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1.发明申请METHOD FOR CONCENTRATING AQUEOUS 3-HYDROXY-2,2-DIMETHYLPROPANAL SOLUTION 有权浓缩水性3-羟基-2,2-二甲基丙烯酸溶液的方法公开(公告)号：US20130334028A1
公开(公告)日：2013-12-19
申请号：US14002442
申请日：2012-03-02
IPC分类号： C07C45/84
CPC分类号： C07C45/84 , C07D319/06 , C07C47/19
摘要： The present invention provides a method for concentrating an aqueous solution containing at least 3-hydroxy-2,2-dimethyl propanal and/or a dimer thereof, which includes subjecting a mixed solution of an aqueous solution containing at least 3-hydroxy-2,2-dimethyl propanal and/or a dimer thereof and an azeotropic agent to azeotropic distillation in a distillation column to distil off water and the azeotropic agent from the mixed solution, wherein the mixed solution is prepared by adding, as the azeotropic agent, at least one selected from the group consisting of 1-butanol, 2-butanol, 2-methyl-1-propanol, 1-pentanol and 1-hexanol to the aqueous solution.
摘要翻译： 本发明提供一种浓缩含有至少3-羟基-2,2-二甲基丙醛和/或其二聚体的水溶液的方法，其包括将含至少3-羟基-2,2-二甲基丙醛和/ 2-二甲基丙醛和/或其二聚体和共沸剂在蒸馏塔中共沸蒸馏以从混合溶液中蒸馏出水和共沸剂，其中混合溶液通过作为共沸剂至少加入至少 一种选自1-丁醇，2-丁醇，2-甲基-1-丙醇，1-戊醇和1-己醇的水溶液。
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2.发明授权公开(公告)号：US09061985B2
公开(公告)日：2015-06-23
申请号：US14002442
申请日：2012-03-02
IPC分类号： C07C45/84 , C07D319/06
CPC分类号： C07C45/84 , C07D319/06 , C07C47/19
摘要： The present invention provides a method for concentrating an aqueous solution containing at least 3-hydroxy-2,2-dimethyl propanal and/or a dimer thereof, which includes subjecting a mixed solution of an aqueous solution containing at least 3-hydroxy-2,2-dimethyl propanal and/or a dimer thereof and an azeotropic agent to azeotropic distillation in a distillation column to distil off water and the azeotropic agent from the mixed solution, wherein the mixed solution is prepared by adding, as the azeotropic agent, at least one selected from the group consisting of 1-butanol, 2-butanol, 2-methyl-1-propanol, 1-pentanol and 1-hexanol to the aqueous solution.
摘要翻译： 本发明提供一种浓缩含有至少3-羟基-2,2-二甲基丙醛和/或其二聚体的水溶液的方法，其包括将含至少3-羟基-2,2-二甲基丙醛和/ 2-二甲基丙醛和/或其二聚体和共沸剂在蒸馏塔中共沸蒸馏以从混合溶液中蒸馏出水和共沸剂，其中混合溶液通过作为共沸剂至少加入至少 一种选自1-丁醇，2-丁醇，2-甲基-1-丙醇，1-戊醇和1-己醇的水溶液。
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3.发明授权Process for production of flake-like dried 2-(5-ethyl-5-hydroxymethyl-1,3-dioxan-2-yl)-2-methylpropan-1-ol 有权制备片状干燥的2-（5-乙基-5-羟甲基-1,3-二恶烷-2-基）-2-甲基丙-1-醇的方法公开(公告)号：US07915431B2
公开(公告)日：2011-03-29
申请号：US12445782
申请日：2007-10-10
IPC分类号： C07D319/06
CPC分类号： C07D319/06
摘要： A method for producing flake-like dried DOG by making DOG containing from 10 to 50% by mass of a liquid go through a continuous melt-drying step of a specified condition and then making it go through, as a next step, a vacuum-drying step of a specified condition or a ventilation-drying step of a specified condition while holding a molten state thereof, to obtain DOG in which the liquid in DOG is reduced to not more than 0.5% by mass (dried DOG), and flaking the obtained dried DOG in a flake production step.
摘要翻译： 通过使含有10〜50质量％的液体的DOG通过规定条件的连续熔融干燥工序，然后使其通过真空 - 干燥DOG，从而生产片状干燥DOG的方法， 干燥步骤，在保持其熔融状态的同时进行规定条件的通风干燥工序，得到DOG中的液体减少为0.5质量％以下的DOG（干燥DOG），剥离 在片状生产步骤中获得干燥的DOG。
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公开(公告)号：US20070191646A1
公开(公告)日：2007-08-16
申请号：US11641104
申请日：2006-12-19
申请人： Ikutaro Kuzuhara , Atsushi Iwamoto
发明人： Ikutaro Kuzuhara , Atsushi Iwamoto
IPC分类号： C07C41/01
CPC分类号： C07C41/01 , C07C41/40 , C07C43/132
摘要： In the method of producing ditrimethylolpropane of the present invention, the distillation still residue obtained in the production of trimethylolpropane is subjected to crystallizing treatment while strictly regulating the amount of organic solvent to be used, the crystallization temperature and the crystallization time within the specific ranges. With the method of the present invention, a highly pure di-TMP is obtained only by a single operation of the crystallization.
摘要翻译： 在本发明的二羟甲基丙烷的制造方法中，在严格调节所使用的有机溶剂的使用量，结晶温度和结晶时间在特定范围内的同时，对三羟甲基丙烷的制造中得到的蒸馏釜残渣进行结晶处理。 利用本发明的方法，仅通过单次结晶操作获得高纯度的二 - TMP。
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公开(公告)号：US20050261506A1
公开(公告)日：2005-11-24
申请号：US11130122
申请日：2005-05-17
IPC分类号： C07D493/10 , C07C323/02
CPC分类号： C07D493/10
摘要： In the production of spiroglycol by the reaction of pentaerythritol and hydroxypivalaldehyde in water in the presence of an acid catalyst, (A) a total content of amines and amine salts in hydroxypivalaldehyde is reduced to 1.5% by weight or lower; (B) seed crystals are added to the reaction system before initiating the reaction and/or during the reaction in an amount from 1.5 to 30% by weight on the basis of the total feed amount of pentaerythritol, hydroxypivalaldehyde, water, the acid catalyst and the seed crystals, each being fed into the reaction system; (C) the pH of the reaction system is kept from 0.1 to 4.0 from initiation of the reaction to completion of the reaction; and (D) the sum of a maximum theoretical amount of spiroglycol to be synthesized from pentaerythritol and hydroxypivalaldehyde to be fed into the reaction system and an amount of spiroglycol contained in the seed crystals to be added to the reaction system is controlled within a range from 5 to 35% by weight on the basis of the total feed amount. The spiroglycol produced has an increased particle size. By washing the spiroglycol with a basic solution, the heat stability is improved.
摘要翻译： 在酸催化剂存在下，季戊四醇与羟基新戊醛在水中的反应生产中，（A）羟基新戊醛中胺和胺盐的总含量降低至1.5重量％以下; （B）基于季戊四醇，羟基新戊醛，水，酸催化剂的总进料量和基于季铵盐的总进料量，在开始反应和/或反应期间将晶种加入到反应体系中的量为1.5至30重量％ 种子晶体，各自被送入反应体系; （C）反应体系的pH从反应开始至反应完全为止保持在0.1〜4.0; 和（D）将从进料到反应体系中的季戊四醇和羟基新戊醛合成的螺旋体的最大理论量的总和和加入到反应体系中的晶种中所含的螺旋体的量控制在 基于总进料量5至35重量％。 所生产的螺旋体具有增加的粒度。 通过用碱性溶液洗涤螺旋藻，热稳定性得到改善。
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公开(公告)号：US20070078271A1
公开(公告)日：2007-04-05
申请号：US11542274
申请日：2006-10-04
IPC分类号： C07D319/06
CPC分类号： C07D319/06
摘要： A process of producing 2-(5-ethyl-5-hydroxymethyl-1,3-dioxane-2-yl)-2-methylpropane-1-ol (DOG) by the acetalization of hydroxypivalaldehyde with trimethylolpropane in water in the presence of an acid catalyst and optional seed crystals. DOG crystals having an increased particle size and containing the trans isomer in a high content are produced by the process in which the reaction temperature, pH of the reaction system and concentration of DOG to be produced in the reaction system are controlled.
摘要翻译： 通过羟丙甲醛与三羟甲基丙烷在水中的缩醛化反应生产2-（5-乙基-5-羟甲基-1,3-二恶烷-2-基）-2-甲基丙烷-1-醇（DOG）的方法， 酸催化剂和任选的晶种。 通过反应温度，反应体系pH和反应体系中产生的DOG浓度的控制方法，可以制得具有较高含量的反式异构体的具有高含量的反式异构体的DOG晶体。
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公开(公告)号：US20070078270A1
公开(公告)日：2007-04-05
申请号：US11541531
申请日：2006-10-03
申请人： Ikutaro Kuzuhara , Yutaka Nakamura
发明人： Ikutaro Kuzuhara , Yutaka Nakamura
IPC分类号： C07D319/06
CPC分类号： C07D319/06
摘要： A production method of 2-(5-ethyl-5-hydroxymethyl-1,3-dioxane-2-yl)-2-methylpropane-1-ol (DOG) which includes a step of acetalizing hydroxypivalaldehyde with trimethylolpropane in a solvent in the presence of an acid catalyst. After the acetalization, the reaction product liquid is neutralized and then heated to dissolve the deposited DOG crystals. Then, the reaction product liquid is cooled to recrystallize DOG. DOG produced in such manner has an adequately large particle size. Therefore, DOG is easy to handle and involves little danger of dust explosion.
摘要翻译： 2-（5-乙基-5-羟甲基-1,3-二恶烷-2-基）-2-甲基丙烷-1-醇（DOG）的制备方法，其包括将羟基新戊醛与三羟甲基丙烷缩合在溶剂中的步骤 存在酸催化剂。 缩醛化后，反应产物液体被中和，然后加热以溶解沉积的DOG晶体。 然后，将反应产物液冷却至重结晶DOG。 以这种方式生产的DOG具有足够大的粒度。 因此，DOG易于处理，并且几乎不会有粉尘爆炸的危险。
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8.发明申请PROCESS FOR PRODUCTION OF FLAKE-LIKE DRIED 2-(5-ETHYL-5-HYDROXYMETHYL-1,3-DIOXAN-2-YL)-2-METHYLPROPAN-1-OL 有权2-（5-乙基-5-羟基甲基-1,3-二氧戊环-2-基）-2-甲基丙-2-醇的类似松香类干燥方法公开(公告)号：US20100317878A1
公开(公告)日：2010-12-16
申请号：US12445782
申请日：2007-10-10
IPC分类号： C07D319/06
CPC分类号： C07D319/06
摘要： A method for producing flake-like dried DOG by making DOG containing from 10 to 50% by mass of a liquid go through a continuous melt-drying step of a specified condition and then making it go through, as a next step, a vacuum-drying step of a specified condition or a ventilation-drying step of a specified condition while holding a molten state thereof, to obtain DOG in which the liquid in DOG is reduced to not more than 0.5% by mass (dried DOG), and flaking the obtained dried DOG in a flake production step.
摘要翻译： 通过使含有10〜50质量％的液体的DOG通过规定条件的连续熔融干燥工序，然后使其通过真空 - 干燥DOG，从而生产片状干燥DOG的方法， 干燥步骤，在保持其熔融状态的同时进行规定条件的通风干燥工序，得到DOG中的液体减少为0.5质量％以下的DOG（干燥DOG），剥离 在片状生产步骤中获得干燥的DOG。
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公开(公告)号：US06835852B2
公开(公告)日：2004-12-28
申请号：US10657155
申请日：2003-09-09
申请人： Shinichi Nagao , Ikutaro Kuzuhara , Hiroshi Ogawa
发明人： Shinichi Nagao , Ikutaro Kuzuhara , Hiroshi Ogawa
IPC分类号： C07C5116
CPC分类号： C07C51/265 , C07C29/48 , C07C29/50 , C07C45/36 , C07C51/235 , C07C51/44 , Y02P20/582 , C07C47/542 , C07C63/307 , C07C63/04 , C07C33/20 , C07C33/26
摘要： A process for producing trimellitic acid which comprises step A for oxidizing pseudocumene, thereby obtaining a reaction mixture comprising dimethyl benzoic acid, dimethyl benzyl alcohol, and dimethyl benzaldehyde, step B for separating dimethyl benzoic acid, dimethyl benzyl alcohol and dimethyl benzaldehyde from the reaction mixture obtained in step A, step C for oxidizing dimethyl benzyl alcohol separated in step B, thereby obtaining dimethyl benzoic acid and dimethyl benzyl aldehyde and then feeding dimethyl benzoic acid and dimethyl benzyl aldehyde thus obtained to step B, and step D for oxidizing dimethyl benzoic acid and/or dimethyl benzaldehyde separated in step B, thereby obtaining trimellitic acid.
摘要翻译： 一种制备偏苯三酸的方法，其包括用于氧化假枯烯的步骤A，从而得到包含二甲基苯甲酸，二甲基苄醇和二甲基苯甲醛的反应混合物，步骤B从反应混合物中分离二甲基苯甲酸，二甲基苄醇和二甲基苯甲醛 在步骤A步骤C中获得的用于氧化步骤B中分离的二甲基苄醇的步骤C，从而得到二甲基苯甲酸和二甲基苄基醛，然后将如此获得的二甲基苯甲酸和二甲基苄基酯加到步骤B中，步骤D用于氧化二甲基苯甲酸 和/或在步骤B中分离的二甲基苯甲醛，从而得到偏苯三酸。
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公开(公告)号：US09169184B2
公开(公告)日：2015-10-27
申请号：US13820586
申请日：2011-09-05
摘要： The present invention provides a method for producing ditrimethylolpropane which is characterized by the following (1) and (2): (1) a distillation still residue separated from purified trimethylolpropane is subjected to re-distillation under specific conditions to obtain a ditrimethylolpropane-containing solution having given contents of bis-TMP and tri-TMP; and (2) when subjecting the ditrimethylolpropane-containing solution to crystallization with an organic solvent, the crystallization is initiated under pressure at a temperature exceeding a boiling point of the organic solvent as measured under normal pressures, and the resulting crystallization product solution is cooled at a temperature drop rate of 2° C./min or less. According to the above method, it is possible to produce a high-purity ditrimethylolpropane from a distillation still residue obtained upon production of trimethylolpropane in a simple, industrially useful manner.
摘要翻译： 本发明提供一种二羟甲基丙烷的制造方法，其特征在于以下（1）和（2）：（1）在纯化的三羟甲基丙烷中分离出的蒸馏残余物在特定条件下进行再蒸馏，得到含二羟甲基丙烷的溶液 给出了双TMP和三TMP的内容; 和（2）当使含二羟丙基丙烷的溶液用有机溶剂结晶时，在常压下测量的超过有机溶剂沸点的温度下，在压力下开始结晶，并将所得结晶产物溶液冷却至 降温速度为2℃/分钟以下。 根据上述方法，可以以简单的工业上有用的方式从由三羟甲基丙烷制备得到的蒸馏釜残渣中制备高纯度的二羟甲基丙烷。
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