Method for improving synthesis yield of adamantane

Abstract

The invention discloses a method for improving the synthesis yield of adamantane. The method comprises the following specific steps: placing 1 part by weight of catalyst and 1.4 to 2 parts by weight of tetrahydro-dicyclopentadiene into a reaction kettle, and heating slowly with stirring; adding water to break the catalyst after the reaction finishes; performing steam distillation to obtain solid adamantane, wherein the catalyst is granules prepared by phenol or derivatives thereof, anhydrous aluminum chloride and naphtha; the phenol or the derivatives thereof, the anhydrous aluminum chloride and the naphtha are in the weight: volume: weight ratio of 1:(20-50):(30-200) in g / mL / g. The catalyst granules are uniform, and an antioxidant is attached to the surface of the catalyst, so that the generation of tar when the adamantane is generated by the isomerization reaction of the tetrahydro-dicyclopentadiene can be effectively reduced; meanwhile, the yield of adamantane in the reaction can be greatly improved.

Description

technical field [0001] The invention relates to the field of chemical synthesis, in particular to a method for improving the synthesis yield of adamantane. Background technique [0002] As an important fine chemical product, adamantane is widely used in the fields of medicine, polymer materials, lubricants, catalysts, photographic photosensitive materials and aviation. The arrangement of carbon atoms in adamantane is equivalent to the arrangement of some carbon atoms in the diamond lattice. The structure is highly symmetrical and has a high melting point. The hydrogen atoms on the structure are prone to substitution reactions and have high activity. Adamantane is formed from the catalytic isomerization of tetrahydrodicyclopentadiene. The catalyst used requires not only good activity and selectivity, but also sufficient strength and moderate particle size. The main catalysts are aluminum tribromide and aluminum trichloride, and the cocatalysts are bromide, hydrogen fluoride,...

AI Technical Summary

Problems solved by technology

Adamantane is formed from the catalytic isomerization of tetrahydrodicyclopentadiene. The catalyst used requires not only good activity and selectivity, but also sufficient strength and moderate particle size. The main catalysts are aluminum tribromide and aluminum trichloride, and the cocatalysts are bromide, hydrogen fluoride, hydrogen chloride, etc. The catalyst used in practice is anhydrous aluminum trichloride. Although the yield of adamantane synthesized by this catalytic system is high , but the large amount of solvent, main catalyst and co-catalyst makes the synthesis cost of adamantane higher and the post-treatment is complicated

The application practice shows that in the actual production of adamantane in the isomerization reaction of tetrahydrodicyclopentadiene as a powdery aluminum trichloride catalyst, the catalytic effect is not ideal, and the yield is difficult to reach the predetermined level. Although the catalytic effect of aluminum is slightly better, due to the uneven particle size, it is difficult for some to have a good catalytic effect in the reaction, and it is difficult to increase the yield of adamantane, resulting in a low actual yield.

In the isomerization reaction, under the action of an acidic catalyst, tetrahydrodicyclopentene is oxidatively polymerized to produce a large amount of tar, which not only greatly reduces the reaction yield, but also brings great difficulties to the post-processing of the product

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