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Method for synthesizing adamantane from tetrahydrodicyclopentadiene

A technology of tetrahydrodicyclopentadiene and hanging tetrahydrodicyclopentadiene, which is applied in the field of adamantane synthesis, can solve problems such as cumbersome operation process, and achieve the effects of simple recovery processing, reduction of production cost and reduction of consumption

Active Publication Date: 2020-05-29
四川众邦新材料股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this method still directly uses aluminum trichloride as a catalyst, and there is still a problem that a large amount of hydrogen chloride gas needs to be absorbed and disposed of during the treatment of a large amount of deactivated aluminum trichloride, and the reaction operation is carried out intermittently in the reactor, and the operation process is more cumbersome.

Method used

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Experimental program
Comparison scheme
Effect test

Embodiment

[0042] In the catalyst storage tank protected by nitrogen, the catalyst (the chloroaluminic acid type room temperature ion synthesized by 3-methyl-1-butylimidazole chloride and anhydrous aluminum chloride according to the molar ratio of 1:1.8~2) is pre-loaded. Liquid) about 50Kg, fill the bridged tetrahydrodicyclopentadiene in the starting material storage tank protected with nitrogen, the initial loading amount is 120Kg, and preheat to 60 ° C ~ 65 ° C to make it in a liquid state. Start the micro-metering pump in turn to pump the catalyst chloroaluminate room temperature ionic liquid and the starting material bridged tetrahydrodicyclopentadiene into the micro-reactor, while heating to control the reaction temperature of the reactor so that the reaction tube is in the Gradually increase in the range of 60°C to 90°C.

[0043] The reaction tube of the microreactor is a special-shaped inner channel, the diameter (inner diameter) of which is in the range of 0.5 mm to 1.5 mm, and t...

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Abstract

The invention relates to a method for synthesizing adamantane from tetrahydrodicyclopentadiene. The method comprises the following steps: reacting anhydrous AlCl3 with alkyl tertiary amine, alkyl imidazole and alkyl pyridine to prepare chloroaluminate room-temperature ionic liquid as a catalyst; continuously using the catalyst with reduced activity after activation treatment; respectively pumpingthe catalyst and the bridge-type tetrahydrodicyclopentadiene into a micro-tube reactor by using a metering pump, and partially converting to generate adamantane; and feeding the material discharged from the reactor into a cylindrical separation container, performing standing for layering, transferring the upper-layer oil-phase material into a crystallizer, performing cooling to separate out adamantane crystals, returning mother liquor to be continuously used as a starting raw material, and returning a lower-layer catalyst to be continuously used. The method has the characteristics of process link simplification, the high product yield, continuous production and the like.

Description

technical field [0001] The invention relates to a synthesis method of adamantane, in particular to a reaction method for synthesizing target product adamantane from tetrahydrodicyclopentadiene as a starting material through catalytic isomerization reaction. Background technique [0002] The chemical name of Adamantane is tricyclic [3,3,1,13,7] decane, which is a cyclic tetrahedral hydrocarbon composed of 10 carbon atoms and 16 hydrogen atoms. Due to its symmetry and rigidity, adamantane has relatively stable properties. In addition, the hydrogen atoms in its molecule are prone to SN1-type nucleophilic substitution reactions and SE2-type electrophilic substitution reactions, resulting in a variety of derivatives, making it widely used in medicine, Functional polymer materials, lubricants, surfactants, catalysts, etc. have a wide range of uses. [0003] At present, the industrialized adamantane synthesis methods at home and abroad all use bridged tetrahydrodicyclopentadiene a...

Claims

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Application Information

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IPC IPC(8): C07C5/29C07C13/615B01J31/02
CPCC07C5/29B01J31/0279B01J31/0284C07C2603/74B01J2231/52C07C2531/02C07C13/615Y02P20/584
Inventor 王南
Owner 四川众邦新材料股份有限公司