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公开(公告)号：US4891437A
公开(公告)日：1990-01-02
申请号：US133664
申请日：1987-12-16
申请人： Edward T. Marquis , Kenneth P. Keating , John F. Knifton , William A. Smith , John R. Sanderson , Jonathan Lustri
发明人： Edward T. Marquis , Kenneth P. Keating , John F. Knifton , William A. Smith , John R. Sanderson , Jonathan Lustri
IPC分类号： C07D301/19 , C07D303/04
CPC分类号： C07D301/19 , C07D303/04
摘要： A hydroperoxide charge stock (t-butyl hydroperoxide or t-amyl hydroperoxide) is reacted with a C.sub.3 to C.sub.20 olefin charge stock in liquid phase in a reaction zone in the presence of a catalytically effective amount of a soluble molybdenum catalyst to form a product olefin epoxide corresponding to the olefin charge stock and a product alcohol corresponding to the hydroperoxide charge (t-butyl alcohol or t-amyl alcohol), which process is improved in accordance with the present invention by maintaining a reaction medium composed of more than 60 wt % of polar components (hydroperoxide charge stock, product alcohol and product epoxide) in the reaction zone by charging to the reaction zone at least about a 30 wt % solution of the hydroperoxide charge stock in the corresponding product alcohol and charging said olefin charge stock to said reaction zone in an amount relative to the amount of said charged solution of charged hydroperoxide in product alcohol sufficient to provide a ratio of from about 0.5 to about 2 moles of charged olefin per mole of charged hydroperoxide.The preferred olefin charge stock is propylene and the preferred hydroperoxide charge stock is t-butyl hydroperoxide. The corresponding epoxide in this situation is propylene oxide and the corresponding product alcohol is t-butyl alcohol.
摘要翻译： 在催化有效量的可溶性钼催化剂的存在下，将氢过氧化物电荷原料（叔丁基过氧化氢或叔戊基过氧化氢）与液相中的C3至C20烯烃加料原料在反应区中反应以形成产物烯烃 对应于烯烃电荷原料的环氧化物和对应于氢过氧化物电荷的产物醇（叔丁醇或叔戊醇），根据本发明，通过保持由60重量％以上的反应介质组成的反应介质， 的反应区中的极性组分（氢过氧化物电荷原料，产物醇和产物环氧化物）通过向反应区中加入至少约30重量％的氢过氧化物电荷原料在相应产物醇中的溶液，并将所述烯烃电荷原料装入所述 反应区的量相对于产物醇中充入的氢过氧化物的所述带电溶液的量足以提供从ab的比例 每摩尔加入的氢过氧化物中含有0.5至约2摩尔的带电烯烃。 优选的烯烃电荷原料是丙烯，优选的氢过氧化物电荷原料是叔丁基过氧化氢。 在这种情况下相应的环氧化物是环氧丙烷，相应的产物醇是叔丁醇。
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2.发明授权Purification of propylene oxide by treatment with calcium hydroxide in glycerol or sugar water 失效通过用氢氧化钙在甘油或糖水中处理来净化环氧丙烷
公开(公告)号：US4691034A
公开(公告)日：1987-09-01
申请号：US851842
申请日：1986-04-14
IPC分类号： C07D301/32
CPC分类号： C07D301/32
摘要： Methyl formate is removed from propylene oxide by treatment with aqueous calcium hydroxide slurry. Calcium hydroxide solubility is increased by adding a solubilizer selected from the group consisting of sucrose, fructose, maltose, glycerol and mixtures thereof. Methyl formate hydrolysis rate is improved by propylene oxide/water ratio control. Addition of an aldehyde scavenger improves propylene oxide purity.
摘要翻译： 通过用氢氧化钙水溶液处理，从环氧丙烷中除去甲酸甲酯。 通过加入选自蔗糖，果糖，麦芽糖，甘油及其混合物的增溶剂来提高氢氧化钙的溶解度。 通过环氧丙烷/水比控制改善甲酸甲酯的水解速率。 添加醛清除剂可提高环氧丙烷的纯度。
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公开(公告)号：US4650886A
公开(公告)日：1987-03-17
申请号：US804131
申请日：1985-12-06
IPC分类号： B01J31/18 , B01J31/22 , C07D301/19 , C07F11/00
CPC分类号： C07D301/19 , B01J31/2208 , B01J31/2226 , B01J2231/72 , B01J2531/64
摘要： Storage stable solutions of molybdenum/alkanol complexes in the alkanol are prepared by reacting an ammonium molybdate with an amount of a straight chain or branched chain C.sub.6 -C.sub.13 alkanol, within the range of about 7 to about 20 moles of alkanol per gram atom of molybdenum sufficient to form a storage stable molybdenum/alkanol complex. The complex-forming reaction is initiated in the presence of about 1 to about 4 moles of added water per gram atom of molybdenum and is conducted at a temperature of about 120.degree. to about 190.degree. C. for a period of time, normally about 3 to about 8 hours, sufficient to substantially completely remove ammonia and water to provide a liquid reaction product comprising said solution of molybdenum/alkanol complex dissolved in unreacted alkanol and containing about 0.001 to about 0.1 wt. % of water. The reaction product is filtered to provide a clarified storage stable solution of the molybdenum/alkanol complex.
摘要翻译： 通过使钼酸铵与一定量的直链或支链C 6 -C 13烷醇在约7至约20摩尔的链烷醇/克原子钼的范围内反应来制备钼/烷醇配合物在烷醇中的储存稳定溶液 足以形成储存稳定的钼/烷醇络合物。 络合物形成反应在每克原子钼约1至约4摩尔加入水存在下开始，并在约120℃至约190℃的温度下进行一段时间，通常约3 至约8小时，足以基本上完全除去氨和水，以提供液体反应产物，其包含溶解在未反应的链烷醇中的钼/烷醇络合物溶液，并含有约0.001至约0.1wt。 ％的水。 将反应产物过滤以提供钼/烷醇复合物的澄清储存稳定溶液。
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4.发明授权Purification of propylene oxide by treatment with a selected base and inert salt 失效通过用选择的碱和惰性盐处理来纯化环氧丙烷
公开(公告)号：US4691035A
公开(公告)日：1987-09-01
申请号：US851846
申请日：1986-04-14
IPC分类号： C07D301/32
CPC分类号： C07D301/32
摘要： Methyl formate is removed from propylene oxide by treatment with a selected base such as sodium hydroxide in water and glycerol. Selected inert salts may be added. The rate of methyl formate hydrolysis by selected bases was increased to commercially acceptable levels by addition of the glycerol. The glycerol and inert salts reduced the amount of residual water in the propylene oxide.
摘要翻译： 通过用选择的碱如氢氧化钠在水和甘油中处理，从环氧丙烷中除去甲酸甲酯。 可以加入选择的惰性盐。 通过加入甘油将选择的碱的甲酸甲酯水解速率提高到商业上可接受的水平。 甘油和惰性盐减少环氧丙烷中残留水的量。
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公开(公告)号：US4654427A
公开(公告)日：1987-03-31
申请号：US804132
申请日：1985-12-06
IPC分类号： B01J31/22 , C07D301/19 , C07F11/00
CPC分类号： C07D301/19 , B01J31/2208 , B01J31/2226 , B01J2231/72 , B01J2531/64
摘要： Storage stable solutions of molybdenum/alkanol complexes in the alkanol are prepared by reacting a molybdenum oxide and ammonium hydroxide and an amount of a straight chain or branched chain C.sub.6 -C.sub.13 alkanol, within the range of about 10 to about 55 moles of alkanol per gram atom of molybdenum sufficient to form a storage stable molybdenum/alkanol complex. The complex-forming reaction is initiated in the presence of about 1 to about 4 moles of water per gram atom of molybdenum and about 0.5 to about 10 moles of ammonia per gram atom of molybdenum, the water and ammonia preferably being added in the form of concentrated ammonium hydroxide. The reaction is conducted at a temperature of about 120.degree. to about 190.degree. C. for a period of time, normally about 3 to about 8 hours, sufficient to substantially completely remove ammonia and water to provide a liquid reaction product comprising said solution of molybdenum/alkanol complex dissolved in unreacted alkanol and containing about 0.001 to about 0.1 wt. % of water. The reaction product is filtered to provide a clarified storage stable solution of the molybdenum/alkanol complex having a dissolved molybdenum content of about 3 to about 10.5 wt. %.
摘要翻译： 钼/烷醇配合物在烷醇中的储存稳定溶液是通过使氧化钼和氢氧化铵与一定量的直链或支链C 6 -C 13烷醇在约10-约55摩尔的链烷醇/克 足以形成储存稳定的钼/烷醇络合物的钼原子。 在约1至约4摩尔水/克原子钼和约0.5至约10摩尔氨/克原子钼的存在下引发络合物形成反应，优选以水和氨的形式加入水和氨 浓氢氧化铵。 反应在约120℃至约190℃的温度下进行一段时间，通常约3至约8小时，足以基本上完全除去氨和水，以提供包含所述钼溶液的液体反应产物 /链烷醇络合物溶解在未反应的链烷醇中并含有约0.001至约0.1wt。 ％的水。 将反应产物过滤以提供溶解的钼含量为约3至约10.5重量％的钼/烷醇络合物的澄清储存稳定溶液。 ％。
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公开(公告)号：US5107067A
公开(公告)日：1992-04-21
申请号：US351512
申请日：1989-05-12
IPC分类号： B01J31/22 , C07D301/19
CPC分类号： C07D301/19 , B01J31/2213 , B01J31/2286 , B01J2231/72 , B01J2531/64 , B01J2531/96
摘要： Complexes made by reacting an ammonium-containing molybdenum compound with an alkylene glycol in the presence of water at an elevated temperature are described. Mild stripping of the water subsequent to complex formation is preferred. If some of the water is left in the complex, it may serve as an excellent olefin epoxidation catalyst. The ratio of moles of alkylene glycol to gram atoms of molybdenum in the complex forming reaction ranges from 7:1 to 20:1. Ethylene glycol and propylene glycol are the particularly preferred alkylene glycols.
摘要翻译： 描述了在升高的温度下在水存在下使含铵的钼化合物与亚烷基二醇反应制得的络合物。 复合物形成后水的轻度汽提是优选的。 如果一些水留在络合物中，它可以用作优异的烯烃环氧化催化剂。 在络合物形成反应中，亚烷基二醇与钼的克原子摩尔数的比例为7:1至20:1。 亚乙基二醇和丙二醇是特别优选的亚烷基二醇。
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7.发明授权Synthesis of molybdenum/alkylene glycol complexes useful as epoxidation catalysts 失效用作环氧化催化剂的钼/亚烷基二醇配合物的合成
公开(公告)号：US4626596A
公开(公告)日：1986-12-02
申请号：US687701
申请日：1984-12-31
IPC分类号： C07F11/00 , B01J31/22 , C07D301/19
CPC分类号： C07D301/19 , B01J31/2208 , B01J31/2226 , B01J2231/72 , B01J2531/64
摘要： Complexes made by reacting an ammonium-containing molybdenum compound with an alkylene glycol in the presence of water at an elevated temperature are described. Mild stripping of the water subsequent to complex formation is preferred. If some of the water is left in the complex, it may serve as an excellent olefin epoxidation catalyst. The ratio of moles of alkylene glycol to gram atoms of molybdenum in the complex forming reaction ranges from 7:1 to 20:1. Ethylene glycol and propylene glycol are the particularly preferred alkylene glycols.
摘要翻译： 描述了在升高的温度下在水存在下使含铵的钼化合物与亚烷基二醇反应制得的络合物。 复合物形成后水的轻度汽提是优选的。 如果一些水留在络合物中，它可以用作优异的烯烃环氧化催化剂。 在络合物形成反应中，亚烷基二醇与钼的克原子摩尔数的比例为7:1至20:1。 亚乙基二醇和丙二醇是特别优选的亚烷基二醇。
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公开(公告)号：US4742179A
公开(公告)日：1988-05-03
申请号：US926159
申请日：1986-11-03
IPC分类号： C10L1/182 , B01J23/86 , B01J23/88 , C07C27/00 , C07C29/132 , C07C29/88 , C07C31/12 , C07C67/00 , C07C27/26
CPC分类号： C07C29/88
摘要： Motor-fuel grade tertiary butyl alcohol contaminated with residual amounts of tertiary butyl hydroperoxide and ditertiary butyl peroxide (which is prepared, for example, by reacting propylene with tertiary butyl hydroperoxide to form propylene oxide and a motor fuel grade tertiary butyl alcohol reaction product) can be effectively catalytically treated under mild conversion conditions including a temperature of about 80.degree. to 180.degree. C. with a base-treated hydrogenation catalyst from groups VIB or VIIIB of the Periodic Table 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.
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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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公开(公告)号：US4939281A
公开(公告)日：1990-07-03
申请号：US368009
申请日：1989-06-19
CPC分类号： C07D301/19 , B01J31/0201 , B01J31/34 , B01J31/4015 , B01J38/48 , C01B35/127 , C01G39/02 , B01J21/02 , B01J2231/72 , B01J31/26 , Y02P20/584 , Y10S210/912
摘要： A process for substantially completely removing a minor amount of molybdenum dissolved in a substantially anhydrous organic solution, such as a heavy distillation fraction resulting from the removal of unreacted propylene, propylene oxide and tertiary butyl alcohol from an epoxidation reaction mixture:wherein from about 1 to about 10 wt. % of an aqueous solution of sodium meta borate containing from about 1 to about 10 wt. % of dissolved sodium meta borate is added to an organic solution containing dissolved molybdenum catalyst in an amount sufficient to provide a molar excess of sodium meta borate, based on the gram atoms of dissolved molybdenum in said organic solution, to provide a mixture,wherein the mixture is maintained at a temperature ranging from about ambient temperature up to about 100.degree. C. at a pressure of about 0 to about 1,000 psig. for about 0.5 to about 5 hours, sufficient to precipitate at least about 95 mol % of the soluble molybdenum from the mixture, andwherein the mixture is filtered to obtain a filtrate containing not more than about 100 ppm of molybdenum.
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