Synthetic resins or natural rubbers -- part of the class 520 ser – Synthetic resins – Polymers from only ethylenic monomers or processes of...
Reexamination Certificate
1998-11-23
2003-09-02
Wu, David W. (Department: 1713)
Synthetic resins or natural rubbers -- part of the class 520 ser
Synthetic resins
Polymers from only ethylenic monomers or processes of...
C526S134000, C526S195000, C502S104000, C502S202000, C502S203000
Reexamination Certificate
active
06613850
ABSTRACT:
TECHNICAL FIELD
The present invention relates to a method for feeding a specific boron compound to a reactor, a boron compound having a controlled particle diameter useful as a component of a catalyst for polymerization of an olefin and a method for producing the same. More particularly, it relates to a method for continuously feeding a boron compound useful as a component of a catalyst for polymerization of an olefin to a reactor, particularly an apparatus for preparing a catalyst or a reactor for polymerization of an olefin, said boron compound having a controlled particle diameter, and a method for producing said boron compound.
BACKGROUND ART
Many reports have already been presented on methods for producing olefin polymers with catalysts for olefin polymerization, which uses a transition metal compound (e.g. a metallocene complex or non-metallocene complex) and a specific boron compound. Said boron compound, which is also commercially available in recent years, is usually solid containing large size particles having a particle diameter of several hundreds micrometers to several millimeters, and while it is soluble in toluene to some extent, it has a low solubility in most solvents including saturated hydrocarbons. Therefore, conventionally it has been used in a solution having not so high concentration or used by adding undissolved part of said boron compound remaining in solid form into a vessel.
For example, In Japanese Patent Publication (Kohyo) No. Hei 1-502036 discloses a method for producing an olefin polymer in which tri-n-butylammonium tetrakis(phenyl)borate is suspended in toluene, bis(pentamethylcyclopentadienyl) zirconium dimethyl is added thereto, Cp*
2
Zr(C
6
H
4
)B(C
6
H
5
)
3
<<wherein Cp* represents &eegr;
5
-pentamethylcyclopentadienyl group>> is isolated and used as a catalyst for polymerization of an olefin. In this method, tri-n-butylammonium tetrakis(phenyl)borate is provided in advance in the form of a suspension in toluene in a reactor for preparing a catalyst, and the catalyst is prepared by adding a metallocene complex thereto.
In addition, in U.S. Pat. No. 5,408,017, it is disclosed that a method for producing an olefin polymer in a high-pressure polymerization apparatus at 1,300 bar, in which method N,N-dimethylanilnium tetrakis(pentafluorophenyl)borate and dimethylsilylbis(4,5,6,7-tetrahydroindenyl) zirconium dimethyl are mixed in toluene to prepare a homogeneous catalyst solution, which is used as a catalyst for polymerization of an olefin. In this method, while a solid N,N-dimethylanilnium tetrakis(pentafluorophenyl)borate is used for the preparation of the catalyst, a homogeneous catalyst solution is provided before use for polymerization by mixing it with the metallocene complex in toluene, and then said solution is continuously fed to a polymerization reactor with a high-pressure pump.
Furthermore, Japanese Patent Publication (Kokai) No. Hei 7-157508 discloses a method in which a solution of triisobutyl aluminum in toluene is added to a solution of diphenylmethylene (cyclopentadienyl) (fluorenyl) zirconium dichloride in toluene in a separate vessel before use for polymerization, and further, a solution of N,N-dimethylanilnium tetrakis(pentafluorophenyl)borate in toluene is added to obtain a homogeneous catalyst solution, then said solution is fed to a high-temperature high-pressure polymerization reactor.
Conventionally, as described above, when said boron compound is continuously fed to a reactor, a discontinuous procedure for preparing a homogeneous catalyst solution in a separate vessel, was adopted or a solution having not so high concentration was used.
In Published Specification No. WO94/00459, there is described a method for producing said boron compound and a method for purifying a produced crude boron compound that is colored. According to said method for purification, a method is disclosed in which the produced crude boron compound dissolved in ethers, alcohols, ketones or halogenated aliphatic hydrocarbons as a solvent is precipitated by water or an aliphatic hydrocarbon solvent, but there is no description for particle diameter of the obtained boron compound.
DISCLOSURE OF INVENTION
In view of these circumstances, the problem to be solved by the present invention, in other words, the purpose of the present invention is to provide a method capable of feeding a boron compound useful as a catalyst component for polymerization of an olefin continuously and in large amount to a reactor, and additionally, to provide a boron compound capable of allowing steady feed thereof without using it in the state of a solution and allowing stable operation of a feeding apparatus, when used as a catalyst component for polymerization of olefin or the like, and to provide a method for producing said boron compound.
Namely, the present invention relates to a method for feeding a boron compound, which comprises feeding at least one boron compound selected from (1) to (3) described below in the state suspended or slurried in a solvent continuously to a reactor; a boron compound in the form of fine particles having a maximum particle diameter of 50 &mgr;m or less comprising one or more boron compounds selected from (1) to (3) described below; a catalyst component for olefin polymerization consisting of said boron compound in the form of fine particles; a method for producing a boron compound in the form of fine particles which comprises dissolving one or more boron compounds selected from (1) to (3) described below in an aromatic hydrocarbon solvent and then precipitating in an aliphatic hydrocarbon solvent; and a method for producing boron compound in the form of fine particles, which comprises pulverizing one or more boron compounds selected from (1) to (3) described below so that their maximum particle diameter is 50 &mgr;m or less.
(1) a boron compound represented by the general formula: BQ
1
Q
2
Q
3
,
(2) a boron compound represented by the general formula: G
+
(BQ
1
Q
2
Q
3
Q
4
)
−
, and
(3) a boron compound represented by the general formula: (L-H)
+
(BQ
1
Q
2
Q
3
Q
4
)
−
(in each of the above general formulae, B is a boron atom in the trivalent valence state, Q
1
to Q
4
are a halogen atom, a hydrocarbon group, a halogenated hydrocarbon group, a substituted silyl group, an alkoxy group or a di-substituted amino group, which may be the same or different, respectively. G
+
is an inorganic or organic cation, L is a neutral Lewis base, and (L-H)
+
is a Brønsted acid.)
The present invention is described below in more detail.
The boron compound used in the present invention is at least one boron compound selected from (1) to (3) described below.
(1) a boron compound represented by the general formula: BQ
1
Q
2
Q
3
,
(2) a boron compound represented by the general formula: G
+
(BQ
1
Q
2
Q
3
Q
4
)
−
, and
(3) a boron compound represented by the general formula: (L-H)
+
(BQ
1
Q
2
Q
3
Q
4
)
−
(in each of the above general formulae, B is a boron atom in the trivalent valence state, Q
1
to Q4 are a halogen atom, a hydrocarbon group, a halogenated hydrocarbon group, a substituted silyl group, an alkoxy group or a di-substituted amino group, which may be the same or different, respectively. G
+
is an inorganic or organic cation, L is a neutral Lewis base, and (L-H)
+
is a Brønsted acid.)
In the boron compound (1) represented by the general formula: BQ
1
Q
2
Q
3
, B is a boron atom in the trivalent valence state, Q
1
to Q
3
are a halogen atom, a hydrocarbon group, a halogenated hydrocarbon group, a substituted silyl group, an alkoxy group or a di-substituted amino group, which may be the same or different, respectively. Q
1
to Q
3
are preferably a halogen atom, a hydrocarbon group containing 1-20 carbon atoms, a halogenated hydrocarbon group containing 1 to 20 carbon atoms (for example, a fluorinated aryl group of 6 to 20 carbon atoms containing at least one fluorine atom being preferred), a substituted silyl group containing 1 to 20 carbon atoms, an alkoxy group containing
Katayama Hiroaki
Sato Hideki
Wakamatsu Kazuki
Harlan B.
Sumitomo Chemical Comoany, Limited
Wu David W.
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