CN1107828A - 线性烯烃的制备方法 - Google Patents
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Abstract
通过乙烯低聚制备线性α-烯烃的方法。低聚在
一种有机溶剂和一种均相液体催化剂存在下于一个
空管低聚反应器中进行,该反应器上部装有一个分离
器。进行低聚时的压力为31—50巴,温度约为
80℃。
Description
本发明涉及通过在一种有机溶剂和一种由锆化合物和有机金属化合物组成的均相液体催化剂存在下低聚乙烯来制备线性α-烯烃的一种方法和一种设备。
线性α-烯烃,例如含4至8个碳原子的线性α-烯烃,是被广泛用作聚烯烃改性用共聚单体或制备增塑剂、表面活性物质及类似物用原料并被大批量使用的化合物。
由IT-A-24498A/79已知,乙烯在液相低聚成线性α-烯烃。该反应在60至100℃温度和5至30大气压压力下于有机溶剂(例如甲苯、苯或庚烷)中进行。液体催化剂溶于溶剂中,该催化剂由两个组分组成,即由一种锆化物和一种有机金属化合物组成。锆化合物是式Zr(OCOR)4的有机酸锆盐,式中R为烷基、烯或苯基。第二个组分由一种有机铝化合物组成,其中证明最有效的是烷基倍半氯化铝。在该已知方法中,将乙烯送入装有含催化剂之溶剂的搅拌反应器。通过调节温度、锆组分的浓度和摩尔比Al/Zr可将低聚产物的组成控制在窄的范围内。
然而,已知方法使用搅拌反应器的建议却被证明是不利的。理由是,由于要求轴承不透气,因而在高压下操作的搅拌装置非常昂贵,从而确定,必须频繁地关闭搅拌反应器,以便清除在反应器壁上沉积的聚合物,因为它们易于解聚并因而降低产物纯度。
因此,本发明的任务是改进已知的方法并使其在一个简单的反应器中进行,该反应器不需要搅拌装置,因而相当便宜,并不容易受干扰。
按照本发明,该任务的解决方案是,在31至50巴,优选31至40巴压力下,和大约80℃温度下,于一种装有溶剂-催化剂混合物的空管反应器中进行该低聚反应,乙烯从反应器底部送入,低聚产物与溶剂和催化剂一起从反应器下部排出。
本发明的方法在高于已知方法的压力下进行。由于用本发明的空管反应器代替了已知的搅拌反应器,使得这样作成为可能的,因为这里没有轴承,从而不存在密封问题。较高的压力还有一个重要的优点,即可以取得更高的产物纯度。已证明可用31至50巴的压力,而31至40巴是特别合适的。
低聚在低聚反应器下部的液相中进行。由于反应是放热的,反应温度太高会导致产物质量降低,因而必须导出反应热。在本发明的方法中,这由通过反应器循环的乙烯来完成。将乙烯循环中的乙烯溶入液相,以保持低聚反应所需的乙烯浓度。用过量的乙烯控制反应温度。该温度有目的地保持在大约80℃。业已证明,实际上将乙烯以50℃的温度送入低聚反应。
与已知的搅拌反应器相比,本发明的空管反应器还有一个优点,可以通过调节输入气流量控制气态乙烯与流态催化剂之间的交换面积,并使其满足各种要求,首先是物质转变的要求。通常,与搅拌反应器相比,不用多消耗能量即可明显提高交换面积。尽管这样,在本发明的空管反应器中观察到形成的泡沫低于已知的搅拌反应器。
按照本发明,低聚反应器基本上为圆筒状,上端有一截面收敛的部分,它具有分离和洗涤功能。已经确定,在已知的搅拌器中,在乙烯和轻质的低聚物的主要操作温度下,溶剂的蒸气向上蒸出。这不仅在以后的设备部件中是不希望的,而且必须重新排出并处理掉。因此,在本发明的空管反应器中,为了在上部收敛段分离出蒸气,其内设置了洗涤塔板。
本发明空管反应器的顶部蒸气在反应器外冷却,用它来液化溶剂蒸气和轻的低聚物。分离出气相后,使液相部分回流到收敛段顶部,并在洗涤板上分布。由此大量地降低从低聚反应器中上升的蒸气中所含的高沸点组分,使其经板的降液管重新流回反应区。
反应器外壳的截面在分离器范围收敛的作用是提高洗涤塔板上的贮液层高度,这可导致更好的洗涤和冷凝回收效果。
与本发明相关而有目的地使用的催化剂由两个组分组成,其中之一是一种锆化合物ZrClm羧酸根n,式中m+n=4,m=0至2,羧酸根由C4至C8脂肪酸衍生得到,另一个是一种至少有一个乙基配位体的有机铝化合物形式的有机金属化合物,例如像Al(C2H5)3、Al2Cl3(C2H5)3或AlCl(C2H5)2。
下面借助于一个附图所示的实施例进一步说明本发明。
在图示设备中,溶入甲苯的液体催化剂由管线1流入低聚反应器2。该液体由11085kg/h含少量低聚物的甲苯和35kg/h催化剂组成,该催化剂又由7.5kg四异丁酸锆和27.5kg/h乙基倍半氯化铝组成。该液体在31巴压力和40℃温度下送入反应器2。
由管线3向设备供给流量为15000kg/h,压力为30.5巴和温度为30℃的乙烯。这种数量的乙烯是正常操作所必需的。在设备启动前必须以此方式首先加入与设备体积相应数量的乙烯。乙烯经反应器、两个冷却器、两个分离器、一台压缩机和一个加热器循环流动,以使从反应器导出反应热。在压缩机4中加压至32.0巴的压力,在加热器5中加热至50℃的温度,并由下面送入低聚反应器2。在反应器2中在乙烯以吹入提高的情况下在溶剂-催化剂混合物中进行乙烯的低聚。低聚产物保持溶解在溶剂中。
由乙烯与轻质α-烯烃组成的混合物由管6离开反应器,按照反应器中的热力学平衡关系,该混合物还含有一些甲苯。该混合物在冷却器7中冷却到35℃,并收集在分离器8中。在冷却时分出的由甲苯和α-烯烃组成的液体由管9回流反应器2的分离段,在分离段的洗涤塔板上分布,并用来尽可能多地降低由反应器2下部上升的甲苯。分离器8中剩下的气体部分在冷却器10中进行而冷却到温度为5℃,并送入分离器11中。调节冷却器10中的冷却,使得比乙烯重的烯烃尽可能地液化。由管线12向分离器11供给一种来自未示出的烃分离设备的再循环C2馏份。该C2馏份的量为5137kg/h。由管线13抽出基本上纯的循环乙烯,与管线13供给的新鲜乙烯混合后,经管3、压缩机4和加热装置5重新送往反应器2。分离器11的液体产物由管14送向一个未示出的烯烃分解工序,在那里用已知方法将低聚混合物精馏成单一的馏份。
由管15从反应器2中采出一种由甲苯、催化剂、溶解的乙烯和线性α-烯烃组成的液体混合物。为了不让催化剂在以后的设备部件中具有可以导致不希望反应的低聚活性,必须在短时间内破坏催化剂。这可以通过添加水或醇来实现。已证明最有利的是添加脂肪酸来完成该任务。因此,在一个位于反应器2后管线15上不远处的混合段16中,向混合物中添加脂肪酸。对此,3-6kg/h就已足够了。该混合物尔后到达一个例如装有氧化铝的吸附器17的下部。在此吸附除去液体混合物中的金属化合物,即催化剂。该混合物随后由吸附器17顶部进入管14,并由此进行前面提出的分馏馏份中。
总体上,由设备经管14的离开的料流含下述量的下述物质:
乙烯 4922.9kg/h
C2-C4烷烃和烯烃 2338.8kg/h
C6-C8烯烃 4509.7kg/h
C10-C12烯烃 3788.2kg/h
C14-C16烯烃 2724.3kg/h
C18-C20烯烃 1504.5kg/h
C22-C24烯烃 579.9kg/h
C26-C28烯烃 193.2kg/h
甲苯 10661.0kg/h
31222.5kg/h
在这些烃在已经提出的烯烃分解设备中分解成单一馏份之前,按已知方法分离出甲苯,并由管1重新送往反应器2。
Claims (9)
1、在一种有机溶剂和一种由一种锆化合物和一种有机金属化合物组成的均相液体催化剂存在下通过乙烯低聚制备线性α-烯烃的方法,其特征在于,低聚在31至50巴压力下于一个装有溶剂-催化剂混合物的空管低聚反应器中进行,乙烯送入反应器底部,低聚产物与溶剂和催化剂一起从反应器下部排出。
2、按照权利要求1所述的方法,其特征是,用甲苯作溶剂。
3、按照权利要求1或2所述的方法,其特征是,催化剂中的锆化合物是ZrClm羧酸根n,式中m+n=4;m=0至2且羧酸根由C4-C8脂肪酸得到。
4、按照权利要求3所述的方法,其特征是,催化剂中的有机金属化合物是至少有一个乙基配位体的有机铝化合物。
5、按照权利要求4所述的方法,其特征是,催化剂中的有机金属化合物是Al(C2H5)3、Al2Cl3(C2H5)3或AlCl(C2H5)2。
6、按照权利要求1至5所述的方法,其特征是,压力为31至40巴。
7、实施权利要求1所述方法的低聚反应器,具有乙烯和低聚产物用和溶剂-催化剂混合物用的进料和出料管,其特征在于,垂直设置的、基本上呈圆筒状的低聚反应器在其上部段收敛且其内装有一个分离器。
8、按照权利要求7所述的低聚反应器,其特征是,分离器设有多层洗涤塔板。
9、按照权利要求8所述的低聚反应器,其特征是,乙烯和低级低聚产物的出口管与一台冷却器和一台分离器相连接,分离器底部与低聚反应器的分离段相连接。
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FR3105019B1 (fr) * | 2019-12-18 | 2022-07-22 | Ifp Energies Now | Reacteur gaz/liquide d’oligomerisation a zones successives de diametre variable |
FR3123354B1 (fr) * | 2021-05-28 | 2023-05-26 | Ifp Energies Now | Procede d'oligomerisation dans un reacteur a zones de diametres variables comprenant une etape de recyclage d'un solvant prealablement refroidi |
Family Cites Families (4)
Publication number | Priority date | Publication date | Assignee | Title |
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US3726938A (en) * | 1971-11-16 | 1973-04-10 | A Berger | Olefin production |
US4886933A (en) * | 1988-02-15 | 1989-12-12 | Idemitsu Petrochemical Co., Ltd. | Production of linear alpha-olefins |
IT1243745B (it) * | 1990-10-17 | 1994-06-21 | Vectorpharma Int | Composizioni terapeutiche transdermali contenenti farmaco e/o agente promotore dell'assorbimento cutaneo supportato su particelle microporose e microsfere polimeriche e loro preparazione. |
US9403123B2 (en) * | 2014-06-24 | 2016-08-02 | Alstom Technology Ltd | High rotational momentum disperser and use |
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1993
- 1993-11-10 DE DE19934338414 patent/DE4338414C1/de not_active Expired - Fee Related
-
1994
- 1994-11-08 CN CN94118705A patent/CN1048976C/zh not_active Expired - Fee Related
Cited By (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101238083B (zh) * | 2005-08-10 | 2012-02-08 | 林德股份公司 | 改进的线型α-烯烃的干燥方法 |
CN105753622A (zh) * | 2008-01-30 | 2016-07-13 | 林德股份公司 | 制备线性α-烯烃的方法 |
US9593055B2 (en) | 2008-01-30 | 2017-03-14 | Saudi Basic Industries Corporation | Method for preparing linear alpha-olefins |
CN105753622B (zh) * | 2008-01-30 | 2019-01-29 | 林德股份公司 | 制备线性α-烯烃的方法 |
US8809613B2 (en) | 2009-07-24 | 2014-08-19 | Saudi Basic Industries Corporation | Method for preparing linear alpha-olefins |
CN102029137A (zh) * | 2009-10-07 | 2011-04-27 | 林德股份公司 | 对放热反应进行反应控制的方法及其设备 |
KR20170058935A (ko) * | 2014-09-22 | 2017-05-29 | 미쓰비시 가가꾸 가부시키가이샤 | α-올레핀 저중합체의 제조 방법 및 제조 장치 |
KR102385968B1 (ko) * | 2014-09-22 | 2022-04-12 | 미쯔비시 케미컬 주식회사 | α-올레핀 저중합체의 제조 방법 및 제조 장치 |
Also Published As
Publication number | Publication date |
---|---|
DE4338414C1 (de) | 1995-03-16 |
CN1048976C (zh) | 2000-02-02 |
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