CN102015586A - 用于乙烯低聚的方法及为此使用的反应器系统 - Google Patents
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- 238000000034 method Methods 0.000 title claims abstract description 18
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 title claims abstract description 17
- 239000005977 Ethylene Substances 0.000 title claims abstract description 12
- 238000002156 mixing Methods 0.000 claims abstract description 29
- 239000000203 mixture Substances 0.000 claims abstract description 23
- 239000003054 catalyst Substances 0.000 claims abstract description 22
- 239000002904 solvent Substances 0.000 claims abstract description 7
- 230000002779 inactivation Effects 0.000 claims description 9
- 238000006384 oligomerization reaction Methods 0.000 claims description 9
- 239000004711 α-olefin Substances 0.000 claims description 8
- 238000005520 cutting process Methods 0.000 claims description 6
- 238000000605 extraction Methods 0.000 claims description 5
- 125000000217 alkyl group Chemical group 0.000 claims description 4
- 239000003513 alkali Substances 0.000 claims description 3
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- 230000008569 process Effects 0.000 claims description 3
- 238000011144 upstream manufacturing Methods 0.000 claims description 3
- 229910007926 ZrCl Inorganic materials 0.000 claims description 2
- 229910052782 aluminium Inorganic materials 0.000 claims description 2
- -1 aluminum compound Chemical class 0.000 claims description 2
- 229910052799 carbon Inorganic materials 0.000 claims description 2
- 125000004432 carbon atom Chemical group C* 0.000 claims description 2
- 230000009849 deactivation Effects 0.000 claims description 2
- 238000006386 neutralization reaction Methods 0.000 claims description 2
- 150000007524 organic acids Chemical class 0.000 claims description 2
- 150000002899 organoaluminium compounds Chemical class 0.000 claims description 2
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 claims description 2
- 125000002769 thiazolinyl group Chemical group 0.000 claims description 2
- 238000007599 discharging Methods 0.000 abstract 1
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- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/18—Stationary reactors having moving elements inside
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C11/00—Aliphatic unsaturated hydrocarbons
- C07C11/02—Alkenes
- C07C11/04—Ethylene
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- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C2/00—Preparation of hydrocarbons from hydrocarbons containing a smaller number of carbon atoms
- C07C2/02—Preparation of hydrocarbons from hydrocarbons containing a smaller number of carbon atoms by addition between unsaturated hydrocarbons
- C07C2/04—Preparation of hydrocarbons from hydrocarbons containing a smaller number of carbon atoms by addition between unsaturated hydrocarbons by oligomerisation of well-defined unsaturated hydrocarbons without ring formation
- C07C2/06—Preparation of hydrocarbons from hydrocarbons containing a smaller number of carbon atoms by addition between unsaturated hydrocarbons by oligomerisation of well-defined unsaturated hydrocarbons without ring formation of alkenes, i.e. acyclic hydrocarbons having only one carbon-to-carbon double bond
- C07C2/08—Catalytic processes
- C07C2/14—Catalytic processes with inorganic acids; with salts or anhydrides of acids
- C07C2/20—Acids of halogen; Salts thereof ; Complexes thereof with organic compounds
- C07C2/22—Metal halides; Complexes thereof with organic compounds
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- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C2521/00—Catalysts comprising the elements, oxides or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium or hafnium
- C07C2521/06—Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C2531/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- C07C2531/02—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides
- C07C2531/12—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides containing organo-metallic compounds or metal hydrides
- C07C2531/14—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides containing organo-metallic compounds or metal hydrides of aluminium or boron
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Abstract
本发明涉及一种用于乙烯低聚的方法,包括以下步骤:(i)将乙烯在一种溶剂和一种催化剂组合物的存在下于一种反应器中低聚;(ii)从所述反应器中排出一种含有催化剂组合物的出口物流;(iii)将所述催化剂组合物用一种极性相失活并萃取,其中所述出口物流与所述极性相在一种动态混合设备中混合,所述动态混合设备具有包括同心工具环的转子和定子元件;并涉及一种为此使用的反应器系统。
Description
本发明涉及一种用于乙烯低聚的方法和一种为此使用的反应器系统。
通过乙烯低聚制备直链α-烯烃的低聚方法是广为所知的。这些方法通常在这样一种反应器系统中进行,其中将引入的乙烯在溶剂的存在下通过适宜的催化剂组合物转化为直链α-烯烃。在反应器中进行低聚后,气体和液体出口物流被进一步地加工。来自反应器的液体出口物流通常含有直链α-烯烃、溶剂和仍有活性的催化剂组合物。各方法中的一个基本特征为催化剂组合物中组分的失活以及从有机相中萃取。通常,失活和萃取是通过将液体反应器出口物料与一种极性相(例如一种苛性碱水溶液)混合而实现。这方面,需要使有机相与所述极性相快速而有效地混合。另外,还必须保证混合器中形成极小的液滴且出口物流和极性相的停留时间最小(直至达到有效混合),以产生足够的相转移表面。如果失活不能被足够快速地实现,则将产生不希望有的副反应。这导致产物纯度的降低,并且不希望有的副产品还可在分离部分形成腐蚀性组分。
在现有技术中,静态混合器、喷嘴或搅拌釜混合器已用于混合有机出口相和极性相。然而,迄今,这些混合设备已不足以满足所有上述需求,其可被进一步地改进。
因此,本发明的一个目的是提供一种能克服现有技术缺点的乙烯低聚方法。特别是提供这样一种方法,其中在低聚后,催化剂组合物可被容易而快速地失活并从低聚反应器的有机出口物流中萃取出来。
此外,本发明的一个目的是提供一种用于所述低聚的反应器系统。
本发明的第一个目的是通过一种用于乙烯低聚的方法实现,所述方法包括以下步骤:
(i)将乙烯在一种溶剂和一种催化剂组合物的存在下于一种反应器中低聚;
(ii)从所述反应器中排出一种含有催化剂组合物的出口物流;
(iii)将所述催化剂组合物用一种极性相失活并萃取,其中所述出口物流与所述极性相在一种动态混合设备中混合,所述动态混合设备具有转子和定子元件,所述元件包括同心工具环。
优选地,所述混合设备包括经径向开槽和/或钻孔的元件,其中相邻工具环之间的环形剪切间隙为0.1至5mm。
优选地,所述极性相为一种苛性碱水溶液。
更优选地,所述动态混合器的转速为2.5至40m/s。
在一个实施方案中,所述催化剂组合物包括一种有机酸的锆盐和至少一种有机铝化合物。
此外,优选地,所述锆盐具有式ZrCl4-mXm,其中X=OCOR或OSO3R′,R和R′独立地为烷基、烯基或苯基,并且其中0<m<4。
此外,优选提出的是,至少一种铝化合物具有通式R1 nAl3-n或Al2Y3R1 3,其中R1代表具有1至20个碳原子的烷基,Y代表Cl、Br或I,n为在1<n<2范围内的任意数值。
根据本发明,还提供一种用于乙烯低聚的反应器系统,包括一种具有将乙烯、α-烯烃、溶剂和催化剂组合物供给至反应器中和从反应器中排出的入口和出口的反应器,所述反应器与一种动态混合设备连接,在所述动态混合设备中,一种含有催化剂组合物的出口物流与一种用于将催化剂失活并萃取的极性相进行混合,所述动态混合设备具有转子和定子元件,所述元件包括经径向开槽和/或钻孔的同心工具环,其中环形剪切间隙为0.1至5mm。
优选地,所述动态混合设备包括用于处理高分子量直链α-烯烃的切割设备,所述切割设备位于定子和转子元件的上游,或整合至所述动态混合设备的一个入口区域中或一个单独的套管(separate casing)中。
出乎意料地,已发现上文公开的特定动态混合设备的使用获得了一种乙烯低聚方法,其中可以快速而有效地混合含有催化剂组合物的液体反应器出口物流和一种用于失活和萃取的极性相。此外,还能形成极小的液滴并达到直至已实现有效混合的最小停留时间。此外,使用所述动态混合设备的失活足够快速,从而可避免不希望有的副反应。因此,不会降低产品纯度,并可避免分离部分中腐蚀性组分的形成。
通过按需改制混合设备的几何结构,可调整液滴尺寸以满足所需快速而有效的失活和萃取。另一方面,还可避免稳定乳液的形成,从而使得此后仍可在倾析器中通过重力分离作用实现有机相与极性相的分离。
具体而言,所述动态混合设备的性能可通过混合器几何结构的改制来优化,所述几何机构例如转子和定子元件之间的间隙和距离以及所应用的转速。
还已发现,其中混合将通过湍流实现的混合器类型不适用于本发明目的,而需要高剪切力来实现所需的高效混合作业。只有使用上文公开的动态混合器才能获得令人满意的结果。如此可实现高剪切力和低停留时间。
所获得的液滴尺寸为10μm左右,并具有狭窄的尺寸分布。
在另一个实施方案中,所述混合设备可包括用于处理高分子量直链α-烯烃的切割设备,所述切割设备位于混合元件的上游,或整合至所述动态混合设备的一个入口区域中或一个单独的套管中。这有助于避免反应器系统的沉积和堵塞。
此外,还可显著避免所述动态混合设备中的死区域,这同样也作为本发明的方法和反应器系统的优点。
以上说明书或权利要求中所公开的特征既可以单独的形式又可以其任意结合的形式作为用于实现各种形式的本发明的素材。
Claims (8)
1.乙烯低聚的方法,包括以下步骤:
(i)将乙烯在一种溶剂和一种催化剂组合物的存在下于一种反应器中低聚;
(ii)从所述反应器中排出一种含有催化剂组合物的出口物流;
(iii)将所述催化剂组合物用一种极性相失活并萃取,其中所述出口物流与所述极性相在一种动态混合设备中混合,所述动态混合设备具有转子和定子元件,所述元件包括经径向开槽和/或钻孔的同心工具环,其中环形剪切间隙为0.1至5mm。
2.权利要求1的方法,其中所述极性相为一种苛性碱水溶液。
3.权利要求1或2的方法,其中所述动态混合设备的转速为2.5至40m/s。
4.前述权利要求中任一项的方法,其中所述催化剂组合物包括一种有机酸的锆盐和至少一种有机铝化合物。
5.权利要求4的方法,其中所述锆盐具有式ZrCl4-mXm,其中X=OCOR或OSO3R′,R和R′独立地为烷基、烯基或苯基,并且其中0<m<4。
6.权利要求4或5的方法,其中所述至少一种铝化合物具有通式R1 nAl3-n或Al2Y3R1 3,其中R1代表具有1至20个碳原子的烷基,Y代表Cl、Br或I,n为在1<n<2范围内的任意数值。
7.用于乙烯低聚的反应器系统,包括一种具有将乙烯、α-烯烃、溶剂和催化剂组合物供给至反应器中和从反应器中排出的入口和出口的反应器,所述反应器与一种动态混合设备连接,在所述动态混合设备中,一种含有催化剂组合物的出口物流与一种用于将催化剂失活并萃取的极性相进行混合,所述动态混合设备具有转子和定子元件,所述元件包括经径向开槽和/或钻孔的同心工具环,其中环形剪切间隙为0.1至5mm。
8.权利要求7的反应器系统,其中所述动态混合设备包括用于处理高分子量直链α-烯烃的切割设备,所述切割设备位于定子和转子元件的上游,或整合至所述动态混合设备的一个入口区域中或一个单独的套管中。
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EP07025109A EP2080745B1 (en) | 2007-12-27 | 2007-12-27 | Method for oligomerisation of ethylene and reactor system therefore |
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US9963648B2 (en) * | 2013-06-28 | 2018-05-08 | Dow Global Technologies Llc | Process for the preparation of branched polyolefins for lubricant applications |
US10513473B2 (en) | 2015-09-18 | 2019-12-24 | Chevron Phillips Chemical Company Lp | Ethylene oligomerization/trimerization/tetramerization reactor |
US10519077B2 (en) | 2015-09-18 | 2019-12-31 | Chevron Phillips Chemical Company Lp | Ethylene oligomerization/trimerization/tetramerization reactor |
EP3441136B1 (de) * | 2017-08-08 | 2020-12-23 | Tuma Pumpensysteme GmbH | Zerkleinerungs- und mischvorrichtung, sowie anlage und verfahren zur katalytischen drucklosen verölung |
US11667590B2 (en) | 2021-05-26 | 2023-06-06 | Chevron Phillips Chemical Company, Lp | Ethylene oligomerization processes |
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JP4766634B2 (ja) * | 2001-04-09 | 2011-09-07 | 栄司 西本 | 汚染液体処理装置 |
DE60210794T2 (de) * | 2001-10-17 | 2007-05-10 | E.I. Dupont De Nemours And Co., Wilmington | Rotor-stator apparat und verfahren zur bildung von partikeln |
WO2003082933A1 (fr) * | 2002-04-01 | 2003-10-09 | Daicel Chemical Industries, Ltd. | Procede de production de composes a poids moleculaire eleve pour resine photosensible |
JP2007153825A (ja) * | 2005-12-07 | 2007-06-21 | Sumitomo Chemical Co Ltd | α−オレフィンの製造方法 |
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2007
- 2007-12-27 DE DE602007008127T patent/DE602007008127D1/de active Active
- 2007-12-27 EP EP07025109A patent/EP2080745B1/en not_active Expired - Fee Related
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2008
- 2008-12-18 WO PCT/EP2008/010802 patent/WO2009083163A1/en active Application Filing
- 2008-12-18 US US12/735,267 patent/US20110054233A1/en not_active Abandoned
- 2008-12-18 CN CN201510455690.4A patent/CN105130739A/zh active Pending
- 2008-12-18 JP JP2010540052A patent/JP5800348B2/ja not_active Expired - Fee Related
- 2008-12-18 MY MYPI2010002691A patent/MY147766A/en unknown
- 2008-12-18 CN CN2008801224727A patent/CN102015586A/zh active Pending
- 2008-12-18 RU RU2010131191/04A patent/RU2458031C2/ru not_active IP Right Cessation
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2010
- 2010-06-10 ZA ZA2010/04157A patent/ZA201004157B/en unknown
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Also Published As
Publication number | Publication date |
---|---|
DE602007008127D1 (de) | 2010-09-09 |
EP2080745A1 (en) | 2009-07-22 |
RU2010131191A (ru) | 2012-02-10 |
CN105130739A (zh) | 2015-12-09 |
JP5800348B2 (ja) | 2015-10-28 |
EP2080745B1 (en) | 2010-07-28 |
MY147766A (en) | 2013-01-31 |
JP2011507917A (ja) | 2011-03-10 |
RU2458031C2 (ru) | 2012-08-10 |
ZA201004157B (en) | 2011-08-31 |
WO2009083163A1 (en) | 2009-07-09 |
US20110054233A1 (en) | 2011-03-03 |
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