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Method for preparing adamantine on solid acid catalyst

A solid acid catalyst, adamantane technology, applied in the direction of isomerization to hydrocarbon production, can solve the problems of high reaction temperature and high cost, and achieve the effects of low reaction temperature, low equipment investment and high reaction activity

Inactive Publication Date: 2008-02-20
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this type of catalyst uses noble metal as the main catalyst, the cost is high, and the reaction temperature is higher than 250°C. In order to increase the yield of adamantane, HCl gas needs to be added during the reaction process, which requires the reaction equipment to have strong corrosion resistance.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] (1) Catalyst preparation

[0017] fixed bed AlCl 3 Fill the generator with 20mL high-purity γ-Al 2 o 3 (spherical d=1.8-2.0mm), heated to 500°C, and fed N at flow rates of 40ml / min and 0.8-2.0mL / h respectively 2 and CCl 4 , producing AlCl 3 Vapor; fixed bed AlCl 3 γ-Al with mesoporous structure is loaded into the immobilization reactor 2 o 3 (60-100 mesh) 5mL (3.08g), dehydration heat treatment at 500°C for 2h; at 40mL / min N 2 The AlCl produced under the loading band 3 Add AlCl 3 In the immobilization reactor, AlCl was carried out at 300 3 Immobilized reaction, reaction time 3.0h, then at 400 ° C with N 2 Purged for 1h, then lowered to room temperature for later use.

[0018] (2) Synthesis of adamantane

[0019] The isomerization reaction of synthetic adamantane was carried out in a batch-type suspended bed reactor, and 5 mL (3.08 g) of solid-supported AlCl 3 Catalyst, 20mL of cyclohexane and 0.5g of tetrahydrodicyclopentadiene were successively added into...

Embodiment 2

[0023] (1) Catalyst preparation

[0024] In high purity N 2 Under protection, 5mL 60-100 mesh mesoporous γ-Al 2 o 3 After the carrier particles were treated in a muffle furnace at 400 ° C for 3 h, they were placed in a round bottom flask equipped with a magnet, and then CCl dehydrated with a 5 Å molecular sieve was added. 4 Solution, back distillation at 80°C for 2h, then add anhydrous AlCl to the flask 3 , Continue to distill at 80°C for 48h. Evaporate residual CCl 4 . Reuse new CCl 4 Wash the solid sample several times until no chloride ions are detected in the washing solution, then the immobilized AlCl 3 catalyst precursor. The resulting catalyst precursor was heated at 400 °C with N 2 Gas purged for 1h, then in N 2 Purge under protection and cool to room temperature.

[0025] (2) Synthesis of adamantane

[0026] The catalyst prepared in Example 2 (1), 20mL cyclohexane and 0.5g tetrahydrodicyclopentadiene are added successively to a stainless steel autoclave wi...

Embodiment 3

[0028] (1) Catalyst preparation

[0029] In high purity N 2 Under protection, 5mL 60-100 mesh mesoporous γ-Al 2 o 3 After the carrier particles were treated in a muffle furnace at 400 °C for 3 h, they were placed in a round-bottomed flask equipped with a magnet, and then CCl dehydrated with a 5 Å molecular sieve was added. 4 Solution, back distillation at 80°C for 2h, then add TiCl to the flask 4 and anhydrous AlCl 3 , Continue to distill at 80°C for 48h. Evaporate residual CCl 4 . Reuse new CCl 4 Wash the solid sample several times until no chloride ions are detected in the washing solution, then the immobilized AlCl 3 catalyst precursor. The resulting catalyst precursor was heated at 400 °C with N 2 Gas purged for 1h, then in N 2 Purge under protection and cool to room temperature.

[0030] (2) Synthesis of adamantane

[0031]The catalyst prepared in Example 3 (1), 20mL cyclohexane and 0.5g tetrahydrodicyclopentadiene are added successively to a stainless steel ...

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Abstract

The invention relates to a method for synthesizing adamantane on solid-acid catalyst. The solid-acid catalyst is a solid-borne halide comprising chloride or bromide of aluminum, titanium, zinc or iron, etc., on carriers of mesopore Al2O3, Al2O3-SiO2 or silicon-aluminum molecular sieve, etc., uses tetrahydric dicyclopentadiene as raw material and synthesizes adamantane by isomerization reaction. Isomerization reaction is carried out in the mode of liquid-solid multiphase stirring reaction or fixed bed reaction and uses C6 to C10 linear paraffin or cyclane as solvent, the reaction temperature is 10 DEG C to 200 DEG C, reaction pressure is 0.5 to 5.0MPa in the atmosphere of H2 or N2. Reaction system does not need catalyst accelerato of HCl or HBr, etc., therefore, reaction equipment is not required to have great erosion-resistance. No separation process between catalyst and result is required after reaction and the method does not pollute the environment.

Description

technical field [0001] The present invention relates to a method for producing adamantane. More specifically, it is a method for producing adamantane by liquid-solid heterogeneous stirring reaction or fixed-bed reaction on a solid acid catalyst. Background technique [0002] The scientific name of adamantane is tricyclo[3,3,1,73.7]decane. Its basic skeleton is similar to a diamond lattice structure. It is a highly symmetrical cage hydrocarbon. It is used in medicine, polymer materials, lubricants, photography It has a wide range of uses in photosensitive materials, catalysts, surfactants, pesticides, aviation and other fields. The industrial production of adamantane generally adopts the catalytic isomerization of tetrahydrodicyclopentadiene, and aluminum trichloride is used as a catalyst. The amount of catalyst used in this process is relatively large, and complexes are formed with heavy components during the isomerization reaction process, which cannot be recycled. This ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C13/615C07C5/27
Inventor 纪敏蔡天锡贺民李秀媛张有家田福平
Owner DALIAN UNIV OF TECH
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