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公开(公告)号：US4977285A
公开(公告)日：1990-12-11
申请号：US447934
申请日：1989-12-08
IPC分类号： B01J27/24 , C07B61/00 , C07C27/00 , C07C27/28 , C07C29/80 , C07C31/12 , C07C407/00 , C07D301/19 , C07D301/32 , C07D303/04
CPC分类号： C07D301/19 , C07C29/80 , C07C407/003 , C07D301/32
摘要： A heavy distillation fraction comprising tertiary butyl hydroperoxide, tertiary butyl alcohol, impurities and dissolved molybdenum catalyst resulting from the removel of propylene, propylene oxide and tertiary butyl alcohol from an epoxidation reaction product is mixed with about 5 to about 10 wt. %, based on the weight of the heavy liquid distilation fraction, of a lower aliphatic alcohol containing from 1 to 3 carbon atoms to provide a charge mixture, and the charge mixture is:charged to a falling film evaporator and separator therein, under evaporator operating conditions including a temperature within the range of about 20.degree. to about 150.degree. C. and a pressure of about 1 to about 200 mm Hg., into an overhead vaporized fraction comprising substantially all of the aliphatic alcohol and from about 80 to about 95 wt. % of the heavy distillation fraction charged to the falling film evaporator.The practice of the present invention will also provide a clear liquid falling film evaporator residue fraction comprising tertiary butyl hydroperoxide, tertiary butyl alcohol, substantially all of the molybdenum contained in the heavy liquid fraction, and impurities.
摘要翻译： 将来自环氧化反应产物的丙烯，环氧丙烷和叔丁醇的除去产生的叔丁基过氧化氢，叔丁醇，杂质和溶解的钼催化剂的重蒸馏馏分与约5至约10重量％ ％，基于重液体蒸馏馏分的重量，含有1至3个碳原子的低级脂族醇以提供电荷混合物，并且充电混合物：在蒸发器操作下将其装入降膜蒸发器和分离器中 包括温度在约20℃至约150℃范围内的温度和约1至约200mm Hg的压力的塔顶蒸发馏分包含基本上所有脂族醇和约80至约95wt 。 ％的重蒸馏馏分装入降膜蒸发器中。 本发明的实践还将提供包含叔丁基过氧化氢，叔丁醇，重质液体馏分中所含的基本上所有钼以及杂质的透明液体降膜蒸发器残渣馏分。
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公开(公告)号：US4992566A
公开(公告)日：1991-02-12
申请号：US401381
申请日：1989-08-31
IPC分类号： C07D301/14 , B01J23/28 , B01J23/92 , B01J31/22 , B01J38/00 , C07B61/00 , C07C27/28 , C07C29/03 , C07C29/80 , C07C31/12 , C07C407/00 , C07D301/19 , C07D303/04
CPC分类号： C07D301/19 , C07C29/80 , C07C407/003
摘要： Tertiary butyl hydroperoxide and tertiary butyl alcohol are recovered from the reaction product formed by reacting excess propylene with tertiary butyl hydroperoxide in solution in tertiary butyl alcohol in the presence of a soluble molybdenum catalyst, by fractionating the reaction produce to provide distillate propylene, propylene oxide, and tertiary butyl alcohol fractions and a heavy distillation fraction comprising tertiary butyl hydroperoxide, tertiary butyl alcohol and impurities, including dissolved molybdenum catalyst, the tertiary butyl hydroperoxide and tertiary butyl alcohol being recovered from the heavy distillation fraction by vacuum evaporation under evaporation conditions including a temperature of about 25.degree. to about 160.degree. C. and a pressure of about 2 to about 200 mm Hg. in order to provide a lighter condensate fraction comprising about 60 to about 95 wt. % of the heavy distillation fraction and containing from about 70 to about 95 wt. % of tertiary butyl alcohol, about 1 to about 20 wt. % of the tertiary butyl hydroperoxide and from about 15 to about 3 wt. % of impurities and also into a clear liquid heavier residue fraction comprising tertiary butyl alcohol, tertiary butyl hydroperoxide and substantially all of the soluble molybdenum catalyst originally contained in the heavy liquid fraction.
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3.发明授权Treatment of tertiary butyl hydroperoxide distillation fraction to remove acidic contaminants 失效处理叔丁基过氧化氢蒸馏馏分去除酸性污染物
公开(公告)号：US5151530A
公开(公告)日：1992-09-29
申请号：US765610
申请日：1991-09-25
IPC分类号： C07C407/00 , C07C409/04 , C07D301/19 , C07D303/04
CPC分类号： C07D301/19 , C07C407/00 , C07C407/003 , C07C409/04 , C07D303/04
摘要： The distillation product fraction obtained from an isobutane oxidation reaction product after the removal of unreacted isobutane will contain tertiary butyl hydroperoxide, tertiary butyl alcohol and carboxylic acid contaminants such as formic acid, acetic acid and isobutyric acid. It has been discovered that when the distillation product fraction is treated with about 1/2 to 1 equivalents of calcium oxide and/or calcium hydroxide based on the carboxylic acid content of the distillate product fraction, a portion of the carboxylic acid contaminants will precipitate thus partially purifying the distillation product fraction so that, thereafter, molybdenum precipitation will be substantially inhibited when the thus-treated distillation product fraction is used as a feedstock for an epoxidation reaction wherein tertiary butyl hydroperoxide is reacted with an olefin in the presence of a soluble molybdenum catalyst to provide an olefin epoxide and additional tertiary butyl hydroperoxide.
摘要翻译： 在除去未反应的异丁烷之后由异丁烷氧化反应产物得到的蒸馏产物馏分将含有叔丁基过氧化氢，叔丁醇和羧酸污染物如甲酸，乙酸和异丁酸。 已经发现，当蒸馏产物馏分基于馏出物产物级分的羧酸含量用约1/2至1当量的氧化钙和/或氢氧化钙处理时，一部分羧酸污染物将沉淀，因此 部分纯化蒸馏产物部分，使得当将如此处理的蒸馏产物馏分用作环氧化反应的原料时，钼沉淀将基本上被抑制，其中叔丁基过氧化氢在可溶性钼存在下与烯烃反应 催化剂以提供烯烃环氧化物和另外的叔丁基过氧化氢。
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公开(公告)号：US5093506A
公开(公告)日：1992-03-03
申请号：US400901
申请日：1989-08-30
IPC分类号： C07C407/00 , C07C409/04 , C07D301/19 , C07D303/04
CPC分类号： C07D301/19 , C07C407/00 , C07C407/003 , C07C409/04 , C07D303/04
摘要： The distillation product fraction obtained from an isobutane oxidation reaction product after the removal of unreacted isobutane will contain tertiary butyl hydroperoxide, tertiary butyl alcohol and carboxylic acid contaminants such as formic acid, acetic acid and isobutyric acid. It has been discovered that when the distillation product fraction is treated with about 1/2 to 1 equivalents of calcium oxide and/or calcium hydroxide based on the carboxylic acid content of the distillate product fraction, a portion of the carboxylic acid contaminants will precipitate thus partially purifying the distillation product fraction so that, thereafter, molybdenum precipitation will be substantially inhibited when the thus-treated distillation product fraction is used as a feedstock for an epoxidation reaction wherein tertiary butyl hydroperoxide is reacted with an olefin in the presence of a soluble molybdenum catalyst to provide an olefin epoxide and additional tertiary butyl hydroperoxide.
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公开(公告)号：US4810809A
公开(公告)日：1989-03-07
申请号：US945629
申请日：1986-12-23
IPC分类号： C07C29/80 , C07C407/00 , C07D301/19
CPC分类号： C07D301/19 , C07C29/80 , C07C407/003
摘要： It has been discovered in accordance in accordance with the present invention that a tertiary butyl alcohol/ditertiary butyl peroxide azeotrope may be recovered from a product containing tertiary butyl alcohol and ditertiary butyl peroxide by distilling the tertiary butyl alcohol product to obtain an overhead fraction containing substantially all of the ditertiary butyl peroxide/tertiary butyl alcohol azeotrope and other contaminants.It has been further discovered in accordance with the present invention that the ditertiary butyl peroxide can be recovered from the distillate fraction by extraction with ethylene glycol (e.g., in a countercurrent ethylene glycol extraction tower) to provide a ditertiary butyl peroxide product of any desired degree of purity.
摘要翻译： 根据本发明已经发现，通过蒸馏叔丁醇产物可从含有叔丁醇和二叔丁基过氧化物的产物中回收叔丁醇/二叔丁基过氧化物共沸物，得到基本上含有 所有二叔丁基过氧化物/叔丁醇共沸物等杂质。 根据本发明进一步发现，二乙基丁基过氧化物可以通过用乙二醇（例如，在逆流乙二醇萃取塔）中提取从馏出物馏分中回收，以提供任何所需程度的二叔丁基过氧化物产物 的纯度。
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公开(公告)号：US4704482A
公开(公告)日：1987-11-03
申请号：US879660
申请日：1986-06-27
IPC分类号： B01J23/74 , B01J23/86 , C07B61/00 , C07C27/00 , C07C29/132 , C07C29/88 , C07C29/90 , C07C31/12 , C07C67/00
CPC分类号： C07C29/132 , C07C29/88
摘要： Motor-fuel grade tertiary butyl alcohol which is prepared, for example, by reacting propylene with tertiary butyl hydroperoxide to form propylene oxide and a tertiary butyl alcohol reaction product contaminated with residual amounts of tertiary butyl hydroperoxide and ditertiary butyl peroxide can be effectively catalytically treated under mild conversion conditions including a temperature of about 80.degree. to 280.degree. C. with an unsupported catalyst composed of nickel, copper, chromia and iron, or the oxides thereof, or a catalyst containing nickel, copper, chromia and iron which is supported on silica in order to substantially selectively convert the two peroxide contaminants to tertiary butyl alcohol and to thereby provide a treated tertiary butyl alcohol product substantially free from contaminating quantities of such peroxides.
摘要翻译： 通过例如丙烯与叔丁基过氧化氢反应形成环氧丙烷和残留量的叔丁基过氧化氢和二叔丁基过氧化物污染的叔丁醇反应产物，可以有效催化处理汽油燃料级叔丁醇， 包括温度为约80-280℃的温和转化条件与由镍，铜，氧化铬和铁或其氧化物组成的无负载催化剂，或负载在二氧化硅上的含有镍，铜，氧化铬和铁的催化剂 以便基本上选择性地将两种过氧化物污染物转化为叔丁醇，从而提供基本上不含污染量的这种过氧化物的经处理的叔丁醇产物。
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公开(公告)号：US5093509A
公开(公告)日：1992-03-03
申请号：US702523
申请日：1991-05-20
申请人： Robert A. Meyer , Edward T. Marquis
发明人： Robert A. Meyer , Edward T. Marquis
IPC分类号： B01J31/34 , B01J31/40 , B01J38/00 , B01J38/48 , C07B61/00 , C07C27/00 , C07C29/04 , C07C31/12 , C07D301/19 , C07D301/32
CPC分类号： C07D301/19 , B01J31/0202 , B01J31/34 , B01J31/4015 , B01J38/48 , C07D301/32 , B01J21/16 , B01J2231/72 , Y02P20/52 , Y02P20/584
摘要： An epoxidation reaction product formed by the molybdenum catalyzed reaction of propylene with tertiary butyl hydroperoxide to provide propylene oxide and tertiary butyl alcohol is separated by distillation into a propylene fraction, a propylene oxide fraction, a tertiary butyl alcohol fraction and a heavy liquid distillation fraction composed primarily of tertiary butyl hydroperoxide, tertiary butyl alcohol, dissolved molybdenum catalyst, and impurities including lower aliphatic C.sub.1 -C.sub.4 carboxylic acids, and the dissolved molybdenum content of the heavy distillation fraction is adjusted to about 300 to 500 ppm of dissolved molybdenum, if necessary, by treatment with a precipitating agent and contacted with a solid adsorbent consisting essentially of a synthetic, porous, high surface area amorphous magnesium silicate.
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公开(公告)号：US5336790A
公开(公告)日：1994-08-09
申请号：US154321
申请日：1993-11-18
IPC分类号： B01D3/00 , C22B34/34 , C07D301/19 , C07F11/00
CPC分类号： C22B34/345 , Y02P10/23
摘要： A process for recovery of molybdenum from residual fractions derived from an epoxidation reaction of propylene with tertiary butyl hydroperoxide in liquid phase with tertiary butyl alcohol, in the presence of soluble molybdenum, which process comprises:Fractionating epoxidation reaction product for obtaining a liquid fraction containing essentially all molybdenum from the reaction product;Contacting the liquid fraction with anhydrous ammonia for forming a precipitate containing the major portion of the molybdenum and a liquid phase containing 500 ppm or less molybdenum;Separating the liquid phase from the precipitated solid;Evaporating the liquid phase under conditions of elevated temperatures and reduced pressure in the presence of 1 to 3% water for separation into an evaporator overhead vapor essentially free of molybdenum and an evaporator concentrate comprising essentially all of the molybdenum fed to the evaporator;Rapidly cooling evaporator concentrate from about evaporation temperature to about room temperature or less for converting the evaporator concentrate into a brittle, fracturable solid which is easier to accumulate and dispose of in an environmentally acceptable manner.
摘要翻译： 在可溶性钼存在下，从丙烯与叔丁基氢过氧化物在液相中与叔丁基氢过氧化物的环氧化反应的残余馏分回收钼的方法，该方法包括：分馏环氧化反应产物，用于获得基本上含有 来自反应产物的所有钼; 将液体馏分与无水氨接触，形成含钼主要部分的沉淀物和含有500ppm以下钼的液相; 将液相与沉淀固体分离; 在1至3％的水存在下，在升高的温度和减压条件下蒸发液相，以分离成基本上不含钼的蒸发器塔顶蒸气和蒸发器浓缩物，其基本上包含进料到蒸发器的所有钼; 将蒸发器浓缩物从大约蒸发温度快速冷却至约室温或更低，以将蒸发器浓缩物转化成脆性，可破碎的固体，其易于以环境可接受的方式积聚和处理。
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公开(公告)号：US5290527A
公开(公告)日：1994-03-01
申请号：US971741
申请日：1992-11-05
CPC分类号： C22B34/345 , Y02P10/23
摘要： A process for recovery of molybdenum from residual fractions derived from an epoxidation reaction of propylene with tertiary butyl hydroperoxide in liquid phase with tertiary butyl alcohol, in the presence of soluble molybdenum, which process comprises:Fractionating epoxidation reaction product for obtaining a liquid fraction containing essentially all molybdenum from the reaction product;Contacting the liquid fraction with anhydrous ammonia for forming a precipitate containing the major portion of the molybdenum and a liquid phase containing 500 ppm or less molybdenum;Separating the liquid phase from the precipitated solid;Evaporating the liquid phase under conditions of elevated temperatures and reduced pressure in the presence of 1 to 3% water for separation into an evaporator overhead vapor essentially free of molybdenum and an evaporator concentrate comprising essentially all of the molybdenum fed to the evaporator;Rapidly cooling evaporator concentrate from about evaporation temperature to about room temperature or less for converting the evaporator concentrate into a brittle, fracturable solid which is easier to accumulate and dispose of in an environmentally acceptable manner.
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10.发明授权Preparation of mono epoxides and tertiary butyl alcohol using regenerated catalyst 失效使用再生催化剂制备单环氧化物和叔丁基醇
公开(公告)号：US5216182A
公开(公告)日：1993-06-01
申请号：US933936
申请日：1992-08-24
申请人： Edward T. Marquis , Robert A. Meyer
发明人： Edward T. Marquis , Robert A. Meyer
IPC分类号： C07C29/132 , C07D301/19 , C07D303/04 , C07D301/14
CPC分类号： C07D301/19 , C07C29/132 , C07D303/04 , Y02P20/584
摘要： In the preparation of tertiary butyl alcohol and a linear C.sub.3 -C.sub.12 mono epoxide by the epoxidation reaction of a linear C.sub.3 -C.sub.12 alpha mono olefin with tertiary butyl hydroperoxide in solution in tertiary butyl alcohol in the presence of a catalytic amount of a soluble complex of molybdenum with ethylene glycol, a portion of the catalyst that is used is a recycle (final) ethylene glycol solution of a complex of ethylene glycol with ammonium-containing molybdenum compounds prepared from ethylene glycol and a precipitate of solid ammonium-containing molybdenum compounds formed by saturating a heavy distillation fraction with ammonia to thereby form a liquid amination product containing a precipitate of solid ammonium-containing molybdenum compounds; the heavy distillation fraction being obtained by distillation of the epoxidation reaction product.
摘要翻译： 在叔丁醇和直链C 3 -C 12单环氧化物的制备中，通过直链C 3 -C 12α-单烯烃与叔丁基过氧化氢在叔丁醇溶液中的环氧化反应，在催化量的可溶性络合物 钼与乙二醇的一部分，所用催化剂的一部分是乙二醇与由乙二醇制备的含铵钼化合物的复合物的循环（最终）乙二醇溶液和由固体含铵的钼化合物沉淀形成的固体含铵钼化合物 用氨使重馏分饱和，从而形成含有固体含铵钼化合物沉淀物的液体胺化产物; 重蒸馏馏分是通过蒸馏环氧化反应产物获得的。
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