公开(公告)号：US3950371A

公开(公告)日：1976-04-13

申请号：US458684

申请日：1974-04-08

申请人： Lutz Jeromin ,  Norbert Bremus ,  Georg Friederici ,  Peter Peiffer

发明人： Lutz Jeromin ,  Norbert Bremus ,  Georg Friederici ,  Peter Peiffer

IPC分类号： C07C51/42 ,  B01D9/02 ,  C07C29/74 ,  C07C67/48 ,  C11B7/00 ,  C11C1/08 ,  B01D9/00 ,  C11B3/00

CPC分类号： C11B7/0091

摘要： A method for separating fatty substance mixtures into components of different melting points by the "Rewetting or Hydrophilization Process," with the heat removal necessary for cooling and crystallizing higher melting fatty substance fractions being obtained essentially by vacuum evaporation of an aqueous, non-surface-active electrolyte solution in direct contact with the fatty substance mixture.THE PRIOR ARTThe separation of fatty acid mixtures or of fatty acid ester mixtures into components of different melting points by a wetting agent process is known from U.S. Pat. No. 2,800,493, July 23, 1957, Stein et al. This process has become known as the "Rewetting or Hydrophilization Process." According to this patent, a mixture of solid and oily fatty substance particles is transformed by means of a wetting agent solution, optionally containing non-surface-active electrolyte, into a dispersion of separate solid and oily fatty substance particles. This dispersion is separated by means of solid jacket centrifuges into an oily phase and an aqueous phase containing the solid fatty substance particles in dispersion. The heat removal necessary for the crystallization of the solid fatty substance particles is obtained by cooling devices, in particular scraping condensers. After termination of the separating process, the recovered wetting agent solution is recycled. German Pat. No. 1,010,062, or U.S. Pat. No. 2,972,636, Stein et al, describes a corresponding process for the separation of fatty alcohols.The essential disadvantages of the above mentioned processes are the high investment and operating costs for cooling equipment and cooling devices. In particular the required scraping condensers are costly and require continual servicing.From U.S. Pat. No. 3,541,122 a method is further known for the separation of mixtures of fat-like materials into fractions of different melting points, which is also carried out by the rewetting process. Here, however, the cooling of the molten fatty substance mixture required for crystallization is obtained by vacuum evaporation of water. After completion dispersion of the fatty substance mixture consisting of liquid and solid particles in a wetting agent solution, the crystallized solid phase is separated by filtration, and the oily dispersion passes through the filter. In this procedure the separation of the oily fraction and the solid particles is not complete, so that the latter have a relatively high iodine number and hence a comparatively poor quality.Published German Patent Application (DOS) No. 1,915,298, discloses a method of separating fatty acid, fatty alcohol, or fatty acid ester mixtures into components of different melting points by mixing the molten mixture with an aqueous wetting agent solution. The crystallization of the solid fractions to be separated is obtained by evaporating a part of the aqueous wetting agent solution under reduced pressure. Because the fatty substances used can be degased only with difficulty and incompletely on being fed into the crystallizer vessel, intense foaming takes place upon addition of the wetting agent solution, whereby the progress of the process is greatly disturbed. Moreover, the wetting agent hinders crystal growth, which in turn leads to difficulties in the further separation of oily and solid phase.OBJECTS OF THE INVENTIONIt is an object of the present invention, in carrying out the rewetting process to avoid the high investment costs for the installation and servicing of refrigeration equipment and cooling devices, in particular scraping condensers, and, furthermore, to improve the effectiveness of the separation method and hence to improve the quality of the products obtained.It is another object of the present invention to provide a method of separating fatty substance mixtures into components of different melting points by the rewetting process, with the heat removal necessary for cooling and crystallizing higher melting fatty substance fractions being obtained essentially by vacuum evaporation of an aqueous, non-surface-active electrolyte solution in direct contact with the fatty substance mixture.These and further objects of the present invention will become apparent as the description thereof proceeds.DESCRIPTION OF THE INVENTIONThe present invention relates to a method of separating fatty substance mixtures into components of different melting points.Generally speaking, the present invention concerns a method of separating fatty substance mixtures into components of different melting points by the rewetting process, with the heat removal necessary for cooling and crystallizing higher melting fatty substance fractions being obtained essentially by vacuum evaporation of an aqueous, non-surface-active electrolyte solution in direct contact with the fatty substance mixture.More particularly, the present invention provides a method of separating fatty substance mixtures into components of different melting points by the rewetting process, where the heat removal required for the cooling and crystallization of higher melting fatty substance fractions is obtained by vacuum evaporation of an aqueous phase in direct contact with the fatty substance mixture, characterized by the following steps:a. partial or complete melting of the fatty substance mixture;b. addition of an aqueous non-surface-active electrolyte solution to the molten fatty substance mixture and evaporation of a part of the water of the electrolyte solution by means of a vacuum simultaneously with intensive mixing to produce partial or complete crystallization of the higher melting fraction;c. addition of wetting agent solution with dispersing of the liquid and solid fatty substance therein, preferably while maintaining the vacuum and continuing the water evaporation until the separation temperature is reached;d. separation of the dispersion by means of centrifuge into an oily phase containing the lower melting fatty substance fractions, and an aqueous phase containing the crystallized fatty substance fractions in dispersed form;e. separation of the higher melting fatty substance fractions from the aqueous phase by filtration or by melting and subsequent separation of oily from aqueous phase by centrifuging or allowing to settle.The present invention is preferrably directed to an improvement in the method for the separation of mixtures of fatty substances into components of different melting points by the rewetting process which comprises the steps of (a) at least partial melting of a fatty substance mixture, (b) cooling and crystallizing said fatty substance mixture into a mixture of liquid and solid particles, (c) dispersing said mixture of liquid and solid particles in an aqueous wetting agent solution containing electrolyte at a temperature whereby a dispersion of liquid and solid fatty substance is obtained, (d) separation said dispersion into a lighter phase consisting substantially of the liquid, lower-melting fatty substance fractions and a heavier phase consisting substantially of solid, higher-melting fatty substance fractions dispersed in said aqueous wetting agent solution, (e) separating the solid higher-melting fatty substance fractions from said aqueous wetting agent solution, and (f) recovering said separated fatty components of different melting points; the improvement which comprises in step (b) adding an aqueous non-surface-active electrolyte solution to said at least partially melted fatty substance mixture and cooling to substantially the separation temperature by evaporation under vacuum of a part of the water of said aqueous electrolyte solution with simultaneously intensely mixing said at least partially melted fatty substance mixture and said aqueous electrolyte solution.In addition the invention comprises the further improvement of optionally adding a part or all of the said aqueous wetting agent solution while maintaining the vacuum and continuing the water evaporation until the desired separation temperature is reached.In a preferred embodiment of the process, the aqueous electrolyte containing wetting agent solution is recycled entirely or partially.The method is suitable for the separation of a variety of fatty substance mixtures; in particular, mixtures of fatty acids, fatty acid esters or fatty alcohols can be separated when the melting points of the components to be separated are sufficiently far apart.Of particular technical importance is the separation of fatty acid mixtures into technical olein and technical stearin (oleic and stearic acids), or of fatty alcohol mixtures into oleyl alcohol and stearyl alcohol. Correspondingly, solid mixtures of fatty acid triglycerides can be separated at room temperature into lower and higher melting fractions. Such fatty acid triglyceride fractions are used for the production of edible fats. It is not necessary that one of the components to be separated is present as a liquid oil at room temperature. The method can also be successfully utilized when both fractions are solid at room temperature and merely differ sufficiently in their melting points.The process of the present invention is carried out in the following manner:a. The fatty substance mixture to be separated is wholly or partially melted in a suitable heatable vessel, for example, in a melting device equipped with a stirrer, so that the temperature of the mixture is above the anticipated separation temperature. Alternatively the procedure may be to precool a fully molten mixture in a conventional manner, for example, in a heat exchanger, so that a partial elimination of the fatty fraction to be separated has already occurred. It is generally desirable for technical reasons to avoid a partial crystallization in this stage and to select the temperature somewhat above the starting crystallization temperature.b. The further cooling of the partially or completely molten fatty substance mixture is achieved by vacuum evaporation cooling. The process may be conducted by batches or continuously. The vaporizable liquid utilized is preferably an aqueous non-surface-active electrolyte solution. Preferably this is a makeup solution where a continuous process is employed with a discharge of part of the cycling aqueous solution. This solution is brought into contact with the fatty substance mixture under vacuum and is simultaneously mixed intensively. This mixture is maintained under reduced pressure with continual evacuation of the water vapor formed until a viscous crystal paste has been formed, by crystallization of solid fatty substance from the fatty substance mixture which can hardly be handled by the mixer. The temperature reached at this point is termed the temperature limit of incipient crystallization. At this stage the evaporation of water is greatly hindered due to insufficient mixing, so that the cooling rate decreases considerably and continuation of the process would become uneconomical.When working by batches, the pressure in the mixing vessel is reduced by means of a suitable evacuating system. Above the liquid, the vapor pressure of water adjusts itself to the respective temperature so that the cooling takes place without temperature discontinuities in the metastable range of crystallization along the vapor pressure curve of water. In this temperature range spontaneous seed formation is largely avoided; and relatively large crystals are formed which are capable of good separation from the oily phase.The addition of electrolyte solution occurs either intermittently or continuously after evacuation of the vessel. The electrolyte solution may be introduced below the surface of the fatty substance mixture, possibly in finely divided form, whereby intensive mixing takes place simultaneously.For continuous operation it is preferred to work with a cascade vessel equipped with a stirrer. The fatty substance mixture and electrolyte solution are fed into the first stirrer equipped vessel of the cascade apparatus and then pumped from one stage to the next. In the downstream flow direction of the product stream, the pressure and hence the temperature decreases by discontinuous steps from vessel to vessel according to the vapor pressure of the water. The temperature steps must be made very small, and hence the number of mixing vessels of the cascade apparatus must be made so large that the continuous process will come as close as possible to the "ideal crystallization" along the vapor pressure curve of water, attainable in batch operation. This is because in the batch process the crystallization occurs in the metastable range and spontaneous seed formation is avoided.The quantity of heat to be removed by evaporation depends on the heat capacity of the batch, upon the desired temperature decrease, and upon the heat of crystallization obtained. The amount of electrolyte solution added to the fatty substance mixture in partially to completely molten form is such that the necessary temperature reduction is obtained and that upon reaching the temperature limit of incipient crystallization a just barely stirrable and pumpable crystal plate is present. As a rule, however, as much electrolyte solution is added as water and wetting agent solution is removed during the cycle. The quantity of wetting agent solution to be eliminated from the cycle depends largely on the purity of the fatty substances and is necessary for the removal of slime and dirt substances from the process, which would influence the crystallization and, if not removed, would cause progressively higher iodine numbers in the components of the fatty substances that are solid at the separation temperature.The temperature of the electrolyte solution when added should be approximately equal to that of the fatty substance mixture batch.The aqueous non-surface-active electrolyte solution used in the process contains about 0.1% to 10% by weight, preferably from 0.5% to 2% by weight of a water-soluble salt for example a chloride, sulfate or nitrate of a mono-di- or tri-valent metal, such as a salt of an alkali metal, an alkaline earth metal, or an earth metal. Salts such as sodium sulfate, magnesium sulfate or aluminum sulfate have proved particularly successful as agents in forming the electrolyte solution. The total quantity of electrolyte to be added depends upon the proportion of electrolyte containing wetting agent solution removed from the cycle at the end of the separating process.c. After the desired temperature has been reached, the vacuum may be broken; and the quantity of wetting agent solution necessary for dispersing the liquid and solid fatty substance is added. With intense mixing the rewetting process begins. The oily fractions of the fatty substance mixture are displaced from the surfaces of the crystallized or solid fractions.In a preferred embodiment of the process, a portion of the wetting agent solution is introduced before the desired separation temperature is reached. This is done appropriately as soon as the temperature limit of incipient crystallization is reached; and the addition of wetting agent causes the crystal paste to liquefy again. The vacuum is then maintained, such that the process of evaporation and cooling can now proceed until the anticipated separation temperature is reached. At the same time the rewetting process takes place, and a highly fluid dispersion is formed which contains both the oily as well as the crystallized fatty substance fractions as separate particles in dispersion.The wetting agent solution utilized is essentially the so-called "old diluted" wetting agnt solution recycled from the process. If necessary, fresh wetting agent is added to the "old diluted" solution as replacement for the wetting agent fraction lost in separation or discharged. Difficulties due to foaming do not occur even when operating according to the preferred process embodiment; that is when the wetting agent solution is introduced into the vessel while still under vacuum. This is preferably done by feeding in (flashing in) above the liquid surface, due to which extensive degasing and removal of the dissolved air, occurs before the mixture of fatty substance and electrolyte solution is stirred in. The fatty substances used are degased anyway by the preceding vacuum evaporation cooling. The water vapor evolved during the continued evaporation cooling forms relatively closely below the surface of the liquid; and the distance it travels while rising is very short, so that no foaming occurs.To obtain a separable dispersion, the proportion of aqueous phase at the end of the evaporation cooling step should be from 0.3 to 5 times, preferably from 0.7 to 3 times, the fatty substance mixture charged. The losses due to discharging a part of the wetting agent solution, the so-called "old diluted" solution, from the process cycle are replaced expediently after the vacuum has been broken by a corresponding amount of electrolyte solution for incipient crystallization and of fresh wetting agent.Examples of wetting agents include anionic or non-ionic water-soluble compounds, which lower the surface tension of the aqueous solution and thus bring about a displacement of the oily components of the starting mixture from the surface of the crystallized or solid fractions. The surface-active compounds disclosed in U.S. Pat. No. 2,800,493 can be used as wetting agents in particular, compounds with alkyl radicals having 8 to 18 carbon atoms, preferably 10 to 16 carbon atoms in the molecule. Examples of suitable anionic surface-active compounds include soaps; sulfonates such as alkylbenzene sulfonates having 8 to 18 carbon atoms in the alkyl, and alkyl sulfonates having 8 to 18 carbon atoms; sulfates such as fatty alcohol sulfates having 8 to 18 carbon atoms, sulfatized reaction products of fatty alcohols having 8 to 18 carbon atoms, adducted with 1 to 10, preferably 2 to 5 mols of ethylene oxide and/or propylene oxide, and fatty acid monoglyceride sulfates having 8 to 18 carbon atoms in the fatty acid moiety, etc. These anionic surface-active compounds are used in the form of their alkali metal salts, preferably as the sodium salt, but other suitable salts include the potassium salt, ammonium salt, the mono-, di- or tri-lower alkanolamine salts such as the triethanolamine salt. Examples of non-ionic surface-active compounds include the water-soluble products of addition of ethylene oxide and/or propylene oxide to alkyl phenols having 8 to 18 carbon atoms in the alkyl or to fatty alcohols having 8 to 18 carbon atoms. The fatty substance dispersion should contain from 0.05 to 2, preferably 0.1 to 1, parts by weight of wetting agent per 100 parts by weight of solution. This amount of wetting agent includes not only the amount of wetting agent dissolved in the aqueous phase, but also that dissolved in the oil or adsorbed on the surface of the solid fractions.d. After completion of the cooling and breaking of the vacuum, the dispersion of the fatty substance fractions is separated by means of centrifuges, such as full jacket centrifuges or separators, into an oily phase containing the lower melting fatty substance fractions, and into an aqueous phase containing the crystallized or solid fatty substance fractions in dispersed form. For this process various centrifuge types are suitable, for example tube centrifuges, dish centrifuges or scoop tube centrifuges. Especially preferred are the latter type, in which the phases are removed from the centrifuge by scoop tubes.After passing through the centrifuge, the oily fatty substance fractions are recovered, possibly after having been washed and dried. If necessary, another separation step may be employed at a lower temperature, such that an oil of correspondingly lower cloud point will be obtained.e. The suspension of crystallized fatty substance fractions issuing from the centrifuge is separated by heating the suspension. The crystallized fatty substance fractions melt, and subsequently centrifuging or settling takes place, for example in settling tanks. Another possibility is to filter the crystallized fatty substance fractions. After passing through the separating process once, the higher melting fraction of the fatty substance mixture thus obtained has a very high purity.The recovered wetting agent solution is recycled as socalled "old dilution." From 30% to 90% by weight is recovered and recycled, and preferably from 60% to 90%, and especially 70%, is recovered and recycled. It is, however, necessary to remove a part of this solution from the cycle continuously to avoid the accumulation of slime impurities or non-fatty substance organic impurities from the fatty substances charged, which could impair the crystallization and also the quality of the higher melting fatty substance fraction. The resulting loss of wetting agent solution must be compensated by adding fresh wetting agent solution. The simultaneously occurring electrolyte loss is replaced by the electrolyte solution supplied during evaporation cooling, and in particular, during incipient crystallization. Further the process must be controlled so that the losses of water occurring during evaporation cooling, or due to removal of wetting agent solution, are compensated by the electrolyte solution or fresh wetting agent solution supplied. Some discussion of these procedures is to be found in U.S. Pat. No. 3,737,444, June 5, 1973, Hartmann et al.The procedure according to the invention has special advantages over the known process. On the one hand, operating in the metastable range of crystallization and in the presence of electrolyte solution brings about the formation of particularly large crystals which permit a very neat separation of the oily fatty substance fraction. Compared with the method described in U.S. Pat. No. 3,541,122 (incipient crystallization in water) and with the mode of operation set forth in German Offenlegungsschrift No. 1,915,298 (incipient crystallization in wetting agent solution), it is possible to obtain a purer and hence more valuable, crystallized fatty substance by utilizing the new process involving incipient crystallization in the presence of electrolyte solution. For example it is possible to obtain from tallow fatty acids, a purer and more valuable, crystallized fatty substance, stearin or technical stearic acid. At the same time, the yield of the oily fatty substance phase, the olein or technical oleic acid, is thereby increased.On the other hand, the foaming problems occurring in the known process of evaporation cooling in the presence of wetting agents are avoided, since in the presence of electrolyte solution, a complete degasing of the fatty substance mixture readily takes place during the evaporation cooling. A special pretreatment of the fatty substance mixture or, respectively, a preceding additional separative process step is thus unnecessary with the continuous mode of operation. On the other hand, the process of the invention is particularly favorable also from the aspect of instrumentation, inasmuch as special cooling devices, such as refrigeration machines, scraping condensers and the like, become superfluous. Naturally, however, a combination of the conventional cooling method with the described new method is conceivable, but as a rule such combinations are not important because they lack economic efficiency.The following examples are merely illustrative of the present invention without being deemed limitative in any manner thereof.

公开(公告)号：US6127561A

公开(公告)日：2000-10-03

申请号：US990004

申请日：1997-12-12

申请人： Lutz Jeromin ,  Guenter Wozny ,  Pu Li

发明人： Lutz Jeromin ,  Guenter Wozny ,  Pu Li

IPC分类号： C07C67/03 ,  C07C51/00

CPC分类号： C07C67/03

摘要： The invention discloses a process for the production of monoglycerides by glycerolysis of methyl ester derived from animal or vegetable fat and oils which includes mixing a surplus of 0.1 to 3 moles of glycerols in relation to methyl ester, subjecting the reaction mixture to a reaction temperature between 130 to 160 at a vacuum of 200 to 400 mbar, adding of alkaline catalysts, stopping the reaction by fast cooling of the reaction mixture and the destruction of the alkaline catalyst when the quantity of glycerides has reached a concentration of mono and diglyceride of 40 to 60%, leaving the catalyst in the reaction mixture to catalyse the reaction downstream in a reactor, separating the surplus methyl ester and glycerol by distillation and stopping the reaction by fast cooling of the reaction mixture with reactor and the destruction of the alkaline catalyst when the quantity of glycerides has reached a concentration of 40 to 60% and the ratio of concentrations of mono and diglyceride lies between 3 to 10.

摘要翻译： 本发明公开了一种通过从动植物脂肪和油衍生的甲酯的甘油分解来生产甘油单体的方法，其包括将相当于甲酯的过量混合0.1至3摩尔甘油，使反应混合物与 在200至400毫巴的真空下加入130至160，加入碱性催化剂，通过快速冷却反应混合物停止反应，并且当甘油酯的量达到单酸甘油酯和甘油二酯的浓度为40至 60％，将催化剂留在反应混合物中以在反应器中催化下游的反应，通过蒸馏分离剩余的甲酯和甘油，并通过与反应器快速冷却反应混合物并停止反应，并且当 甘油酯的用量达到40〜60％，甘油单酯和甘油二酯的浓度比例 在3到10之间。

公开(公告)号：US5710350A

公开(公告)日：1998-01-20

申请号：US522387

申请日：1995-09-25

申请人： Lutz Jeromin ,  Bernhard Gutsche ,  Reinhard Bunte ,  Volkmar Jordan

发明人： Lutz Jeromin ,  Bernhard Gutsche ,  Reinhard Bunte ,  Volkmar Jordan

IPC分类号： B01J23/02 ,  C07C41/09 ,  C07C41/42 ,  C07C43/13 ,  C07C31/18

CPC分类号： C07C41/42 ,  C07C41/09

摘要： A process for preparing diglycerol in high concentrations and high yields by partially reacting glycerol in the presence of an alkaline catalyst to form a reaction mixture containing from 10 to 15% by weight of diglycerol and separating the unreacted glycerol from the reaction mixture in a wiped film or short path first distillation zone at a reduced pressure of 0.5 to 5 mbar and distilling a bottoms product from the first distillation zone in a second distillation zone which is a short path distillation zone at a pressure of 0.05 to 0.3 mbar to obtain a second bottom product containing at least 90% by weight diglycerol. Diglycerol of higher purity can be obtained by recovering diglycerol as a distillate from a third distillation zone.

摘要翻译： PCT No.PCT / EP94 / 00834 Sec。 371 1995年9月25日第 102（e）日期1995年9月25日PCT 1994年3月16日PCT公布。 出版物WO94 / 21582 日期1994年9月29日一种通过在碱性催化剂存在下使甘油部分反应制备高浓度和高收率的双甘油的方法，以形成含有10至15重量％的双甘油并将未反应的甘油与反应物分离的反应混合物 混合物在0.5至5毫巴的减压下的擦拭膜或短路第一蒸馏区中，并在第二蒸馏区中在第二蒸馏区中蒸馏塔底产物，所述第二蒸馏区是0.05至0.3毫巴的压力下的短路蒸馏区 以获得含有至少90重量％的二甘油的第二底部产物。 通过从第三蒸馏区回收作为馏出物的二甘油，可以获得更高纯度的二甘油。

公开(公告)号：US5514820A

公开(公告)日：1996-05-07

申请号：US191746

申请日：1994-02-03

申请人： Georg Assmann ,  Gerhard Blasey ,  Bernhard Gutsche ,  Lutz Jeromin ,  Jean Rigal ,  Rene Armengaud ,  Bernard Cormary

发明人： Georg Assmann ,  Gerhard Blasey ,  Bernhard Gutsche ,  Lutz Jeromin ,  Jean Rigal ,  Rene Armengaud ,  Bernard Cormary

IPC分类号： B01J19/24 ,  C07C67/03 ,  C11C3/04

CPC分类号： B01J19/242 ,  C07C67/03 ,  B01J2219/00103 ,  B01J2219/00166 ,  B01J2219/00168 ,  B01J2219/00171

摘要： The invention relates to a continuous process for the production of lower alkyl esters at temperatures of up to 100.degree. C. and under pressures of up to 10 bar by reaction of fatty acid triglycerides containing less than 1% free fatty acid with a lower alcohol in two stages in the presence of a homogeneous alkaline catalyst, the glycerol formed being removed after the first stage. To enable the process to be carried out with high yields and with lower maintenance, investment and energy costs than in the prior art, the reaction mixture is passed through a reactor and a following static separator only once in each stage, tube reactors are used as the reactors and the Reynolds number of the flow of the reaction mixture is greater than 2,300.

摘要翻译： 本发明涉及用于在高达100℃的温度和高达10巴的压力下生产低级烷基酯的连续方法，其通过使含有少于1％游离脂肪酸的脂肪酸甘油三酯与低级醇的反应 在均相碱性催化剂存在的两个阶段，形成的甘油在第一阶段后被除去。 为了使该方法能够以比现有技术高的产率和较低的维护，投资和能量成本进行，反应混合物在每个阶段仅通过反应器和静态分离器仅一次，管式反应器用作 反应器和反应混合物流的雷诺数大于2,300。

公开(公告)号：US5416239A

公开(公告)日：1995-05-16

申请号：US167926

申请日：1994-02-17

申请人： Alfred Westfechtel ,  Christoph Breucker ,  Bernhard Gutsche ,  Lutz Jeromin ,  Horst Eierdanz ,  Horst Baumann ,  Karl-Heinz Schmid ,  Werner Nonnenkamp

发明人： Alfred Westfechtel ,  Christoph Breucker ,  Bernhard Gutsche ,  Lutz Jeromin ,  Horst Eierdanz ,  Horst Baumann ,  Karl-Heinz Schmid ,  Werner Nonnenkamp

IPC分类号： C07C45/48 ,  C07C45/54 ,  C07C49/04 ,  C07C49/203 ,  C07C45/45

CPC分类号： C07C45/54

摘要： A process for the production of fatty ketones by pyrolysis of fatty acid magnesium salts wherein fatty acids corresponding to formula (I):R.sup.1 COOH (I)in which R.sup.1 CO is an aliphatic acyl radical containing 12 to 22 carbon atoms and 0, 1, 2 or 3 double bonds, are heated to temperatures of 320.degree. to 360.degree. C. in the presence of magnesium oxide and the fatty ketones formed are distilled off from the reaction mixture under reduced pressure.

摘要翻译： PCT No.PCT / EP92 / 01373。 371日期1994年2月17日 102（e）日期1994年2月17日PCT提交1992年6月17日PCT公布。 出版物WO93 / 0032020 日本1993年1月7日。一种通过热解脂肪酸镁盐生产脂肪酮的方法，其中相应于式（I）的脂肪酸：其中R1CO是含有12-22个碳原子的脂族酰基的R1COOH（Ⅰ） 和0,1,2或3个双键在氧化镁存在下加热至320℃至360℃的温度，并且在减压下从反应混合物中蒸出形成的脂肪酮。

公开(公告)号：US4698186A

公开(公告)日：1987-10-06

申请号：US821109

申请日：1986-01-21

申请人： Lutz Jeromin ,  Eberhard Peukert ,  Gerhard Wollmann

发明人： Lutz Jeromin ,  Eberhard Peukert ,  Gerhard Wollmann

IPC分类号： C11B3/02 ,  C11C3/04 ,  C11C3/10

CPC分类号： C07C67/03 ,  C07C67/08 ,  C11B3/02

摘要： A process for reducing the free fatty acid content of fats and oils by esterifying the free fatty acids with a lower monoalcohol in the presence of an acidic cation exchange resin as a solid esterification catalyst.

摘要翻译： 一种通过在酸性阳离子交换树脂作为固体酯化催化剂存在下，通过用较低一元醇酯化游离脂肪酸来降低脂肪和油的游离脂肪酸含量的方法。

公开(公告)号：US4647678A

公开(公告)日：1987-03-03

申请号：US813444

申请日：1985-12-26

申请人： Klemens Eckwert ,  Lutz Jeromin ,  Alfred Meffert ,  Eberhard Peukert ,  Bernhard Gutsche

发明人： Klemens Eckwert ,  Lutz Jeromin ,  Alfred Meffert ,  Eberhard Peukert ,  Bernhard Gutsche

IPC分类号： C07D301/16 ,  C07D301/14 ,  C07D303/04 ,  C07D303/14 ,  C07D303/42

CPC分类号： C07D303/42 ,  C07D301/14 ,  C07D303/04 ,  C07D303/14 ,  B01J2219/0004

摘要： The epoxidation of terminally and/or internally olefinically unsaturated hydrocarbon compounds which are liquid at 50.degree. to 100.degree. C. and at atmospheric pressure (oil phase), in which the oil phase is treated with an acid phase containing acetic acid, hydrogen peroxide and peracetic acid in aqueous solution, after which the aqueous acid phase is separated from the oil phase, the peracetic acid in the aqueous acid phase is regenerated and the regenerated aqueous acid phase is returned to the epoxidation reactor. Epoxidation is carried out using an aqueous acid phase containing at most about 10% by weight of peracetic acid, and the peracetic acid content in the aqueous acid phase is reduced by at most about 50%, based on the peracetic acid content of the aqueous acid phase used, after a single passage through the epoxidation stage. After separation from the oil phase, the aqueous acid phase preferably is cooled before regeneration.

摘要翻译： 末端和/或内部烯属不饱和烃化合物的环氧化，其在50℃至100℃和大气压（油相）下为液体，其中油相用含有乙酸，过氧化氢和 过乙酸在水溶液中，然后从油相中分离含水酸相，酸性水相中的过乙酸再生，再生的含水酸相返回到环氧化反应器。 使用含有至多约10重量％过乙酸的含水酸相进行环氧化，基于酸水溶液的过乙酸含量，酸性水相中的过乙酸含量减少至多约50％ 在单次通过环氧化阶段后使用。 从油相分离后，酸性水相优选在再生前冷却。

公开(公告)号：US06958369B2

公开(公告)日：2005-10-25

申请号：US09403557

申请日：1998-11-16

申请人： Werner Berger ,  Lutz Jeromin ,  Uta Mierau ,  Guntram Opitz

发明人： Werner Berger ,  Lutz Jeromin ,  Uta Mierau ,  Guntram Opitz

IPC分类号： C08G77/442 ,  C08L3/02 ,  C08L3/00 ,  C08L89/00

CPC分类号： C08G77/442 ,  C08L3/02 ,  C08L2666/02

摘要： The invention relates to a component for producing thermoplastically moldable, biodegradable and bright polymer mixtures based on starch, with good dimensional stability in water. The dimensional stability in water and the biodegradability of said component are adjustable and the component can be used for producing sheet materials, semi-finished or finished products, for example for packagings, containers, articles required in horticultural nurseries, and for other purposes. The invention, furthermore, relates to a process for producing the component from polyvinyl acetate and alkali silicate. A suspension of polyvinyl acetate is hydrolized and saponified in the batch process in the presence of catalytic additions such as, in particular glycerol, by adding the alkali silicate and hydroxides at high temperatures. Organosilicates of high homogeneity and fineness are formed. Additions of said component in small amounts have a positive effect on the phase compatibility of the hydrophilic starch and a hydrophobic polymer such as polyvinyl acetate in the course of preparation of the blend in the extruder. The properties of the extruded products are substantially enhanced.

摘要翻译： 本发明涉及一种用于生产基于淀粉的热塑性可模塑，可生物降解和光亮的聚合物混合物的组分，在水中具有良好的尺寸稳定性。 水中的尺寸稳定性和所述组分的生物降解性是可调节的，并且该组分可用于生产片材，半成品或成品，例如用于园艺苗圃所需的包装，容器，制品以及用于其它目的。 此外，本发明涉及一种由聚乙酸乙烯酯和碱金属硅酸盐制备组分的方法。 聚乙酸乙烯酯的悬浮液通过在高温下加入碱金属硅酸盐和氢氧化物，在催化添加物，特别是甘油的存在下，在分批方法中进行水解和皂化。 形成高均匀度和细度的有机硅酸盐。 在挤出机中制备共混物的过程中，少量添加所述组分对亲水性淀粉和疏水性聚合物如聚乙酸乙烯酯的相容性具有积极的影响。 挤出产品的性能显着提高。

公开(公告)号：US5840786A

公开(公告)日：1998-11-24

申请号：US902509

申请日：1997-07-29

申请人： Michael Beck ,  Lutz Jeromin ,  Christiane Hoeltgen ,  Wolfgang Ritter

发明人： Michael Beck ,  Lutz Jeromin ,  Christiane Hoeltgen ,  Wolfgang Ritter

IPC分类号： C08F257/02 ,  C08F285/00 ,  C09J151/00 ,  C08L83/00

CPC分类号： C09J151/003 ,  C08F257/02 ,  C08F285/00

摘要： The invention relates to a plastisol composition based on bead polymers. The bead polymers preferably have a core/shell structure and an average diameter of 1 to 150 .mu.m. The bead polymers are preferably chlorine-free and are made up at least of a) styrene, .alpha.-methyl styrene and/or p-methyl styrene on the one hand and b) 2 to 20% by weight (based on the copolymer) of olefinically unsaturated carboxylic acids. The plastisol composition according to the invention may be used for the production of coating compositions, sealing compounds and adhesives.

摘要翻译： 本发明涉及基于珠聚合物的增塑溶胶组合物。 珠粒聚合物优选具有核/壳结构，平均直径为1-150μm。 珠粒聚合物优选为无氯的，并且一方面由至少a）苯乙烯，α-甲基苯乙烯和/或对甲基苯乙烯制成，b）2-20重量％（基于共聚物）的 烯属不饱和羧酸。 根据本发明的增塑溶胶组合物可用于制备涂料组合物，密封剂和粘合剂。

公开(公告)号：US5427687A

公开(公告)日：1995-06-27

申请号：US960459

申请日：1992-12-15

申请人： Stephan Blum ,  Bernhard Gutsche ,  Lutz Jeromin ,  Levent Yueksel

发明人： Stephan Blum ,  Bernhard Gutsche ,  Lutz Jeromin ,  Levent Yueksel

IPC分类号： B01D53/22 ,  B01D53/26 ,  B01J19/24 ,  C07C67/08 ,  C07C67/48 ,  C07C69/14 ,  C07C69/24 ,  B01D61/36

CPC分类号： B01D53/268 ,  B01D53/22 ,  B01J19/245 ,  B01J19/2465 ,  B01J19/2475 ,  C07C67/08 ,  B01J2219/00108 ,  B01J2219/00126

摘要： Process for carrying out an equilibrium reaction in which one or more products are separated off by vapor permeation comprising the steps of:A) forming a reaction mixture comprising the reactants to be reacted in at least one reaction zone at a reaction temperature and reaction pressure selected so as to provide a reaction temperature above the boiling temperature of at least the product or products to be removed, wherein at least the product or products to be removed enters the resulting vapor phase in vapor form;B) passing the vapor phase containing the product or products to be removed to a zone remote from the reaction zone, which remote zone contains a semi-permeable membrane permeable to the product or products to be removed;C) carrying out vapor permeation in said remote zone to remove at least a portion of the product or products to be removed from said vapor phase; andD) returning the resulting vapor retentate from step C) to a reaction zone in step A). The process is especially useful in carrying out esterification reaction between a carboxylic acid and an alcohol.

摘要翻译： PCT No.PCT / EP91 / 01050 Sec。 371日期：1992年12月15日 102（e）1992年12月15日PCT PCT 1991年6月6日PCT公布。 公开号WO91 / 19559 1991年12月26日。用于进行平衡反应的方法，其中一种或多种产物通过蒸汽渗透分离，包括以下步骤：A）形成包含在至少一个反应区中反应的反应物的反应混合物 选择反应温度和反应压力以提供高于至少要除去的产物或沸点的沸点温度的反应温度，其中至少要被除去的产物或产物进入蒸气形式的所得气相; B）将含有待除去的产品或产品的气相通过到远离反应区的区域，该远程区域包含可渗透待除去的产品的半透膜; C）在所述远程区域中进行蒸气渗透以去除要从所述气相中除去的产物或产物的至少一部分; 和D）在步骤A）中将得到的蒸气滞留物从步骤C）返回到反应区。 该方法在羧酸和醇之间的酯化反应中特别有用。