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- JP2006002146A5 JP2006002146A5 JP2005144271A JP2005144271A JP2006002146A5 JP 2006002146 A5 JP2006002146 A5 JP 2006002146A5 JP 2005144271 A JP2005144271 A JP 2005144271A JP 2005144271 A JP2005144271 A JP 2005144271A JP 2006002146 A5 JP2006002146 A5 JP 2006002146A5
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- 125000004432 carbon atoms Chemical group C* 0.000 claims description 15
- 150000003609 titanium compounds Chemical class 0.000 claims description 14
- 150000002430 hydrocarbons Chemical class 0.000 claims description 13
- 150000002902 organometallic compounds Chemical class 0.000 claims description 12
- 239000011777 magnesium Substances 0.000 claims description 10
- 150000001336 alkenes Chemical class 0.000 claims description 9
- 125000004429 atoms Chemical group 0.000 claims description 9
- 239000000843 powder Substances 0.000 claims description 8
- FYYHWMGAXLPEAU-UHFFFAOYSA-N magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 7
- 229910052749 magnesium Inorganic materials 0.000 claims description 7
- 239000002685 polymerization catalyst Substances 0.000 claims description 7
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 229910052751 metal Inorganic materials 0.000 claims description 6
- 239000002184 metal Substances 0.000 claims description 6
- 229920000098 polyolefin Polymers 0.000 claims description 6
- 230000000737 periodic Effects 0.000 claims description 5
- 239000005977 Ethylene Substances 0.000 claims description 4
- 125000003545 alkoxy group Chemical group 0.000 claims description 4
- 125000005336 allyloxy group Chemical group 0.000 claims description 4
- 150000004718 beta keto acids Chemical group 0.000 claims description 4
- 239000000969 carrier Substances 0.000 claims description 4
- 239000012320 chlorinating reagent Substances 0.000 claims description 4
- VGGSQFUCUMXWEO-UHFFFAOYSA-N ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 claims description 4
- XPXMKIXDFWLRAA-UHFFFAOYSA-N hydrazinide Chemical group [NH-]N XPXMKIXDFWLRAA-UHFFFAOYSA-N 0.000 claims description 4
- 125000004469 siloxy group Chemical group [SiH3]O* 0.000 claims description 4
- 239000011949 solid catalyst Substances 0.000 claims description 4
- RTAQQCXQSZGOHL-UHFFFAOYSA-N titanium Chemical group [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 4
- 229910052719 titanium Inorganic materials 0.000 claims description 4
- 239000004215 Carbon black (E152) Substances 0.000 claims description 3
- 239000003054 catalyst Substances 0.000 claims description 3
- 239000002904 solvent Substances 0.000 claims description 3
- 238000007334 copolymerization reaction Methods 0.000 claims description 2
- 229910052736 halogen Inorganic materials 0.000 claims description 2
- 125000005843 halogen group Chemical group 0.000 claims description 2
- 150000002681 magnesium compounds Chemical class 0.000 claims description 2
- 150000002901 organomagnesium compounds Chemical class 0.000 claims description 2
- 238000006116 polymerization reaction Methods 0.000 claims description 2
- 239000010936 titanium Substances 0.000 claims description 2
- 239000004711 α-olefin Substances 0.000 claims description 2
- -1 2-ethylpentyl Chemical group 0.000 description 7
- 150000001875 compounds Chemical class 0.000 description 3
- 125000002877 alkyl aryl group Chemical group 0.000 description 2
- 125000000217 alkyl group Chemical group 0.000 description 2
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 2
- 125000002914 sec-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 2
- 125000006176 2-ethylbutyl group Chemical group [H]C([H])([H])C([H])([H])C([H])(C([H])([H])*)C([H])([H])C([H])([H])[H] 0.000 description 1
- 125000005916 2-methylpentyl group Chemical group 0.000 description 1
- 125000002704 decyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
- 125000004051 hexyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 1
- 150000002736 metal compounds Chemical class 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 125000001624 naphthyl group Chemical group 0.000 description 1
- 125000001400 nonyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 125000002347 octyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 125000002734 organomagnesium group Chemical group 0.000 description 1
- 125000001147 pentyl group Chemical group C(CCCC)* 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 125000001424 substituent group Chemical group 0.000 description 1
- 125000000999 tert-butyl group Chemical group [H]C([H])([H])C(*)(C([H])([H])[H])C([H])([H])[H] 0.000 description 1
Description
すなわち、本発明は、
[1] 固体触媒成分[A]および有機金属化合物成分[B]からなるオレフィン重合用触媒であり、
固体触媒成分[A]が、
一般式1で表される不活性炭化水素溶媒に可溶である有機マグネシウム化合物と、一般式2で表される塩素化剤との反応により調製された担体(A−1)に、
チタン化合物(A−2)を担持させることにより調製され、
該有機マグネシウム化合物と該塩素化剤との反応が60℃以上150℃以下で行われることを特徴とする、オレフィン重合用触媒。
(M1)α(Mg)β(R1)a(R2)b(OR3)c ・・・式1
(式中、M1は周期律表第1族、第2族、第13族および第14族からなる群に属するマグネシウム以外の金属原子であり、R1、R2およびR3は炭素数2以上20以下の炭化水素基であり、α、β、a、bおよびcは次の関係を満たす実数である。0≦α、0<β、0≦a、0≦b、0≦c、0<a+b、0≦c/(α+β)≦2、kα+2β=a+b+c(ただし、kはM1の原子価))
HdSiCleR4 (4−(d+e)) ・・・式2
(式中、R4は炭素数1以上12以下の炭化水素基であり、dとeは次の関係を満たす実数である。0<d、0<e、0<d+e≦4)
[2] 担体(A−1)に対するチタン化合物(A−2)の担持が、チタン化合物(A−2)と有機金属化合物(A−3)との反応により行われ、チタン化合物(A−2)が一般式3で表され、有機金属化合物(A−3)が一般式4により表されることを特徴とする、[1]に記載のオレフィン重合用触媒、
Ti(OR5)fX(4−f) ・・・式3
(式中、fは0以上4以下の実数であり、R5は炭化水素基、Xはハロゲンである。)
(M2)γ(Mg)ε(R6)h(R7)iYj ・・・式4
(式中、M2は周期律表第1族、第2族、第13族および第14族からなる群に属するマグネシウム以外の金属原子であり、R6およびR7は炭素数2以上20以下の炭化水素基であり、Yはアルコキシ、シロキシ、アリロキシ、アミノ、アミド、−N=C(R 8 )R 9 、−SR10(ただし、R8、R9およびR10は炭素数2以上20以下の炭化水素基を表す。jが2の場合には、Yはそれぞれ異なっていてもよい。)、β−ケト酸残基のいずれかであり、γ、ε、h、iおよびjは次の関係を満たす実数である。0≦γ、0<ε、0≦h、0≦i、0<h+i、0≦j/(γ+ε)≦2、nγ+2ε=h+i+j(ただし、nはM2の原子価))
[3] [1]または[2]のいずれかに記載のオレフィン重合用触媒を用いたエチレンの単独重合あるいはエチレンと炭素数が3以上のα−オレフィンとの共重合によって得られたポリオレフィンパウダーであって、該パウダーに含まれるチタン原子が5重量ppm以下であり、マグネシウム原子に対するチタン原子のモル比が0.5以下であり、なおかつ該ポリオレフィンパウダーの嵩密度が0.43g/ml以上であることを特徴とするポリオレフィンパウダー、
である。
That is, the present invention
[1] An olefin polymerization catalyst comprising a solid catalyst component [A] and an organometallic compound component [B],
The solid catalyst component [A] is,
An organic magnesium compound in inert hydrocarbon solvent represented by the formula 1 is soluble, on a carrier prepared by reaction of a chlorinating agent and represented by the general formula 2 (A-1),
Is prepared by causing a titanium compound (A-2) bearing,
A catalyst for olefin polymerization, wherein the reaction between the organomagnesium compound and the chlorinating agent is performed at 60 ° C or higher and 150 ° C or lower.
(M 1 ) α (Mg) β (R 1 ) a (R 2 ) b (OR 3 ) c Formula 1
(In the formula, M 1 is a metal atom other than magnesium belonging to the group consisting of Group 1, Group 2, Group 13 and Group 14 of the Periodic Table, and R 1 , R 2 and R 3 have 2 carbon atoms. The hydrocarbon group is 20 or less and α, β, a, b, and c are real numbers that satisfy the following relationship: 0 ≦ α, 0 <β, 0 ≦ a, 0 ≦ b, 0 ≦ c, 0 <A + b, 0 ≦ c / (α + β) ≦ 2, kα + 2β = a + b + c (where k is the valence of M 1 ))
H d SiCl e R 4 (4- (d + e)) Formula 2
(Wherein R 4 is a hydrocarbon group having 1 to 12 carbon atoms, and d and e are real numbers satisfying the following relationship: 0 <d, 0 <e, 0 <d + e ≦ 4)
[2] The titanium compound (A-2) is supported on the carrier (A-1) by a reaction between the titanium compound (A-2) and the organometallic compound (A-3). ) Is represented by the general formula 3, and the organometallic compound (A-3) is represented by the general formula 4, the olefin polymerization catalyst according to [1],
Ti (OR 5 ) f X (4-f) Formula 3
(In the formula, f is a real number of 0 or more and 4 or less, R 5 is a hydrocarbon group, and X is a halogen.)
(M 2 ) γ (Mg) ε (R 6 ) h (R 7 ) i Y j Expression 4
(In the formula, M 2 is a metal atom other than magnesium belonging to the group consisting of Group 1, Group 2, Group 13 and Group 14 of the Periodic Table, and R 6 and R 7 have 2 to 20 carbon atoms. Y is alkoxy, siloxy, allyloxy, amino, amide, —N═C (R 8 ) R 9 , —SR 10 (where R 8 , R 9, and R 10 have 2 to 20 carbon atoms) The following hydrocarbon groups are represented: when j is 2, Y may be different from each other), β-keto acid residues, and γ, ε, h, i and j are 0 ≦ γ, 0 <ε, 0 ≦ h, 0 ≦ i, 0 <h + i, 0 ≦ j / (γ + ε) ≦ 2, nγ + 2ε = h + i + j (where n is an atom of M 2 Price))
[3] A polyolefin powder obtained by homopolymerization of ethylene or copolymerization of ethylene and an α-olefin having 3 or more carbon atoms using the olefin polymerization catalyst according to any one of [1] and [2] The titanium atom contained in the powder is 5 ppm by weight or less, the molar ratio of titanium atom to magnesium atom is 0.5 or less, and the bulk density of the polyolefin powder is 0.43 g / ml or more. Polyolefin powder, characterized by
It is.
次に、有機金属化合物(A−3)について説明する。
(A−3)としては下記一般式4で表されるものが好ましい。
(M2)γ(Mg)ε(R6)h(R7)iYj ・・・式4
(式中、M2は周期律表第1族、第2族、第13族および第14族からなる群に属するマグネシウム以外の金属原子であり、R6およびR7は炭素数2以上20以下の炭化水素基であり、Yはアルコキシ、シロキシ、アリロキシ、アミノ、アミド、−N=C(R 8 )R 9 、−SR10(ただし、R8、R9およびR10は炭素数2以上20以下の炭化水素基を表す。jが2の場合には、Yはそれぞれ異なっていてもよい。)、β−ケト酸残基のいずれかであり、γ、ε、h、iおよびjは次の関係を満たす実数である。0≦γ、0<ε、0≦h、0≦i、0<h+i、0≦j/(γ+ε)≦2、nγ+2ε=h+i+j(ただし、nはM2の原子価))
この化合物は、不活性炭化水素溶媒に可溶な有機マグネシウムの錯化合物の形として示されているが、ジヒドロカルビルマグネシウム化合物およびこの化合物と他の金属化合物との錯体のすべてを包含するものである。記号γ、ε、h、i、jの関係式nγ+2ε=h+i+jは金属原子の原子価と置換基との化学量論性を示している。
Next, the organometallic compound (A-3) will be described.
(A-3) is preferably represented by the following general formula 4.
(M 2 ) γ (Mg) ε (R 6 ) h (R 7 ) i Y j Expression 4
(In the formula, M 2 is a metal atom other than magnesium belonging to the group consisting of Group 1, Group 2, Group 13 and Group 14 of the Periodic Table, and R 6 and R 7 have 2 to 20 carbon atoms. Y is alkoxy, siloxy, allyloxy, amino, amide, —N═C (R 8 ) R 9 , —SR 10 (where R 8 , R 9, and R 10 have 2 to 20 carbon atoms) The following hydrocarbon groups are represented: when j is 2, Y may be different from each other), β-keto acid residues, and γ, ε, h, i and j are 0 ≦ γ, 0 <ε, 0 ≦ h, 0 ≦ i, 0 <h + i, 0 ≦ j / (γ + ε) ≦ 2, nγ + 2ε = h + i + j (where n is an atom of M 2 Price))
This compound is shown as a complex form of organomagnesium soluble in an inert hydrocarbon solvent, but encompasses all dihydrocarbylmagnesium compounds and complexes of this compound with other metal compounds. . The relational expression nγ + 2ε = h + i + j of the symbols γ, ε, h, i, j indicates the stoichiometry between the valence of the metal atom and the substituent.
次にYについて説明する。
Yはアルコキシ、シロキシ、アリロキシ、アミノ、アミド、−N=C(R 8 )R 9 、−SR10(ただし、R8、R9およびR10は炭素数2以上20以下の炭化水素基を表す)、βケト酸残基のいずれかである。
上記のR8、R9およびR10としては炭素原子数が1以上12以下のアルキル基またはアリール基が好ましく、炭素原子数が3以上10以下のアルキル基またはアリール基がさらに好ましい。具体的には、たとえば、メチル、エチル、プロピル、1−メチルエチル、ブチル、1−メチルプロピル、1,1−ジメチルエチル、ペンチル、ヘキシル、2−メチルペンチル、2−エチルブチル、2−エチルペンチル、2−エチルヘキシル、2−エチル−4−メチルペンチル、2−プロピルヘプチル、2−エチル−5−メチルオクチル、オクチル、ノニル、デシル、フェニル、ナフチル基等が好ましく、ブチル、1−メチルプロピル、2−メチルペンチルおよび2−エチルヘキシル基がさらに好ましい。
Next, Y will be described.
Y is alkoxy, siloxy, allyloxy, amino, amide, —N═C (R 8 ) R 9 , —SR 10 (where R 8 , R 9 and R 10 represent a hydrocarbon group having 2 to 20 carbon atoms) ), Β-keto acid residues.
R 8 , R 9 and R 10 are preferably an alkyl group or aryl group having 1 to 12 carbon atoms, and more preferably an alkyl group or aryl group having 3 to 10 carbon atoms. Specifically, for example, methyl, ethyl, propyl, 1-methylethyl, butyl, 1-methylpropyl, 1,1-dimethylethyl, pentyl, hexyl, 2-methylpentyl, 2-ethylbutyl, 2-ethylpentyl, 2-ethylhexyl, 2-ethyl-4-methylpentyl, 2-propylheptyl, 2-ethyl-5-methyloctyl, octyl, nonyl, decyl, phenyl, naphthyl group and the like are preferable, butyl, 1-methylpropyl, 2- More preferred are methylpentyl and 2-ethylhexyl groups.
Claims (3)
固体触媒成分[A]が、
一般式1で表される不活性炭化水素溶媒に可溶である有機マグネシウム化合物と、一般式2で表される塩素化剤との反応により調製された担体(A−1)に、
チタン化合物(A−2)を担持させることにより調製され、
該有機マグネシウム化合物と該塩素化剤との反応が60℃以上150℃以下で行われることを特徴とする、オレフィン重合用触媒。
(M1)α(Mg)β(R1)a(R2)b(OR3)c ・・・式1
(式中、M1は周期律表第1族、第2族、第13族および第14族からなる群に属するマグネシウム以外の金属原子であり、R1、R2およびR3は炭素数2以上20以下の炭化水素基であり、α、β、a、bおよびcは次の関係を満たす実数である。0≦α、0<β、0≦a、0≦b、0≦c、0<a+b、0≦c/(α+β)≦2、kα+2β=a+b+c(ただし、kはM1の原子価))
HdSiCleR4 (4−(d+e)) ・・・式2
(式中、R4は炭素数1以上12以下の炭化水素基であり、dとeは次の関係を満たす実数である。0<d、0<e、0<d+e≦4) An olefin polymerization catalyst comprising a solid catalyst component [A] and an organometallic compound component [B],
The solid catalyst component [A] is,
An organic magnesium compound in inert hydrocarbon solvent represented by the formula 1 is soluble, on a carrier prepared by reaction of a chlorinating agent and represented by the general formula 2 (A-1),
Is prepared by causing a titanium compound (A-2) bearing,
A catalyst for olefin polymerization, wherein the reaction between the organomagnesium compound and the chlorinating agent is performed at 60 ° C or higher and 150 ° C or lower.
(M 1 ) α (Mg) β (R 1 ) a (R 2 ) b (OR 3 ) c Formula 1
(In the formula, M 1 is a metal atom other than magnesium belonging to the group consisting of Group 1, Group 2, Group 13 and Group 14 of the Periodic Table, and R 1 , R 2 and R 3 have 2 carbon atoms. The hydrocarbon group is 20 or less and α, β, a, b, and c are real numbers that satisfy the following relationship: 0 ≦ α, 0 <β, 0 ≦ a, 0 ≦ b, 0 ≦ c, 0 <A + b, 0 ≦ c / (α + β) ≦ 2, kα + 2β = a + b + c (where k is the valence of M 1 ))
H d SiCl e R 4 (4- (d + e)) Formula 2
(Wherein R 4 is a hydrocarbon group having 1 to 12 carbon atoms, and d and e are real numbers satisfying the following relationship: 0 <d, 0 <e, 0 <d + e ≦ 4)
Ti(OR5)fX(4−f) ・・・式3
(式中、fは0以上4以下の実数であり、R5は炭化水素基、Xはハロゲンである。)
(M2)γ(Mg)ε(R6)h(R7)iYj ・・・式4
(式中、M2は周期律表第1族、第2族、第13族および第14族からなる群に属するマグネシウム以外の金属原子であり、R6およびR7は炭素数2以上20以下の炭化水素基であり、Yはアルコキシ、シロキシ、アリロキシ、アミノ、アミド、−N=C(R 8 )R 9 、−SR10(ただし、R8、R9およびR10は炭素数2以上20以下の炭化水素基を表す。jが2の場合には、Yはそれぞれ異なっていてもよい。)、β−ケト酸残基のいずれかであり、γ、ε、h、iおよびjは次の関係を満たす実数である。0≦γ、0<ε、0≦h、0≦i、0<h+i、0≦j/(γ+ε)≦2、nγ+2ε=h+i+j(ただし、nはM2の原子価)) The titanium compound (A-2) is supported on the carrier (A-1) by a reaction between the titanium compound (A-2) and the organometallic compound (A-3), and the titanium compound (A-2) is generally used. 2. The olefin polymerization catalyst according to claim 1, wherein the olefin polymerization catalyst is represented by Formula 3 and the organometallic compound (A-3) is represented by General Formula 4. 3.
Ti (OR 5 ) f X (4-f) Formula 3
(In the formula, f is a real number of 0 or more and 4 or less, R 5 is a hydrocarbon group, and X is a halogen.)
(M 2 ) γ (Mg) ε (R 6 ) h (R 7 ) i Y j Expression 4
(In the formula, M 2 is a metal atom other than magnesium belonging to the group consisting of Group 1, Group 2, Group 13 and Group 14 of the Periodic Table, and R 6 and R 7 have 2 to 20 carbon atoms. Y is alkoxy, siloxy, allyloxy, amino, amide, —N═C (R 8 ) R 9 , —SR 10 (where R 8 , R 9, and R 10 have 2 to 20 carbon atoms) The following hydrocarbon groups are represented: when j is 2, Y may be different from each other), β-keto acid residues, and γ, ε, h, i and j are 0 ≦ γ, 0 <ε, 0 ≦ h, 0 ≦ i, 0 <h + i, 0 ≦ j / (γ + ε) ≦ 2, nγ + 2ε = h + i + j (where n is an atom of M 2 Price))
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JP5829257B2 (en) * | 2012-12-11 | 2015-12-09 | 旭化成ケミカルズ株式会社 | Polyethylene powder, molded body, and separator for lithium ion secondary battery |
JP5829258B2 (en) * | 2012-12-11 | 2015-12-09 | 旭化成ケミカルズ株式会社 | Ethylene polymer powder, molded product, and separator for lithium ion secondary battery |
JP5774084B2 (en) * | 2013-12-20 | 2015-09-02 | 旭化成ケミカルズ株式会社 | Polyethylene powder |
CN108752607B (en) * | 2014-01-29 | 2021-04-20 | 旭化成株式会社 | High molecular weight polyethylene powder, microporous film and high-strength fiber |
JP5829295B2 (en) * | 2014-03-06 | 2015-12-09 | 旭化成ケミカルズ株式会社 | Ethylene polymer powder, method for producing the same, and molded product |
KR101707306B1 (en) * | 2014-04-18 | 2017-02-15 | 아사히 가세이 케미칼즈 가부시키가이샤 | Polyethylene powder for fiber, fiber and molded article |
JP5782558B1 (en) | 2014-11-14 | 2015-09-24 | 旭化成ケミカルズ株式会社 | Polyethylene powder |
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JPS5340696A (en) * | 1976-09-28 | 1978-04-13 | Asahi Chem Ind Co Ltd | Olefin polymerization catalyst |
JPS5958013A (en) * | 1982-09-29 | 1984-04-03 | Asahi Chem Ind Co Ltd | Polymerization of olefin |
EP0099774B2 (en) * | 1982-06-24 | 1995-03-22 | BP Chimie Société Anonyme | Process for the polymerization and copolymerization of alpha-olefins in a fluidized bed |
JPH04216804A (en) * | 1990-12-18 | 1992-08-06 | Asahi Chem Ind Co Ltd | Polymerization of alpha-olefin |
JPH10204116A (en) * | 1997-01-17 | 1998-08-04 | Asahi Chem Ind Co Ltd | Olefin polymerization catalyst and production of polyolefin |
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