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公开(公告)号：US5883288A
公开(公告)日：1999-03-16
申请号：US791052
申请日：1997-01-28
申请人： Gabriele Iffland , Albrecht Dams , Alexander Weck , Heinrich Aichinger , Holger Herbst , Gerhard Nestler , Herbert Exner , Willi Schmidt , Matthias Geisendorfer , Toni Dockner
发明人： Gabriele Iffland , Albrecht Dams , Alexander Weck , Heinrich Aichinger , Holger Herbst , Gerhard Nestler , Herbert Exner , Willi Schmidt , Matthias Geisendorfer , Toni Dockner
CPC分类号： C07C67/08
摘要： In the process for the continuous preparation of alkyl esters of (meth)acrylic acid by reacting (meth)acrylic acid with monohydric alkanols having from 1 to 8 carbon atoms in the presence of an acid esterification catalyst in a reaction zone, there is discharged from the reaction zone a product mixture which comprises the alkyl (meth)acrylate formed, the catalyst and the by-products formed during the course of the esterification having boiling points higher than that of the alkyl (meth)acrylate, and from which the alkyl (meth)acrylate is separated by distillation in a separation zone. The product mixture discharged from the reaction zone is fed to a rectification unit (I), in this unit the product mixture discharged is separated by rectification into at least one product (I) comprising the alkyl ester of (meth)acrylic acid and a product (II) comprising the catalyst, the product (I) is fed to a further rectification unit (II) and in this the alkyl ester of (meth)acrylic acid is separated off by rectification.
摘要翻译： 在反应区酸性酯化催化剂存在下，使（甲基）丙烯酸与具有1〜8个碳原子的一元链烷醇反应连续制备（甲基）丙烯酸烷基酯的方法中， 所述反应区包含形成的（甲基）丙烯酸烷基酯，在酯化过程中形成的催化剂和副产物的沸点高于（甲基）丙烯酸烷基酯的产物混合物，并且烷基（ 甲基）丙烯酸酯在分离区中蒸馏分离。 将从反应区排出的产物混合物供给到精馏单元（I），在该单元中，排出的产物混合物通过精馏分离成至少一种包含（甲基）丙烯酸的烷基酯的产物（I）和产物 （II），将产物（I）进料到另一精馏单元（II）中，通过精馏分离（甲基）丙烯酸的烷基酯。
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公开(公告)号：US5945560A
公开(公告)日：1999-08-31
申请号：US791054
申请日：1997-01-28
申请人： Gabriele Iffland , Albrecht Dams , Alexander Weck , Heinrich Aichinger , Holger Herbst , Gerhard Nestler , Herbert Exner
发明人： Gabriele Iffland , Albrecht Dams , Alexander Weck , Heinrich Aichinger , Holger Herbst , Gerhard Nestler , Herbert Exner
IPC分类号： B01J27/02 , B01J31/02 , C07B41/12 , C07B61/00 , C07C67/08 , C07C67/54 , C07C69/54 , C07C69/52
摘要： In a process and an apparatus for the continuous preparation of alkyl esters of (meth)acrylic acid by reacting (meth)acrylic acid with alkanols having from 1 to 5 carbon atoms in a homogeneous, liquid, solvent-free phase at elevated temperature and in the presence of an acid esterification catalyst, in which the (meth)acrylic acid, the alkanol and the catalyst are fed to a reaction zone, the water formed is removed by rectification during a residence time as constituent of a mixture comprising alkanol in a rectification unit superposed on the reaction zone, the distillate thus obtained is separated into an organic phase comprising alkanol and an aqueous phase comprising water, the organic phase is returned to the rectification unit, the reaction mixture is discharged from the reaction zone and conveyed into a distillative separation zone comprising further rectification units and in the latter the alkyl (meth)acrylate formed is separated off.
摘要翻译： 在（甲基）丙烯酸的烷基酯连续制备方法和装置中，通过使（甲基）丙烯酸与具有1至5个碳原子的链烷醇在高温和均相，液体，无溶剂相中 将（甲基）丙烯酸，链烷醇和催化剂进料到反应区中的酸酯化催化剂的存在，在停留时间内通过精馏除去形成的水，作为在精馏中的链烷醇的混合物的组分 单元重叠在反应区上，将由此获得的馏出物分离成包含链烷醇和含水水相的有机相，将有机相返回至精馏单元，将反应混合物从反应区排出并输送至蒸馏 分离区包含进一步的精馏单元，后者分离形成的（甲基）丙烯酸烷基酯。
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公开(公告)号：US06512138B1
公开(公告)日：2003-01-28
申请号：US09567983
申请日：2000-05-10
IPC分类号： C07C6952
CPC分类号： C07C67/08 , C07C67/327 , C07C69/54
摘要： The process for the esterification of (meth)acrylic acid with an alkanol in the presence of an esterification catalyst, in which unconverted starting compounds and the (meth)acrylate to be formed are separated off by distillation and an oxyester-containing bottom product is formed and is separated off, and (a) in the bottom product separated off, the oxyesters present are cleaved, if required after the addition of (meth)acrylic acid and/or oligomeric (meth)acrylic acid, directly in the presence of acid catalysts differing from (meth)acrylic acid and/or oligomeric (meth)acrylic acid, and the cleavage products are removed, a cleavage residue remaining, or (b) the oxyesters are first removed by distillation from the cleavage product separated off, a distillation residue remaining, and the oxyesters removed are cleaved, if required after addition of (meth)acrylic acid and/or oligomeric (meth)acrylic acid, in the presence of acid catalysts differing from (meth)acrylic acid and/or oligomeric (meth)acrylic acid, and the cleavage products are removed, a cleavage residue remaining, is carried out in such a way that the cleavage residue obtained in step (a) or the cleavage residue obtained in step (b) is hydrolytically cleaved together with the resulting distillation residue in the presence of water and acids or bases.
摘要翻译： 在酯化催化剂存在下，（甲基）丙烯酸与烷醇的酯化反应的方法，其中未转化的起始化合物和待形成的（甲基）丙烯酸酯通过蒸馏和含有含氧酯的底部产物分离出来 并分离出来，（a）在分离出的底部产物中，如果需要，在酸催化剂存在下直接加入（甲基）丙烯酸和/或低聚（甲基）丙烯酸后，存在的氧化酯被切割 与（甲基）丙烯酸和/或低聚（甲基）丙烯酸不同，除去裂解产物，剩余的裂解残余物或（b）氧酯首先通过蒸馏从分离的裂解产物中除去，蒸馏残余物 除去（甲基）丙烯酸和/或低聚（甲基）丙烯酸之外，如果需要，在不同于（甲基）丙烯酸和/或低聚（甲基）丙烯酸的酸催化剂的存在下， 甲基）丙烯酸，并且去除裂解产物，残留切割残余物，使得步骤（a）中获得的裂解残基或步骤（b）中获得的裂解残基与 在水和酸或碱的存在下产生蒸馏残余物。
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4.发明授权Process for stabilizing (METH)acrylic acid esters against unwanted radical polymerization 有权稳定（METH）丙烯酸酯以防止不必要的自由基聚合的方法公开(公告)号：US06518452B1
公开(公告)日：2003-02-11
申请号：US09485192
申请日：2000-02-07
IPC分类号： C07C6952
摘要： A method is described of stabilizing (meth)acrylic esters against unwanted free-radical polymerization, in which the mixture to be stabilized has added to it a polymerization inhibitor mixture comprising at least one nitroxyl radical and/or at least one organic compound having at least one nitroso group, and at least one p-phenylenediamine.
摘要翻译： 描述了稳定（甲基）丙烯酸酯以防止不需要的自由基聚合的方法，其中要稳定的混合物加入其中包含至少一个硝酰基和/或至少一种有机化合物的聚合抑制剂混合物，其至少具有至少 一个亚硝基和至少一个对苯二胺。
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公开(公告)号：US06353130B1
公开(公告)日：2002-03-05
申请号：US09830565
申请日：2001-05-07
IPC分类号： C07C6952
摘要： A method for continuous production of (meth)acrylic alkyl esters by reacting (meth)acrylic acid with alkanols containing 1-8 C-atoms, whereby raw (meth)acrylic acid containing acetic acid is used as a starting compound and the alkyl acetate that is formed as a by-product is evacuated in an appropriate area.
摘要翻译： 使用（甲基）丙烯酸与含有1-8个碳原子的链烷醇反应连续生产（甲基）丙烯酸烷基酯的方法，由此使用含有乙酸的原料（甲基）丙烯酸作为原料化合物， 形成副产物在适当的区域被排空。
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公开(公告)号：US5910603A
公开(公告)日：1999-06-08
申请号：US701989
申请日：1996-08-23
CPC分类号： C07C67/327 , C07C67/08 , C07C67/60
摘要： In a process for esterifying (meth)acrylic acid with an alkanol in the presence of an acidic esterification catalyst, in which unconverted starting compounds and the (meth)acrylates to be formed are separated off by distillation and an oxyester-containing bottom product is formed, the bottom product is separated off and is heated in the presence of an acid to 150-250.degree. C. and the pressure is adjusted so that the cleavage products formed under the abovementioned conditions from the oxyesters contained in the bottom product evaporate directly. The process can be carried out in the presence of molecular oxygen. Mineral acids, for example sulfuric acid or phosphoric acid and/or alkanesulfonic or arylsulfonic acids, for example methanesulfonic acid or p-toluenesulfonic acid, can be added to the bottom product.
摘要翻译： 在酸性酯化催化剂存在下，用链烷醇酯化（甲基）丙烯酸的方法中，其中未转化的起始化合物和待形成的（甲基）丙烯酸酯通过蒸馏分离并形成含有含氧酯的底部产物 将底部产物分离并在酸存在下加热至150-250℃，并调节压力，使得在上述条件下由底部产物中含有的含氧酯形成的裂解产物直接蒸发。 该方法可以在分子氧的存在下进行。 矿物酸，例如硫酸或磷酸和/或链烷磺酸或芳基磺酸，例如甲磺酸或对甲苯磺酸，可以加入到底部产物中。
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公开(公告)号：US06617470B1
公开(公告)日：2003-09-09
申请号：US09831349
申请日：2001-05-11
IPC分类号： C07C6954
CPC分类号： C07C67/08 , C07C67/327 , C07C69/54
摘要： In a process for esterifying (meth)acrylic acid with an alkanol in the presence of an esterification catalyst, in which unconverted starting compounds and (meth)acrylic ester to be formed are separated off by distillation and an oxyester-containing bottom product is formed, the bottom product is first separated off and then the oxyesters contained in it are cleaved in the presence of a relatively long-chain alkylbenzenesulfonic acid at elevated temperatures.
摘要翻译： 在酯化催化剂存在下，用链烷醇酯化（甲基）丙烯酸的方法中，其中未转化的起始化合物和待形成的（甲基）丙烯酸酯通过蒸馏分离出来并形成含有含氧酯的底部产物， 首先将底部产物分离，然后在高温下在相对长链烷基苯磺酸存在下将含有的含氧酯切割。
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8.发明授权Method of cleaning plant parts for the preparation or processing of (meth)acrylic esters 有权（甲基）丙烯酸酯的制备或加工清洁工厂零件的方法公开(公告)号：US06568406B2
公开(公告)日：2003-05-27
申请号：US09509817
申请日：2000-04-18
IPC分类号： G08B900
CPC分类号： B08B3/08 , C11D7/06 , C11D11/0041 , C11D11/0064
摘要： Plant parts which are used for the production or processing of (meth)acrylic esters are cleaned by (a) emptying the plant parts, (b) flushing the plant parts with aqueous 5 to 50% strength by weight alkali metal hydroxide solution, (c) removing the alkali metal hydroxide solution from the plant parts, (d) if required, washing the plant parts with water and (e) if required, drying the plant parts.
摘要翻译： 用于生产或加工（甲基）丙烯酸酯的植物部分通过（a）排空植物部分进行清洁，（b）用5-50％重量的碱金属氢氧化物水溶液冲洗植物部分，（c ）从植物部分去除碱金属氢氧化物溶液，（d）如果需要，用水洗涤植物部分，（e）如果需要，干燥植物部分。
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公开(公告)号：US06207022B1
公开(公告)日：2001-03-27
申请号：US08319667
申请日：1994-10-07
申请人： Toni Dockner , Gerhard Nestler , Holger Herbst , Helmut Lermer , Hans Martan , Herbert Vogel , Herbert Exner
发明人： Toni Dockner , Gerhard Nestler , Holger Herbst , Helmut Lermer , Hans Martan , Herbert Vogel , Herbert Exner
IPC分类号： B01D334
CPC分类号： C07C51/487 , Y10S203/22 , C07C57/04
摘要： Crude (meth)acrylic acid is purified by a process in which a primary amine compound and an organic sulfonic acid are added to the crude (meth)acrylic acid and the latter is then worked up by distillation.
摘要翻译： 粗（甲基）丙烯酸通过其中将伯胺化合物和有机磺酸加入到粗（甲基）丙烯酸中的方法纯化，然后将其通过蒸馏处理。
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公开(公告)号：US06072076A
公开(公告)日：2000-06-06
申请号：US789542
申请日：1997-01-27
申请人： Willi Schmidt , Matthias Geisendorfer , Alexander Weck , Toni Dockner , Holger Herbst , Gerhard Nestler
发明人： Willi Schmidt , Matthias Geisendorfer , Alexander Weck , Toni Dockner , Holger Herbst , Gerhard Nestler
CPC分类号： C07C67/08
摘要： In a process for the continuous preparation of alkyl esters of (meth)acrylic acid by reacting (meth)acrylic acid with alkanols having from 1 to 8 carbon atoms in a homogeneous, liquid, solvent-free phase at elevated temperature and in the presence of an acid esterification catalyst, in which the (meth)acrylic acid, the alkanol and the acid catalyst are fed to a reaction zone, the water formed is removed by rectification during a residence time as constituent of a mixture comprising starting alkanol in a rectification unit (III) superposed on the reaction zone, the distillate obtained is separated into an organic phase comprising alkanol and an aqueous phase comprising water, the organic phase is essentially completely returned to the rectification unit (III), the reaction mixture is discharged from the reaction zone and conveyed into a distillative separation zone comprising further rectification units and in the latter the alkyl (meth)acrylate formed is separated off.a) (Meth)acrylic acid and alkanol are reacted in a molar ratio of from 1:0.75 to 1:2, b) part of the aqueous phase obtained at the top of the rectification unit (III) is returned to the rectification unit, c) the reaction mixture discharged from the reaction zone is fed to a further rectification unit (I) and in this the reaction mixture is separated into a product (II) comprising the catalyst and a product (I) comprising the alkyl ester of (meth)acrylic acid, remaining alkanol and remaining (meth)acrylic acid, and d) the product (I) is fed to a further rectification unit (II) and in this the alkyl ester of (meth)acrylic acid is separated from the remaining alkanol and from the remaining (meth)acrylic acid and the remaining alkanol and the remaining (meth)acrylic acid are returned to the reaction zone.
摘要翻译： 在（甲基）丙烯酸的烷基酯的连续制备方法中，通过使（甲基）丙烯酸与具有1至8个碳原子的链烷醇在均相，液体，无溶剂相中在升高的温度下和在 将（甲基）丙烯酸，链烷醇和酸催化剂进料到反应区中的酸酯化催化剂，在停留时间内通过精馏除去形成的水，作为在精馏单元中起始烷醇的混合物的组分 （III），将获得的馏出物分离成包含链烷醇和含水的水相的有机相，有机相基本上完全返回到精馏单元（III），将反应混合物从反应物中排出 并输送到包含进一步精馏单元的蒸馏分离区中，后者分离形成的（甲基）丙烯酸烷基酯。 a）（甲基）丙烯酸和链烷醇的摩尔比为1:0.75至1:2，b）将在精馏单元（III）顶部获得的部分水相返回至精馏单元， c）将从反应区排出的反应混合物加入到另一精馏单元（I）中，并将反应混合物分离成包含催化剂的产物（II）和包含（甲基）丙烯酸烷基酯的产物（I） ）丙烯酸，残留的链烷醇和剩余的（甲基）丙烯酸，以及d）将产物（I）加入到另一精馏单元（II）中，在此将（甲基）丙烯酸的烷基酯与剩余的链烷醇 和剩余的（甲基）丙烯酸和剩余的链烷醇和剩余的（甲基）丙烯酸返回到反应区。
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