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Method for production of adamantane

A technology of adamantane and methyl norbornane, which is applied in the preparation of organic compounds, organic chemistry methods, chemical instruments and methods, etc., can solve problems such as increasing pressure difference

Inactive Publication Date: 2009-05-27
IDEMITSU KOSAN CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, if oxygen-containing compounds are present in the supplied raw materials, solids derived from oxygen-containing compounds will be generated and accumulated at the inlet of the reactor or in the lower part of the reactor, increasing the pressure difference in the reactor, resulting in unavoidable Emergency Stop Reactor Problems

Method used

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  • Method for production of adamantane

Examples

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Effect test

preparation example 1

[0075] Preparation of Metal-supported Solid Acid Catalyst

[0076] 1.275 kg of sodium ion-exchanged Y-type zeolite (hereinafter referred to as NaY) was stirred and suspended in 7 kg of pure water, and heated to 60°C. While continuing to stir, add an aqueous solution (RE 2 o 3 (CeO 2 +La 2 o 3 +Nd 2 o 3 +Pr 2 o 3 +Sm 2 o 3A total of 890 g)), stirring was continued for 2 hours. After the powder was filtered, it was washed with 15 kg of pure water, dried, and then calcined at 650° C. for 3 hours (one exchange of mixed rare earths). Suspend 340 g of the sintered powder in 2 kg of warm water at 60°C. Hydrochloric acid was added with stirring until the pH reached 5.01. In this slurry, add 2kg above-mentioned mixed rare earth aqueous solution (RE 2 o 3 (CeO 2 +La 2 o 3 +Nd 2 o 3 +Pr 2 o 3 +Sm 2 o 3 A total of 130.6 g)) was stirred at 60° C. for 2 hours. After the powder was filtered, it was washed with 4 kg of pure water (secondary exchange of mixed rare eart...

Embodiment 1

[0078] (1) Isomerization reaction steps

[0079] 13 g of the catalyst obtained in the above Preparation Example 1 were respectively filled in a stainless steel pre-reaction tube and an isomerization reaction tube with a total length of 60 cm and a diameter of 14 mm, and sintered at 300° C. for 3 hours under air flow. After nitrogen substitution, hydrogen reduction was performed at 300° C. for 2 hours under normal pressure and hydrogen flow.

[0080] After that, a mass ratio of 2:1 mixed solution (32 ml / hour) of decalin and trimethylenenorbornane (TMN) containing 1000 mg / L oxygen from oxygen-containing compounds and hydrogen was supplied from the lower part of the pre-reaction tube, When the pressure is 6MPa, the inlet temperature of the pre-reaction tube is 150°C, the outlet temperature is 175°C, and the MHSV (mass space velocity) is 2.4h -1 , Hydrogen / TMN ratio of 2.0 under the condition of pretreatment, so that the oxygen content of the outlet from the oxygen-containing com...

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Abstract

Provided is a method for production of adamantanes, in which, when a tricyclic saturated hydrocarbon compound having 10 or more carbon atoms is isomerized in the presence of a solid catalyst to give adamantanes, no solid matter derived from an oxygen-containing compound is formed or accumulated in the inlet or the bottom of an isomerization reactor by providing a pre-reactor in an isomerization step even if the oxygen-containing compound is present in a raw material to be supplied.

Description

technical field [0001] The present invention relates to a process for the preparation of adamantanes using a prereactor in the isomerization reaction step. More specifically, it relates to a method for continuously producing adamantanes of high purity using a solid catalyst, by disposing a prereactor in the isomerization reaction step, which enables continuous operation for a long period of time. Background technique [0002] Adamantane has a cage structure composed of four cyclohexane rings, and is a highly symmetrical and stable compound. Since adamantanes having the above-mentioned adamantane skeleton exhibit specific functions, they are known to be useful as raw materials and intermediates of various chemicals such as lubricants, agricultural chemicals and pharmaceutical raw materials, and highly functional industrial materials. [0003] A method for producing adamantanes is generally known to be carried out by isomerizing a tricyclic saturated hydrocarbon compound havi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C5/27C07B61/00C07C13/615
CPCC07C5/29C07C2103/74B01J29/126B01J2229/186C07C2529/08C07C2529/12B01J29/088C07C2603/74C07C13/615C07B61/00C07C5/27
Inventor 斋藤昌男小岛明雄间濑淳草场敏彰
Owner IDEMITSU KOSAN CO LTD
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