公开(公告)号：US4550213A

公开(公告)日：1985-10-29

申请号：US625942

申请日：1984-06-29

Applicant: Hubert H. Thigpen ,  Richard J. Clos

Inventor： Hubert H. Thigpen ,  Richard J. Clos

IPC: C07C45/85 ,  C08G2/08 ,  C08G2/28 ,  C07C47/02

CPC classification number: C08G2/28 ,  C07C45/85 ,  C08G2/08

Abstract: An improvement for manufacturing paraformaldehyde prills from an aqueous solution of formaldehyde which comprises polymerizing the formaldehyde in the presence of a catalyst of sodium hydroxide in a concentration of from about 0.5 to about 5 ppm, aging the resulting mixture at about 100.degree. to about 130.degree. C. for about 10 to about 60 minutes, spraying the aged mixture into a prilling tower at from about 100.degree. to about 130.degree. C., collecting the prills in a fluidized bed at the base of the tower at from about 45.degree. to about 60.degree. C., removing the prills to a separate vessel where the prills further polymerize and dry at from about 15.degree. to about 30.degree. C. for about 3 to about 5 hours while operating the vessel in a plugged flow manner, and collecting the resulting prills.

Abstract translation: 从甲醛水溶液制备多聚甲醛颗粒的改进，其包括在约0.5至约5ppm的浓度的氢氧化钠催化剂存在下聚合甲醛，将所得混合物老化至约100至约130℃ 约10至约60分钟，在约100至约130℃下将老化的混合物喷洒到造粒塔中，将塔板的塔底的流化床中的颗粒在约45°至约 60℃下，将颗粒物除去分离的容器，其中颗粒进一步聚合并在约15至约30℃下干燥约3至约5小时，同时以堵塞流动的方式操作容器，并收集 造成了颗粒。

公开(公告)号：US5876570A

公开(公告)日：1999-03-02

申请号：US612599

申请日：1996-01-18

Applicant: Hubert H. Thigpen

Inventor： Hubert H. Thigpen

IPC: B01D3/32 ,  B01D3/36 ,  C07B63/00 ,  C07D317/12 ,  B01D3/34

CPC classification number: C07D317/12 ,  B01D3/322 ,  B01D3/36

Abstract: A purification process for cyclic formals, in which water is efficiently removed from a crude cyclic formal, namely, a mixture of a cyclic formal and water which is difficult to be separated from the mixture, thereby obtaining a cyclic formal of high purity which contains only a very small amount of water.The purification process for cyclic formals is characterized by the steps of supplying a mixture of a cyclic formal and water into a distillation tower, effecting distillation while supplying a hydrophilic solvent (A) having a boiling point from 180.degree. to 250.degree. C. into the distillation tower at a position higher than the supply position of the mixture, and taking out a purified cyclic formal as a distillate.

Abstract translation: 循环甲醛的纯化方法，其中水从粗制环状醛中有效地除去，即难以与混合物分离的环状缩甲醛和水的混合物，从而获得仅含有的纯度的环状缩甲醛 非常少量的水。 循环形式的纯化方法的特征在于将循环甲醛和水的混合物供应到蒸馏塔中，在沸点为180-250℃的亲水性溶剂（A）中进行蒸馏，同时进行蒸馏 蒸馏塔在高于混合物供应位置的位置，并取出纯化的环状缩甲醛作为馏出物。

公开(公告)号：US4289912A

公开(公告)日：1981-09-15

申请号：US146945

申请日：1980-05-02

Applicant: Marvin E. Harris, Jr. ,  Hubert H. Thigpen

Inventor： Marvin E. Harris, Jr. ,  Hubert H. Thigpen

IPC: C07C45/86 ,  C07C47/058 ,  C08G2/08 ,  C07C47/04

CPC classification number: C08G2/08 ,  C07C45/86

Abstract: The tendency of liquid paraformaldehyde containing water and paraformaldehyde in, for example, approximately 80% to approximately 90% concentration to precipitate solid paraformaldehyde therefrom is retarded by the incorporation thereinto of an effective amount of a moderator or stabilizer selected from the group consisting of polyacrylic acid, tartaric acid, dl-malic acid, ethylenediaminetetraacetic acid, and citric acid. The prior-art stabilizers known and used for lower-concentration formaldehyde solutions of, for example, about 50% strength are not effective. Conversely, the present moderators are not effective in the lower-concentration solutions.

Abstract translation: 含有水和多聚甲醛的液体多聚甲醛的倾向，例如约80％至约90％的浓度从而沉淀出固体多聚甲醛，这通过加入有效量的选自聚丙烯酸 ，酒石酸，dl-苹果酸，乙二胺四乙酸和柠檬酸。 已知和用于例如约50％强度的较低浓度甲醛溶液的现有技术的稳定剂是无效的。 相反，目前的主持人在低浓度溶液中无效。

公开(公告)号：US5690793A

公开(公告)日：1997-11-25

申请号：US509793

申请日：1995-08-01

Applicant: Hubert H. Thigpen

Inventor： Hubert H. Thigpen

IPC: C07D319/06 ,  B01D3/32 ,  B01D3/40 ,  C07B63/00 ,  C07D317/12 ,  B01D3/34

CPC classification number: C07D317/12 ,  B01D3/322 ,  B01D3/40

Abstract: A purification process for cyclic formals, in which water is efficiently removed from a crude cyclic formal, namely, a mixture of a cyclic formal and water which is difficult to be separated from the mixture, thereby obtaining a cyclic formal of high purity which contains only extremely small amounts of water and impurities. The purification process for cyclic formals is characterized by the steps of supplying a mixture of a cyclic formal and water into a distillation tower, effecting distillation while supplying a hydrophilic solver (A) having a boiling point from 180.degree. to 250.degree. C. and a purified cyclic formal (X) containing not more than 200 ppm of water into the distillation tower at positions higher than the supply position of the mixture and higher than the supply position of the hydrophilic solvent (A), respectively, and taking out a purified cyclic formal from the top of the tower as a distillate.

Abstract translation: 循环甲醛的纯化方法，其中水从粗制环状醛中有效地除去，即难以与混合物分离的环状缩甲醛和水的混合物，从而获得仅含有的纯度的环状缩甲醛 极少量的水和杂质。 循环形式的纯化方法的特征在于将环状缩甲醛和水的混合物供应到蒸馏塔中，在沸腾温度为180-250℃的同时供给蒸馏，同时进行蒸馏 在高于混合物的供给位置且高于亲水性溶剂（A）的供给位置的位置处，在蒸馏塔中含有不超过200ppm的水的纯化的环状缩聚物（X），并且分离出纯化的环状 正式从塔顶作为馏出物。

公开(公告)号：US5616736A

公开(公告)日：1997-04-01

申请号：US191689

申请日：1994-02-04

Applicant: Hubert H. Thigpen

Inventor： Hubert H. Thigpen

IPC: C07D319/06 ,  C07D317/12 ,  C07D317/10

CPC classification number: C07D317/12

Abstract: A method of preparing cyclic formals which contain only small amounts of by-product impurities and unreacted starting materials, and which are ready to be purified.In preparing a cyclic formal by reacting alkylene glycol with formaldehyde in the presence of a catalyst, a reaction vessel provided with a vapor-liquid contact zone at the upper part thereof is used. Vapor generated from the reaction mixture and containing a cyclic formal goes up and passes through the vapor-liquid contact zone to be condensed. While part of the condensate is returned to the vapor-liquid contact zone, the remainder of the condensate is taken out as a distillate.

Abstract translation: 制备仅含有少量副产物杂质和未反应原料的循环甲缩醛的方法，其准备被纯化。 在催化剂存在下，通过使亚烷基二醇与甲醛反应来制备环状缩甲醛时，使用在其上部设置有气液接触区的反应容器。 由反应混合物产生并含有环状甲醛的蒸气上升并通过气液接触区域进行冷凝。 当冷凝物的一部分返回到气 - 液接触区时，剩余的冷凝物作为馏出物取出。

公开(公告)号：US5456805A

公开(公告)日：1995-10-10

申请号：US185606

申请日：1994-01-21

Applicant: Hubert H. Thigpen

Inventor： Hubert H. Thigpen

IPC: C07D319/06 ,  B01D3/32 ,  C07D317/12 ,  B01D3/36 ,  C07C13/02

CPC classification number: B01D3/322 ,  C07D317/12

Abstract: A purification process for cyclic formals, in which water is efficiently removed from a mixture of a cyclic formal and water which is difficult to be separated from the mixture, thereby obtaining a cyclic formal of high purity which contains only an extremely small amount of water.The purification process for cyclic formals is characterized by the steps of supplying a mixture of a cyclic formal and water into a distillation tower, effecting distillation while supplying n-pentane into the distillation tower and taking out a purified cyclic formal as a bottom liquid.

Abstract translation: 循环甲醛的纯化方法，其中有效地从环状缩水甘油与水的混合物中除去难以与混合物分离的水，从而获得仅含极少量水的高纯度环状缩甲醛。 循环形式的纯化方法的特征在于将环状缩甲醛和水的混合物供应到蒸馏塔中，在将正戊烷供应到蒸馏塔中并进行纯化的环状缩甲醛作为底部液体时进行蒸馏。

公开(公告)号：US3957873A

公开(公告)日：1976-05-18

申请号：US183648

申请日：1971-09-24

Applicant: Hubert H. Thigpen ,  Wallace E. Taylor ,  Arthur W. Schnizer

Inventor： Hubert H. Thigpen ,  Wallace E. Taylor ,  Arthur W. Schnizer

IPC: C07C291/04 ,  C07C87/29 ,  C07C87/54

CPC classification number: C07C291/04

Abstract: An improved process for oxidizing an amine to the corresponding amine oxide with peracetic acid comprises carrying out the reaction in a distillation column, using as oxidant the gaseous mixture of peracetic acid and acetaldehyde resulting from the vapor-phase oxidation of acetaldehyde with oxygen. The amine is introduced in liquid form into the upper portion of the distillation column while the gaseous mixture of peracetic acid and acetaldehyde is simultaneously introduced into an intermediate location in the column. Reaction takes place within the column, with acetic acid and acetaldehyde being withdrawn as vapor from the top while a liquid comprising the amine oxide product is recovered from the base.

公开(公告)号：US5695615A

公开(公告)日：1997-12-09

申请号：US510047

申请日：1995-08-01

Applicant: Hubert H. Thigpen

Inventor： Hubert H. Thigpen

IPC: B01D3/32 ,  B01D3/40 ,  C07B63/00 ,  C07D317/12 ,  B01D3/34

CPC classification number: B01D3/40 ,  B01D3/322 ,  C07D317/12

Abstract: A purification process for cyclic formals, in which water is efficiently removed from a crude cyclic formal, namely, a mixture of a cyclic formal and water which is difficult to be separated from the mixture, thereby obtaining a cyclic formal of high purity which contains only a very small amount of water. The purification process for cyclic formals is characterized by the following two purification steps: (1) Supplying a mixture of a cyclic formal and water into a distillation tower at a supply position, and effecting distillation while supplying a hydrophilic solvent (A) having a boiling point from 180.degree. to 250.degree. C. at a position higher than the supply position of the mixture to take out a cyclic formal (X) containing 100 to 5000 ppm of water as a distillate, and (2) Distilling the cyclic formal (X) obtained in step (1) or treating it with a dehydrant to obtain a purified cyclic formal (Y) which contains less water than in the cyclic formal (X).

Abstract translation: 循环甲醛的纯化方法，其中水从粗制环状醛中有效地除去，即难以与混合物分离的环状缩甲醛和水的混合物，从而获得仅含有的纯度的环状缩甲醛 非常少量的水。 循环甲醛的纯化方法的特征在于以下两个纯化步骤：（1）在供应位置向循环甲醛和水的混合物中提供蒸馏塔，并在提供具有沸点的亲水性溶剂（A）的同时进行蒸馏 在高于供给位置的位置处，从180℃到250℃，取出含有100〜5000ppm作为馏出物的水的循环甲醛（X），（2）蒸馏环状甲缩醛（X ）或用脱水剂处理，得到比循环缩甲醛（X）中含有的水少的纯化的环状缩甲醛（Y）。

公开(公告)号：US4289708A

公开(公告)日：1981-09-15

申请号：US65239

申请日：1979-08-09

Applicant: Robert H. Scott ,  Hubert H. Thigpen ,  Frank Wood, Jr.

Inventor： Robert H. Scott ,  Hubert H. Thigpen ,  Frank Wood, Jr.

IPC: C07C53/00 ,  C07C51/00 ,  C07C51/487 ,  C07C57/07 ,  C07C67/00 ,  C07C51/235 ,  C07C53/122 ,  C07C55/07

CPC classification number: C07C51/487 ,  Y02P20/582

Abstract: A process is described for separating soluble copper and manganese catalysts from organic saturated monocarboxylic acids having 3 to 9 carbon atoms by precipitating the copper and manganese as oxalates.

Abstract translation: 描述了通过使作为草酸盐的铜和锰沉淀来分离可溶性铜和锰催化剂与具有3至9个碳原子的有机饱和一元羧酸的方法。