A kind of process of preparing adamantane by carbon five dicyclopentadiene

A technology for dicyclopentadiene and adamantane, which is applied in the field of producing adamantane from dicyclopentadiene, can solve the problems of low purity of adamantane, and achieve the advantages of reducing the severity of the reaction, the selectivity, and the degree of polymerization and ring opening. Effect

Inactive Publication Date: 2017-09-29
山东玉皇盛世化工股份有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The problem to be solved by the present invention is the problem of low purity of adamantane in the prior art due to the high impurity of dicyclopentadiene, and a new method for preparing adamantane from carbon pentacyclopentadiene is provided

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  • A kind of process of preparing adamantane by carbon five dicyclopentadiene

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Effect test

Embodiment 1

[0020] 1.0 kg of carbon pentadicyclopentadiene (83% by weight) and 4.0 kg of methylcyclohexane (99.95% by weight) were mixed and then put into a magnetic stirring tank, and then 50 grams of nickel catalyst (by weight) were added to the mixed solution. 95%), replaced with 99.99% nitrogen for three times, passed hydrogen into the magnetic stirring tank, then raised the temperature to 105 °C, maintained the pressure in the tank at 6.0 MPa, stirred for 6 hours, and cooled down to room temperature. The reacted mixture was separated to obtain 800 grams of solid product, which was mixed with 500 grams of aluminum trichloride catalyst and 4.8 grams of ethylaluminum dichloride at 45°C for 6 hours to obtain 340 grams of adamantane product. According to NMR and gas chromatography analysis, the product purity is greater than 99%.

Embodiment 2-10

[0022] Carry out hydrogenation to carbon five dicyclopentadiene according to each condition of embodiment 1, just be to regulate the consumption of nickel catalyst, the concentration of dicyclopentadiene, the consumption of aluminum trichloride catalyst and the kind of auxiliary agent and auxiliary agent The ratio with aluminum trichloride is listed in Table 1.

[0023] Table 1

[0024]

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Abstract

The invention relates to the field of preparing adamantane from dicyclopentadiene, in particular to a process for preparing adamantane from carbon pentacyclopentadiene. The process for producing adamantane from C5 dicyclopentadiene uses C5 separation to obtain dicyclopentadiene as a raw material, and uses a nickel-containing metal catalyst to separate the hydrogenated mixed solution. The catalyst containing aluminum trichloride produces adamantane, which effectively solves the problem of low purity of adamantane caused by high carbon pentacyclopentadiene impurities, and can be applied to the industrial production of carbon pentacyclopentadiene to adamantane.

Description

(1) Technical field [0001] The invention relates to the field of preparing adamantane from dicyclopentadiene, in particular to a process for preparing adamantane from carbon pentacyclopentadiene. (2) Background technology [0002] At present, dicyclopentadiene mainly comes from cracking by-product carbon five and cracking by-product carbon nine. Due to the difference in composition and separation process, the purity of dicyclopentadiene obtained from by-product carbon five is generally about 80%, while The purity of dicyclopentadiene obtained from by-product carbon nine is generally above 93%. Although both are dicyclopentadiene, the purity of dicyclopentadiene separated from C5 is obviously low, and the cost of obtaining dicyclopentadiene of the same purity is relatively high. Therefore, the value equivalent to that of carbon nine dicyclopentadiene is realized by adjusting the processing technology of dicyclopentadiene. The important pharmaceutical raw material adamantane...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C5/29C07C13/615B01J23/755B01J23/83B01J23/888
Inventor 冯汝明刘汝玲王玉强陈双喜王胜伟
Owner 山东玉皇盛世化工股份有限公司
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