorine atom, a hydrogen atom, a lower alkyl group, an alkenyl group, an aryl group, a lower alkyl group in which a part or all of hydrogen atoms are substituted with a fluorine atom, an alkenyl group in which a part or all of hydrogen atoms are substituted with a fluorine atom and an aryl group in which a part or all of hydrogen atoms are substituted with a fluorine atom; and R
8
, R
9
and R
10
are the same or different and are selected from the group consisting of a hydrogen atom, a lower alkyl group and a lower alkyl group in which a part or all of hydrogen atoms are substituted with a fluorine atom;
a process as described above wherein the organosilane compound is represented by the general formula (3):
R
11
SiCl
3
wherein R
11
is selected from the group consisting of a fluorine atom, a hydrogen atom, a lower alkyl group, an alkenyl group, an aryl group, a lower alkyl group in which a part or all of hydrogen atoms are substituted with a fluorine atom, an alkenyl group in which a part or all of hydrogen atoms are substituted with a fluorine atom and an aryl group in which a part or all of hydrogen atoms are substituted with a fluorine atom;
a process for preparing a highly pure silicone ladder polymer comprising sodium, potassium, iron, copper, lead, magnesium, manganese and chlorine, each in an amount of at most 1 ppm, and uranium and thorium, each in an amount of at most 1 ppb, represented by the general formula (1):
wherein R
1
and R
2
are the same or different and are selected from the group consisting of a fluorine atom, a hydrogen atom, a lower alkyl group, an alkenyl group, an aryl group, a lower alkyl group in which a part or all of hydrogen atoms are substituted with a fluorine atom, an alkenyl group in which a part or all of hydrogen atoms are substituted with a fluorine atom and an aryl group in which a part or all of hydrogen atoms are substituted with a fluorine atom; R
3
, R
4
, R
5
and R
6
are the same or different and are selected from the group consisting of a hydrogen atom, a lower alkyl group and a lower alkyl group in which a part or all of hydrogen atoms are substituted with a fluorine atom; and n represents an integer of 5 to 10000, which comprises:
(a) obtaining a prepolymer in which at least one organosilane compound is dissolved in an organic solvent and hydrolyzed with ultrapure water; and,
(b) dissolving the obtained prepolymer in an organic solvent and heating without a catalyst;
a process as described above wherein said organosilane compound is represented by general formula (2):
R
7
SiOR
8
OR
9
OR
10
wherein R
7
is selected from the group consisting of a fluorine atom, a hydrogen atom, a lower alkyl group, an alkenyl group, an aryl group, a lower alkyl group in which a part or all of hydrogen atoms are substituted with a fluorine atom, an alkenyl group in which a part or all of hydrogen atoms are substituted with a fluorine atom and an aryl group in which a part or all of hydrogen atoms are substituted with a fluorine atom; and R
8
, R
9
and R
10
are the same or different and are selected from the group consisting of a hydrogen atom, a lower alkyl group and a lower alkyl group in which a part or all of hydrogen atoms are substituted with a fluorine atom;
a process as described above wherein said organosilane compound is represented by general formula (3):
R
11
SiCl
3
wherein R
11
is selected from the group consisting of a fluorine atom, a hydrogen atom, a lower alkyl group, an alkenyl group, an aryl group, a lower alkyl group in which a part or all of hydrogen atoms are substituted with a fluorine atom, an alkenyl group in which a part or all of hydrogen atoms are substituted with a fluorine atom and an aryl group in which a part or all of hydrogen atoms are substituted with a fluorine atom;
a process as described above further comprising (d) a step of pulverizing the resultant highly pure silicone ladder polymer and stirring with a poor solvent;
a process as described above further comprising (c) a step of pulverizing the resultant highly pure silicone ladder polymer and stirring with a poor solvent;
a process as described above further comprising (d) a step of passing a solution of the resultant highly pure silicone ladder polymer in an organic solvent through an impurity-removing device to effect a purification; and
a process as described above further comprising (c) a step of passing a solution of the resultant highly pure silicone ladder polymer in an organic solvent through an impurity-removing device to effect a purification.
DETAILED DESCRIPTION
The present invention is further detailed below.
The invention relates to a process for preparing a highly pure silicone ladder polymer comprising sodium, potassium, iron, copper, l
Taguchi Motohisa
Yamamoto Shigeyuki
Yasuda Naoki
Dawson Robert
Leydig , Voit & Mayer, Ltd.
Mitsubishi Denki & Kabushiki Kaisha
Robertson Jeffrey B.
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