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Environmentally-friendly method for producing adamantine

A technology of green production and adamantane, applied in chemical instruments and methods, chemical recovery, physical/chemical process catalysts, etc., can solve the problems of catalysts not being reusable, polluting the environment, etc., and achieve favorable production, low equipment requirements and good reaction conditions mild effect

Inactive Publication Date: 2014-04-09
NANJING TECH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

What the main catalyst that proposes in above three public descriptions adopts still is traditional liquid acid catalyst, just improved it on this basis, but can't avoid its various shortcomings, as polluting environment, catalyst can not be reused etc.

Method used

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  • Environmentally-friendly method for producing adamantine

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] A. Preparation of two-component supported catalyst: in N 2 Under protection, add 120ml of chloroform and 12g of 20-40 mesh SiO2 which had been roasted at 500°C for 6h to the four-necked flask. 2 , reflux for 6 hours to remove traces of water, then add 2.4g of anhydrous aluminum trichloride and 0.6g of anhydrous stannous chloride, continue to reflux for 12 hours, filter, wash 6 times with 30ml of chloroform, and vacuum dry at 80°C for 12 hours , calcined at 300°C for 5h to prepare the two-component supported catalyst AlCl 3 -SnCl 2 / SiO 2 , the load of the two components was measured to be 18.1%, wherein the mass ratio of anhydrous aluminum trichloride and anhydrous stannous chloride was 1:0.27, and ground to 40-60 mesh for later use.

[0022] B. Preparation of adamantane: In a fixed bed reactor, add 11.6g of two-component supported catalyst AlCl 3 -SnCl 2 / SiO 2 , adopting continuous circulation feed to prepare adamantane by isomerization of pendant tetrahydrodicy...

Embodiment 2

[0024] A. Preparation of two-component supported catalyst: under the protection of He, add 270ml of carbon tetrachloride and 13.5g of 20-40 mesh SiO to a four-necked flask that has been pre-calcined at 600°C for 4h 2 , reflux for 5h to remove traces of water, then add 1.25g of anhydrous aluminum trichloride and 0.25g of anhydrous stannous chloride, continue to reflux for 12h, filter, wash 3 times with 50ml of carbon tetrachloride, 70 ℃ Vacuum drying for 12 hours, followed by calcination at 350°C for 4 hours to prepare the two-component supported catalyst AlCl 3 -SnCl 2 / SiO 2 , the measured two-component loading is 9.4%, wherein the mass ratio of anhydrous aluminum trichloride and anhydrous stannous chloride is 1:0.24, ground to 40-60 mesh for later use.

[0025] B. Preparation of adamantane: In a fixed bed reactor, add 10.3g of two-component supported catalyst AlCl 3 -SnCl 2 / SiO 2 , adopting continuous circulation feed to prepare adamantane by isomerization of pendant tet...

Embodiment 3

[0027] A. Preparation of two-component supported catalyst: in N 2 Under protection, add 157.5ml of ethanol and 10.5g of 20-40 mesh SiO2 which had been roasted at 550°C for 6h to the four-necked flask. 2 , refluxed for 6 hours to remove traces of water, then added 3.21g of anhydrous aluminum trichloride and 1.29g of anhydrous stannous chloride, continued to reflux for 6 hours, filtered, washed 6 times with 30ml of chloroform, and dried in vacuum at 80°C for 9 hours , calcined at 400°C for 3h to prepare the two-component supported catalyst AlCl 3 -SnCl 2 / SiO 2 , the measured two-component loading is 22.3%, wherein the mass ratio of anhydrous aluminum trichloride and anhydrous stannous chloride is 1:0.33, ground to 40-60 mesh for later use.

[0028] B. Preparation of adamantane: In a fixed bed reactor, add 9.9g of two-component supported catalyst AlCl 3 -SnCl 2 / SiO 2 , adopting continuous circulation feed to prepare adamantane by isomerization of pendant tetrahydrodicyclo...

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Abstract

The invention discloses an environmentally-friendly method for producing adamantine. The method comprises the following steps of: under the action of a two-component supported catalyst, continually and circularly feeding into a fixed bed reactor, wherein the two components refer to aluminum chloride and tin dichloride, and isomerizing exo-tetrahydrodicyclopentadiene for preparing adamantine. Under the condition that the reaction temperature is 120-180 DEG C, the reaction pressure is 0.6-1.2MPa, the reaction space velocity is 0.1-2 h<-1> and V(N2) / V (raw material)=50-600, the transformation rate of the exo-tetrahydrodicyclopentadiene is over 95 percent, the yield of the adamantine is up to 76 percent, and the purity of the adamantine is over 99.5 percent. In the method, white adamantine crystals which do not contain any solvent and have high purity can be prepared by performing simple physical-mechanical separation, washing with water and drying without using any solvent; the preparation process is simple; the catalyst is easy to separate and can be used repeatedly; and the method has the advantages of low production cost, low environmental pollution and safe production.

Description

field of invention [0001] The invention relates to a method for producing adamantane, in particular to a green method for producing adamantane by isomerizing pendant tetrahydrodicyclopentadiene, which belongs to the technical field of chemical industry. Background technique [0002] Adamantane is a highly symmetrical cage hydrocarbon. Due to its unique structure and properties, it has been widely used in the fields of medicine, fine chemicals, functional materials, military and aviation since it was discovered and separated from petroleum in the 1930s. the use of. With the wide application of adamantane, more and more scholars are devoted to the research of simpler and economical preparation methods of adamantane. At present, the preparation methods of adamantane mainly include the following types: ① Ring-closing method. This is the earliest preparation method of adamantane, which has complex reactions, many steps and low yield of only 6.5%. ②Aluminum trichloride isomeriz...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C13/615C07C5/29B01J27/135B01J35/02B01J35/00
CPCY02P20/584
Inventor 周志伟武文良秦娟徐卫敏
Owner NANJING TECH UNIV