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1. 发明申请

WO1993019100A1 A POLYMERIZATION CATALYST CARRIER PREPARED BY SPRAY CRYSTALLIZATION 审中-公开
标题翻译：通过喷雾结晶制备的聚合催化剂载体
公开(公告)号：WO1993019100A1
公开(公告)日：1993-09-30
申请号：PCT/FI1993000116
申请日：1993-03-23
申请人： NESTE OY , KOSKINEN, Jukka , JOKINEN, Petri
发明人： NESTE OY
IPC分类号： C08F04/02
CPC分类号： B01J37/32 , B01J19/088 , B01J19/26 , B01J37/0045 , B01J2219/00119 , B01J2219/00121 , B01J2219/00123 , B01J2219/00159 , C08F10/00 , C08F4/022
摘要： When particulate carriers are prepared for olefin polymerization procatalysts that comprise a transition metal compound reacted upon the carrier, the problem is to achieve particles, the particle size, particle size distribution and particle form, i.e. the morphology, of which is suitable. These problems have been solved in the present invention by a method in which: (a) a heated melt of a complex compound is provided having the formula (I): MgC12.nROH.mED in which ROH depicts a lower (C1-6) aliphatic alcohol, ED depicts an electron donor, n is 1 to 6 and m is 0 to 1, (b) the provided heated melt is fed to a nozzle atomizing it, (c) the melt to be atomized is spayed from said nozzle into a chamber, where it is distributed in the form of atomized melt and then solidified to fine carrier particles and (d) the fine carrier particles are recovered. During this process an electric charge is fed into the melt to be atomized or has been atomized, which decreases the surface tension of the solidified melt and prevents the agglomeration of the formed droplets. The charge can be achieved by arranging in connection with the nozzle an electrode, which together with, for example, the grounded melt forms a static electric couple.
摘要翻译：当为包含过渡金属化合物在载体上反应的烯烃聚合原催化剂制备颗粒载体时，问题是实现颗粒，颗粒尺寸，粒度分布和颗粒形式，即其形态是合适的。这些问题已经通过以下方法解决了：（a）提供了具有式（I）的配位化合物的加热熔体：其中ROH表示低级（C1-6）脂族醇，ED表示电子给体，n为1至6，m为0至1，（b）将所提供的加热熔体进料到雾化雾化器的喷嘴中，（c）待雾化的熔体从所述喷嘴喷射到一个室，其中以雾化的熔体的形式分布，然后固化成细小的载体颗粒，（d）回收细的载体颗粒。在该过程中，将电荷送入熔体中以雾化或已被雾化，这降低了凝固熔体的表面张力并防止形成的液滴的聚集。可以通过与喷嘴结合设置电极来实现电荷，电极与例如接地熔体一起形成静电耦合。

2. 发明申请

WO1993011164A1 METHOD FOR THE PREPARATION OF AN OLEFIN POLYMERIZATION CATALYST CONSISTING OF PARTICLES OF EQUAL SIZE 审中-公开
标题翻译：制备均匀颗粒颗粒的烯烃聚合催化剂的方法
公开(公告)号：WO1993011164A1
公开(公告)日：1993-06-10
申请号：PCT/FI1992000322
申请日：1992-11-27
申请人： NESTE OY , GAROFF, Thomas , KOSKINEN, Jukka
发明人： NESTE OY
IPC分类号： C08F04/02
CPC分类号： C08F10/00 , C08F4/6543
摘要： In the invention a particular procatalyst composition intended for the polymerization of olefins is prepared by reacting the carrier particles consisting of a MgCl2-C2H5OH-complex with TiCl4. When the method is applied into pilot-scale it was noticed that the procatalyst composition obtained produced olefin polymer, the finely-divided material portion of which was deterioratingly high. This was caused by the fact that the procatalyst composition particles had decomposed to finely-divided material during the synthesis, which was then in the polymerization repeated in the polymer structure due to the so-called replica phenomenon. In the invention it has unexpectedly been noticed that the breaking of the carrier particles is not a result of e.g. mechanical strain but of the fact that when the carrier particles react with the TiCl4 a heavy discharge of hydrogen chloride is first occurring as a result of the reaction which breaks the carrier particles. The carrier particles can, according to the invention, be maintained undamaged during the reaction by distributing the release in the reaction or from the reaction of the hydrogen chloride created in the reaction to a molar velocity not exceeding the fivefold value of the molar mean velocity of the release. This is achieved among other things by adding reagents unusually slowly, by using lower temperatures and heating velocities, by intensifying the agitation, by using an overpressure and/or by conducting diluting inert gas into the reaction mixture.
摘要翻译：在本发明中，用于烯烃聚合的特定主催化剂组合物是通过使由MgCl 2 -C 2 H 5 O-络合物组成的载体颗粒与TiCl 4反应来制备的。当该方法应用于中试规模时，注意到获得的主催化剂组合物产生的烯烃聚合物，其细碎材料部分劣化。这是由于前催化剂组合物颗粒在合成过程中分解成细碎的材料，然后由于所谓的复制现象而在聚合物结构中重复聚合。在本发明中，已经意外地注意到，载体颗粒的破坏不是例如，机械应变，但是当载体颗粒与TiCl 4反应时，由于引起载体颗粒的反应的结果，首先发生重的氯化氢排放。根据本发明，载体颗粒可以在反应期间通过在反应中分配释放或从反应中产生的氯化氢的反应分散到不超过摩尔平均速度的五倍值的摩尔速度发布。通过使用较低的温度和加热速度，通过使用过压和/或通过将惰性气体稀释到反应混合物中来强化搅拌，实现了异常缓慢的添加试剂。

3. 发明申请

WO1993011166A1 METHOD FOR THE PREPARATION OF A PARTICULATE CARRIER FOR A POLYMERIZATION CATALYST 审中-公开
标题翻译：用于制备聚合催化剂的颗粒载体的方法
公开(公告)号：WO1993011166A1
公开(公告)日：1993-06-10
申请号：PCT/FI1992000324
申请日：1992-11-27
申请人： NESTE OY , KOSKINEN, Jukka , GAROFF, Thomas
发明人： NESTE OY
IPC分类号： C08F04/02
CPC分类号： C08F10/00 , C08F4/6543 , C08F4/022
摘要： The invention relates to a method for preparing a particulate carrier for an olefin polymerization procatalyst comprising a transition metal compound reacted for a carrier. In the method a melt Mg Cl2-CH5OH-complex is provided containing in the average 3.3 to 5.5 C2H5OH-molecules as per each MgCl2-molecule, the melt MgCl2-complex is sprayed through a nozzle dispersing it into a chamber, wherein a particulate carrier is formed of it and the ready particulate carrier is removed from the chamber. In the methods known so far difficulties have been encountered in endeavours to produce a carrier having an optimal C2H5OH content. In this invention the problems have been solved by removing by the aid of heat so much C2H5OH from the MgCl2-CH5OH-complex in connection with the spraying that the particulate carrier obtained will continue at the average 2.0 to 3.2 C2H5OH molecules as per each MgCl2 molecule. Such a carrier has a suitable C2H5OH content and a good morphology and spraying it does not raise any difficulties.
摘要翻译：本发明涉及一种制备用于烯烃聚合主催化剂的颗粒载体的方法，其包括与载体反应的过渡金属化合物。在该方法中，根据每个MgCl 2分子，提供含有平均3.3至5.5个C 2 H 5 OH分子的熔融MgCl 2 -CH 5 OH络合物，熔融MgCl 2 - 络合物通过将其分散到室中的喷嘴喷雾，其中颗粒载体由其形成，并且将容器颗粒载体从室中移出。迄今为止已知的方法已经遇到难以产生具有最佳C2H5OH含量的载体的方法。在本发明中，通过加热除去MgCl 2 -CH 5 OH络合物中的多少C 2 H 5 OH与喷雾相结合，已经解决了这些问题，所得到的颗粒载体将按每个MgCl 2分子在平均2.0-3.2的C2H5OH分子上继续。这种载体具有合适的C2H5OH含量和良好的形态和喷雾性，不会造成任何困难。

4. 发明申请

WO1992021705A1 METHOD FOR PREPARING SOLID CARRIER PARTICLES OF EQUAL SIZE FOR POLYMERIZATION CATALYST USING ROTATING ATOMIZING MEANS 审中-公开
标题翻译：使用旋转原子化方法制备聚合催化剂的等尺寸固体载体颗粒的方法
公开(公告)号：WO1992021705A1
公开(公告)日：1992-12-10
申请号：PCT/FI1992000170
申请日：1992-05-29
申请人： NESTE OY , KOSKINEN, Jukka , LOUHELAINEN, Jarmo
发明人： NESTE OY
IPC分类号： C08F04/02
CPC分类号： C08F10/00 , C08F4/022
摘要： The active carrier particles of even size of the polymerization catalyst are prepared so that a melt of a complex composition is provided having the formula (I): MgCl2 nROH mED, in which ROH depicts an aliphatic alcohol, R is a C1-C6 alkyl, ED depicts an electron donor, n is 1 to 6 and m is 0 to 1; the melt provided is fed to a nozzle (4); the melt is sprayed from the nozzle (4) to the spraying area (5), in which it is divided into fine melt droplets and possibly partly solidifies; the possibly partly solidified melt particles are transferred to a cooled crystallization area (6), where they crystallize to solid carrier particles; and the solid carrier particles are recovered. The melt mentioned is sprayed through a nozzle (4), which is rotated or which has attached to it a member that rotates and throws melt outwards from the rotating center to the spraying area (5).
摘要翻译：制备具有均匀尺寸的聚合催化剂的活性载体颗粒，使得提供具有式（I）的配合物组合物的熔体：MgCl 2 nROH mED，其中ROH表示脂族醇，R是C1-C6烷基， ED描绘电子给体，n为1至6，m为0至1; 所提供的熔体被供给到喷嘴（4）; 熔体从喷嘴（4）喷射到喷涂区域（5），其中它被分成细熔液滴并且可能部分地固化; 可能部分固化的熔体颗粒被转移到冷却的结晶区域（6），在那里它们结晶成固体载体颗粒; 并回收固体载体颗粒。所提到的熔体通过喷嘴（4）喷射，喷嘴（4）旋转或附接到其上旋转并从旋转中心向喷出的喷射区域（5）向外熔化的部件。

5. 发明申请

WO1993011165A1 PREPARATION OF A SOLID ZIEGLER CATALYST BY USING A MULTIFUNCTIONAL, PIVOTING, INCLINABLE REACTOR AND THE EQUIPMENT FOR THIS 审中-公开
标题翻译：通过使用多功能，投放式，不可逆的反应器及其设备来制备固体齐纳尔催化剂
公开(公告)号：WO1993011165A1
公开(公告)日：1993-06-10
申请号：PCT/FI1992000323
申请日：1992-11-27
申请人： NESTE OY , KOSKINEN, Jukka , GAROFF, Thomas , LOUHELAINEN, Jarmo
发明人： NESTE OY
IPC分类号： C08F04/02
CPC分类号： B01J19/18 , B01D21/24 , B01J8/006 , B01J8/10 , B01J2219/00051 , B01J2219/00173 , B01J2219/00182 , B01J2219/185 , B01J2219/187 , C08F10/00 , Y10S502/514 , C08F4/60 , C08F4/651 , C08F4/6545 , C08F110/06 , C08F2500/12
摘要： The invention relates to a method and equipment for the preparation of such a solid catalyst suitable for olefin polymerization that comprises a transition metal compound reacted for a carrier. In the method the reagents mentioned are fed into a reaction vessel (1), reacted to raw procatalyst, after which the liquid reaction residue is removed through a bottom sieve (3) in the vessel (1), the raw procatalyst obtained is washed with a washing liquid, which is also removed through the bottom sieve (3), after which the raw procatalyst is dried and removed from the vessel (1). The problem has previously been that the procatalyst product contains too much harmful, finely-divided material. Now, this disadvantage has been removed by furnishing the vessel (1) with a tilting means (4), whereby the reaction residue liquid and/or the washing liquid along with its impurities can be removed by keeping the vessel (1) tilted to an acute angle with respect to its vertical axis, allowing the raw procatalyst settle to cover the tilted side part of the bottom sieve (3), and by filtering decanting the liquid away from the vessel (1) through the part of the bottom sieve (3) that is not covered by raw procatalyst.
摘要翻译：本发明涉及一种制备适用于烯烃聚合的固体催化剂的方法和设备，其包括对载体反应的过渡金属化合物。在所述方法中，将所述试剂加入到反应容器（1）中，与原始催化剂反应，然后通过容器（1）中的底部筛（3）除去液体反应残余物，将得到的原料前催化剂用洗涤液，也通过底部筛子（3）除去，然后干燥原料主催化剂并从容器（1）中取出。以前的问题是，前催化剂产品含有太多有害的细碎材料。现在，通过用容器（1）提供倾斜装置（4）已经消除了这个缺点，由此可以通过将容器（1）倾斜到相对于其垂直轴线具有锐角，允许原始催化剂沉降以覆盖底部筛（3）的倾斜侧部分，并且通过过滤将液体从容器（1）倾倒通过底部筛（3）的一部分），不包括原始催化剂。

6. 发明申请

WO1992016747A1 METHOD FOR THE DOSAGE OF A FLUIDIZED POLYMERIZATION CATALYST INTO A POLYMERIZATION REACTOR 审中-公开
标题翻译：将聚合催化剂流化成聚合反应器的方法
公开(公告)号：WO1992016747A1
公开(公告)日：1992-10-01
申请号：PCT/FI1992000080
申请日：1992-03-20
申请人： NESTE OY , KOSKINEN, Jukka , NYFORS, Klaus , LESKINEN, Pauli
发明人： NESTE OY
IPC分类号： F04B07/06
CPC分类号： B01J8/003 , B01J8/002 , B01J8/0035 , F04B7/06
摘要： The dosage pump according to the invention comprises a cylinder (2), a piston (4) moving back and forth in it and openable and closable inlet (5) and outlet (6) opening in the piston-swept space (3). The opening and closing of the openings mentioned are carried out by an intermediate pipe (7) arranged movably, and with respect thereto tightly, between the cylinder (2) and the mantles of the piston (4). The transmission opening (8) of the intermediate pipe (7) is transferred by moving the intermediate pipe (7) upon the inlet (5) and the outlet (6) opening, the whole surface of the intermediate pipe always covering one of the inlet (5) and outlet (6) openings mentioned. The dosage pump mentioned can preferably be applied for the dosage of hard-flowing substances, e.g. for feeding solid catalyst or wax into olefin polymerization reactor.
摘要翻译：根据本发明的剂量泵包括气缸（2），在其中前后移动的活塞（4）和在活塞扫掠空间（3）中开口的可开启和关闭的入口（5）和出口（6）。所述开口的打开和关闭由中间管道（7）进行，所述中间管道（7）在所述气缸（2）和所述活塞（4）的外壳之间可移动地并相对于其紧密配置。通过在入口（5）和出口（6）开口处移动中间管（7）来转移中间管（7）的传动开口（8），中间管的整个表面总是覆盖入口（5）和出口（6）开口。所提及的剂量泵可以优选用于硬流动物质的剂量，例如用于将固体催化剂或蜡进料到烯烃聚合反应器中。

7. 发明申请

WO1998021263A1 PROCESS FOR THE PREPARATION OF POLYHYDROXY ACIDS 审中-公开
标题翻译：制备聚羟基酸的方法
公开(公告)号：WO1998021263A1
公开(公告)日：1998-05-22
申请号：PCT/FI1997000675
申请日：1997-11-07
申请人： NESTE OY , SÖDERGÅRD, Anders , STOLT, Mikael
发明人： NESTE OY
IPC分类号： C08G63/08
CPC分类号： C08G63/823
摘要： The invention relates to a process for the polymerization or copolymerization of cyclic lactones of hydroxy acids by using as catalysts organometallic iron compounds containing iron salts or iron esters of carboxylic acids having at maximum 18 carbon atoms or some iron complexes. The invention relates preferably to the polymerization of lactide by using an iron acetate catalyst or initiator.
摘要翻译：本发明涉及通过使用含有最多18个碳原子的羧酸或一些铁络合物的铁盐或铁酯的有机金属铁化合物作为催化剂聚合或共聚羟基酸的环状内酯的方法。本发明优选地通过使用乙酸铁催化剂或引发剂来优化丙交酯的聚合。

8. 发明申请

WO1998007675A1 PROCESS FOR THE PRODUCTION OF 2-BUTYL-2-ETHYL-1,3-PROPANEDIOL 审中-公开
标题翻译： 2-丁基-2-乙基-1,3-丙二醇的制备方法
公开(公告)号：WO1998007675A1
公开(公告)日：1998-02-26
申请号：PCT/FI1997000484
申请日：1997-08-19
申请人： NESTE OY , LINDFORS, Lars-Peter , HEINOLA, Kalevi , KULMALA, Kari , HAKANPÄÄ-LAITINEN, Hannele , RINTALA, Lea , PARKKINEN, Lea , LEHTINEN, Vesa-Matti
发明人： NESTE OY
IPC分类号： C07C31/20
CPC分类号： C07C29/38 , C07C31/20
摘要： the present invention concerns a process for producing 2-butyl-2-ethyl-1,3-propanediol. According to the process, a reaction mixture is formed, containing 2-ethylhexanal and formaldehyde, into which a hydroxide compound is fed, whereby 2-ethylhexanal and formaldehyde are reacted to produce 2-butyl-2-ethyl-1,3-propanediol. According to the invention, the hydroxide compound is incrementally fed into the reaction mixture. Preferably, the hydroxide compound is fed at least at two input rates, in such a way that the heat production of the reaction between 2-ethylhexanal and formaldehyde immediately after each increase of the input rate of the hydroxide compound is at least almost the same. The invention allows for the production of BEPD in a controlled and safe manner, with excellent yields.
摘要翻译：本发明涉及一种生产2-丁基-2-乙基-1,3-丙二醇的方法。根据该方法，形成含有2-乙基己醛和甲醛的反应混合物，其中加入氢氧化物，由此使2-乙基己醛和甲醛反应，生成2-丁基-2-乙基-1,3-丙二醇。根据本发明，向反应混合物中逐渐加入氢氧化物。优选地，氢氧化物化合物至少以两种输入速率进料，使得在每次增加氢氧化物化合物的输入速率之后立即在2-乙基己醛和甲醛之间的反应的热产生至少几乎相同。本发明允许以控制和安全的方式生产BEPD，具有优异的产率。

9. 发明申请

WO1997023474A1 ADDITIVES USABLE IN PREPARATION OF ALKENYL SUCCINIC ANHYDRIDE 审中-公开
标题翻译：添加剂可用于制备烷基苯甲酸酐
公开(公告)号：WO1997023474A1
公开(公告)日：1997-07-03
申请号：PCT/FI1996000657
申请日：1996-12-12
申请人： NESTE OY , MÄKIPEURA, Petri , KAPANEN, Mika , TULISALO, Jukka , KOSKIMIES, Salme
发明人： NESTE OY
IPC分类号： C07D307/60
CPC分类号： C07C51/567 , C07C57/13
摘要： In the preparation of alkenyl succinic anhydride (ASA) from an olefinically unsaturated hydrocarbon and a maleic anhydride, additives are used in the preparation reaction in order to improve the yield of the product and to reduce side reactions. According to the present invention, quinone and hydroquinone derivatives as well as dialkyl sulfoxides and transition-metal acetylacetonate have such properties. The amounts to be added are approx. 0.01-2 mol % of the amount of maleic anhydride. The olefin is preferably a straight-chain alpha -olefin or a straight-chain or branched internal olefin having a chain length of 6-20 carbon atoms. The olefin may also be a polyolefin, in which case the preferred molecular weight is 900-1500. The preparation process may be of the batch type or the semi-batch type, and the maleic anhydride and the additive may be added in several batches or as a continuous feed which may be even or variable. The ASA obtained by the process may be used in particular as an additive in foods, for hydroxy sizing of paper, or as a dispersing agent in lubricants.
摘要翻译：在由烯属不饱和烃和马来酸酐制备链烯基琥珀酸酐（ASA）时，在制备反应中使用添加剂以提高产物的产率并减少副反应。根据本发明，醌和氢醌衍生物以及二烷基亚砜和过渡金属乙酰丙酮化物具有这样的性质。添加量约为。 0.01-2摩尔％的马来酸酐。烯烃优选为直链α-烯烃或链长为6-20个碳原子的直链或支链内烯烃。烯烃也可以是聚烯烃，在这种情况下，优选的分子量为900-1500。制备方法可以是间歇式或半批式，并且马来酸酐和添加剂可以分批加入或作为可以均匀或可变的连续进料。通过该方法获得的ASA可特别用作食品中的添加剂，用于纸张的羟基上浆或作为润滑剂中的分散剂。

10. 发明申请

WO1996026913A1 PROCESS FOR PREPARATION OF POLY-N-BUTENES HAVING HIGH VISCOSITY 审中-公开
标题翻译：制备具有高粘度的聚N-丁烯的方法
公开(公告)号：WO1996026913A1
公开(公告)日：1996-09-06
申请号：PCT/FI1995000106
申请日：1995-02-27
申请人： NESTE OY , KAPANEN, Mika , HALME Erkki , KOSKIMIES Salme
发明人： NESTE OY
IPC分类号： C07C02/20
CPC分类号： C07C2/04 , C07C2527/1213 , C07C2531/02 , C07C2531/04
摘要： The application relates to a process for the oligomerization of olefins, preferably a hydrocarbon blend which contains 1-butenes and/or 2-butenes, for example the so-called Raffinate II stream and cyclic aromatic or alicyclic hydrocarbons, by means of BF3 and a cocatalyst. The aromatic hydrocarbon may preferably be styrene, alpha-methyl styrene, alkyl styrene, or a blend thereof, and the alicyclic hydrocarbon may be vinyl cyclohexane, vinyl cyclohexene, or a blend thereof. The cocatalyst is an aliphatic alcohol, carboxylic acid or inorganic acid. The oligomerization may be carried out with or without a medium, at a temperature above 0 DEG C, by adjusting the pressure to 1-10 bar by means of BF3 gas. The oligomer prepared by the process may be used as a solvent or an additive in fuels or lubricants, in surfactants, in white and cosmetic oils requiring extra purity, and in PVC and polyolefin plastics. In polyester and vinyl ester resins this oligomer can be used for replacing in part the monomer (e.g. styrene), thus reducing monomer evaporation and to inhibit shrinkage at the hardening stage, and it also improves the optical properties of the said resins.
摘要翻译：本申请涉及烯烃低聚的方法，优选含有1-丁烯和/或2-丁烯的烃共混物，例如所谓的残液II类和环状芳族或脂环族烃，通过BF 3和助催化剂。芳族烃可以优选为苯乙烯，α-甲基苯乙烯，烷基苯乙烯或其共混物，脂环族烃可以是乙烯基环己烷，乙烯基环己烯或其共混物。助催化剂是脂族醇，羧酸或无机酸。通过用BF 3气调节压力至1-10巴，可以在高于0℃的温度下使用或不用介质进行低聚。通过该方法制备的低聚物可以用作燃料或润滑剂，表面活性剂，需要额外纯度的白色和化妆油以及PVC和聚烯烃塑料中的溶剂或添加剂。在聚酯和乙烯基酯树脂中，该低聚物可用于部分单体（例如苯乙烯）的替代，从而减少单体蒸发并抑制硬化阶段的收缩，并且还改善了所述树脂的光学性能。

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