JP2007321136A5 - - Google Patents
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- JP2007321136A5 JP2007321136A5 JP2006156536A JP2006156536A JP2007321136A5 JP 2007321136 A5 JP2007321136 A5 JP 2007321136A5 JP 2006156536 A JP2006156536 A JP 2006156536A JP 2006156536 A JP2006156536 A JP 2006156536A JP 2007321136 A5 JP2007321136 A5 JP 2007321136A5
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- Prior art keywords
- solid component
- purified
- range
- moles
- heptane
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- IMNFDUFMRHMDMM-UHFFFAOYSA-N n-heptane Chemical group CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 description 14
- 239000007787 solid Substances 0.000 description 11
- 239000010936 titanium Substances 0.000 description 9
- YXFVVABEGXRONW-UHFFFAOYSA-N toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 9
- 229910052719 titanium Inorganic materials 0.000 description 8
- RTAQQCXQSZGOHL-UHFFFAOYSA-N titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 5
- 239000007795 chemical reaction product Substances 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 4
- 239000002002 slurry Substances 0.000 description 4
- -1 vinylsilane compound Chemical class 0.000 description 3
- 125000003545 alkoxy group Chemical group 0.000 description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 125000000956 methoxy group Chemical group [H]C([H])([H])O* 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Substances N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 2
- 150000003961 organosilicon compounds Chemical class 0.000 description 2
- 238000005070 sampling Methods 0.000 description 2
- DOIRQSBPFJWKBE-UHFFFAOYSA-N Dibutyl phthalate Chemical compound CCCCOC(=O)C1=CC=CC=C1C(=O)OCCCC DOIRQSBPFJWKBE-UHFFFAOYSA-N 0.000 description 1
- 229910003902 SiCl 4 Inorganic materials 0.000 description 1
- QRHCILLLMDEFSD-UHFFFAOYSA-N bis(ethenyl)-dimethylsilane Chemical compound C=C[Si](C)(C)C=C QRHCILLLMDEFSD-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000001771 impaired Effects 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000011949 solid catalyst Substances 0.000 description 1
- 125000003944 tolyl group Chemical group 0.000 description 1
Description
本発明における固体触媒成分（Ａ）を構成する各成分の使用量の量比は、本発明の効果を損なわない範囲で任意のものでありうるが、一般的には、次の範囲内が好ましい。
ビニルシラン化合物（Ａ２）の使用量は、固体成分（Ａ１）を構成するチタン成分に対するモル比（ビニルシラン化合物（Ａ２）のモル数／チタン原子のモル数）で、好ましくは０．００１から１，０００の範囲内であり、特に好ましくは０．０１から１００の範囲内が望ましい。
アルコキシ基を有する有機ケイ素化合物（Ａ３ａ）を用いる場合の使用量は、固体成分（Ａ１）を構成するチタン成分に対するモル比で（アルコキシ基を有する有機ケイ素化合物（Ａ３ａ）のモル数／チタン原子のモル数）で、好ましくは０．０１から１，０００の範囲内であり、特に好ましくは０．１から１００の範囲内が望ましい。
少なくとも二つのエーテル結合を有する化合物（Ａ３ｂ）を用いる場合は、その使用量は、固体成分（Ａ１）を構成するチタン成分に対するモル比（少なくとも二つのエーテル結合を有する化合物（Ａ３ｂ）のモル数／チタン原子のモル数）で、好ましくは０．０１から１，０００の範囲内であり、特に好ましくは０．１から１００の範囲内が望ましい。
任意成分として有機アルミニウム化合物（Ａ４）を用いる場合の使用量は、固体成分（Ａ１）を構成するチタン成分に対するモル比（有機アルミニウム化合物（Ａ４）のモル数／チタン原子のモル数）で、好ましくは０．１から１００の範囲内であり、特に好ましくは１から５０の範囲内が望ましい。
The amount ratio of each component constituting the solid catalyst component (A) in the present invention may be any as long as the effects of the present invention are not impaired, but generally it is preferably within the following range. .
The amount of the vinylsilane compound (A2) used is a molar ratio to the titanium component constituting the solid component (A1) (number of moles of vinylsilane compound (A2) / number of moles of titanium atoms), preferably 0.001 to 1,000. And particularly preferably within the range of 0.01 to 100.
The amount used when the organosilicon compound having an alkoxy group (A3a) is used is the molar ratio to the titanium component constituting the solid component (A1) (number of moles of organosilicon compound having an alkoxy group (A3a) / titanium atom). The number of moles) is preferably in the range of 0.01 to 1,000, and particularly preferably in the range of 0.1 to 100.
When the compound (A3 b ) having at least two ether bonds is used, the amount used is a molar ratio with respect to the titanium component constituting the solid component (A1) (mole of the compound (A3 b ) having at least two ether bonds). Number / number of moles of titanium atoms), preferably in the range of 0.01 to 1,000, particularly preferably in the range of 0.1 to 100.
The amount used when the organoaluminum compound (A4) is used as an optional component is preferably a molar ratio to the titanium component constituting the solid component (A1) (number of moles of organoaluminum compound (A4) / number of moles of titanium atoms). Is in the range of 0.1 to 100, particularly preferably in the range of 1 to 50.
（実施例１）
（１）固体成分の調製
撹拌装置を備えた容量１０Ｌのオートクレーブを充分に窒素で置換し、精製したトルエン２Ｌを導入した。ここに、室温で、Ｍｇ（ＯＥｔ）２を２００ｇ、ＴｉＣｌ４を１Ｌ添加した。温度を９０℃に上げて、フタル酸ジ−ｎ−ブチルを５０ｍｌ導入した。その後、温度を１１０℃に上げて３ｈｒ反応を行った。反応生成物を精製したトルエンで充分に洗浄した。次いで、精製したトルエンを導入して全体の液量を２Ｌに調整した。室温でＴｉＣｌ ４ を１Ｌ添加し、温度を１１０℃に上げて２ｈｒ反応を行った。反応生成物を精製したトルエンで充分に洗浄した。更に、精製したｎ−ヘプタンを用いて、トルエンをｎ−ヘプタンで置換し、固体成分（Ａ１）のスラリーを得た。このスラリーの一部をサンプリングして乾燥した。分析したところ、固体成分（Ａ１）のＴｉ含量は２．７質量％であった。
次に、撹拌装置を備えた容量２０Ｌのオートクレーブを充分に窒素で置換し、上記固体成分（Ａ１）のスラリーを固体成分（Ａ１）として１００ｇ導入した。精製したｎ−ヘプタンを導入して、固体成分（Ａ１）の濃度が２５ｇ／Ｌとなるように調整した。ＳｉＣｌ４５０ｍｌを加え、９０℃で１ｈｒ反応を行った。反応生成物を精製したｎ−ヘプタンで充分に洗浄した。
その後、精製したｎ−ヘプタンを導入して液レベルを４Ｌに調整した。ここに、ジメチルジビニルシランを３０ｍｌ、（ｉ−Ｐｒ）２Ｓｉ（ＯＭｅ）２を３０ｍｌ、Ｅｔ３Ａｌのｎ−ヘプタン希釈液をＥｔ３Ａｌとして８０ｇ添加し、４０℃で２ｈｒ反応を行った。反応生成物を精製したｎ−ヘプタンで充分に洗浄し、得られたスラリーの一部をサンプリングして乾燥した。分析したところ、固体成分にはＴｉが１．２質量％、（ｉ−Ｐｒ）２Ｓｉ（ＯＭｅ）２が８．８質量％含まれていた。
Example 1
(1) Preparation of solid component A 10 L autoclave equipped with a stirrer was sufficiently replaced with nitrogen, and 2 L of purified toluene was introduced. To this, 200 g of Mg (OEt) 2 and 1 L of TiCl 4 were added at room temperature. The temperature was raised to 90 ° C. and 50 ml of di-n-butyl phthalate was introduced. Thereafter, the temperature was raised to 110 ° C. to carry out a reaction for 3 hours. The reaction product was thoroughly washed with purified toluene. Subsequently, the refined toluene was introduce | transduced and the whole liquid quantity was adjusted to 2L. 1 L of TiCl 4 was added at room temperature , the temperature was raised to 110 ° C., and the reaction was performed for 2 hours. The reaction product was thoroughly washed with purified toluene. Further, using purified n-heptane, toluene was replaced with n-heptane to obtain a slurry of the solid component (A1). A portion of this slurry was sampled and dried. As a result of analysis, the Ti content of the solid component (A1) was 2.7% by mass.
Next, a 20 L autoclave equipped with a stirrer was sufficiently substituted with nitrogen, and 100 g of the solid component (A1) slurry was introduced as a solid component (A1). Purified n-heptane was introduced to adjust the concentration of the solid component (A1) to 25 g / L. 50 ml of SiCl 4 was added and a reaction was performed at 90 ° C. for 1 hr. The reaction product was thoroughly washed with purified n-heptane.
Thereafter, purified n-heptane was introduced to adjust the liquid level to 4 L. To this, 30 ml of dimethyldivinylsilane, 30 ml of (i-Pr) 2 Si (OMe) 2 and 80 g of Et 3 Al in an n-heptane diluted solution were added as Et 3 Al, and a reaction was carried out at 40 ° C. for 2 hours. The reaction product was thoroughly washed with purified n-heptane, and a portion of the resulting slurry was sampled and dried. As a result of analysis, the solid component contained 1.2% by mass of Ti and 8.8% by mass of (i-Pr) 2 Si (OMe) 2 .
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2006156536A JP2007321136A (en) | 2006-06-05 | 2006-06-05 | Method for producing polypropylene-based block copolymer |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2006156536A JP2007321136A (en) | 2006-06-05 | 2006-06-05 | Method for producing polypropylene-based block copolymer |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JP2007321136A JP2007321136A (en) | 2007-12-13 |
| JP2007321136A5 true JP2007321136A5 (en) | 2009-05-28 |
Family
ID=38854224
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2006156536A Pending JP2007321136A (en) | 2006-06-05 | 2006-06-05 | Method for producing polypropylene-based block copolymer |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2007321136A (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP5244514B2 (en) * | 2008-09-16 | 2013-07-24 | 日本ポリプロ株式会社 | Process for continuous gas phase production of propylene-based block copolymer |
| WO2011055802A1 (en) | 2009-11-06 | 2011-05-12 | 日本ポリプロ株式会社 | Reactor for propylene polymerization and process for producing propylene polymer |
| JP2012214556A (en) * | 2011-03-31 | 2012-11-08 | Japan Polypropylene Corp | Catalyst for propylene-ethylene block copolymerization and method for producing propylene-ethylene block copolymer |
| JP6107585B2 (en) * | 2013-10-01 | 2017-04-05 | 日本ポリプロ株式会社 | Propylene-based block copolymer production method |
Family Cites Families (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0680101B2 (en) * | 1986-09-09 | 1994-10-12 | 三井東圧化学株式会社 | Process for producing block copolymer of propylene |
| JP3162441B2 (en) * | 1991-10-28 | 2001-04-25 | 三菱化学株式会社 | High rigidity propylene copolymer composition |
| JPH07109313A (en) * | 1993-08-18 | 1995-04-25 | Mitsui Petrochem Ind Ltd | Production of propylene-based block copolymer |
| JPH07247311A (en) * | 1994-03-09 | 1995-09-26 | Asahi Chem Ind Co Ltd | Production of propylene block copolymer |
| JP3355819B2 (en) * | 1994-09-28 | 2002-12-09 | チッソ株式会社 | Method for producing propylene / ethylene block copolymer |
| JP3580001B2 (en) * | 1995-12-21 | 2004-10-20 | チッソ株式会社 | Method for producing propylene-olefin block copolymer |
| JP4098419B2 (en) * | 1998-03-11 | 2008-06-11 | 三菱化学株式会社 | Impact resistant propylene block copolymer |
| JP2001206905A (en) * | 2000-01-27 | 2001-07-31 | Japan Polychem Corp | Method for producing propylenic block copolymer |
| JP4039961B2 (en) * | 2003-02-28 | 2008-01-30 | 三井化学株式会社 | Method for producing polypropylene copolymer |
-
2006
- 2006-06-05 JP JP2006156536A patent/JP2007321136A/en active Pending
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