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Preparation method of 2-methyltetrahydrofuran

A technology of methyl tetrahydrofuran and hydrogen, which is applied in chemical instruments and methods, organic compound/hydride/coordination complex catalysts, physical/chemical process catalysts, etc., can solve the problem of undurable catalytic activity and reduced stability of catalytic activity, etc. problems, to achieve the effects of stable catalytic activity, lower production costs, and high catalytic activity

Pending Publication Date: 2022-06-07
ANHUI JIXI COUNTY HUIHUANG CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

When targeting multi-component catalysts, due to the different volatility of each component (or the difference in phase transition temperature), the separation and enrichment between different components are caused, resulting in changes in the properties of the catalyst, resulting in multi-component catalysts The stability of the catalytic activity is reduced, and its catalytic activity is not durable

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Preparation of Porous Resin Solution:

[0027] Add 0.02mol acrylic acid, 0.1mol vinylpyridine, 0.02mol sodium hydroxide, 60mL deionized water and 40mL tetrahydrofuran into a three-port reactor with a stirrer and a reflux condenser, stir for 30min, and then add 0.06mol octavinyl POSS , 0.1g Tween 85, 0.002mol N,N-methylenebisacrylamide and 0.05g sodium persulfate, stirred at 50°C for 30min to obtain a porous resin solution, octavinyl POSS was purchased from Angxing New Carbon Materials Changzhou Co., Ltd. company.

Embodiment 2

[0029] Preparation of Porous Resin Solution:

[0030] Add 0.02mol acrylic acid, 0.1mol vinylpyridine, 0.05mol sodium hydroxide, 60mL deionized water and 40mL tetrahydrofuran into a three-port reactor with a stirrer and a reflux condenser, stir for 30min, and then add 0.08mol octavinyl POSS , 0.2g Tween 85, 0.003mol N,N-methylenebisacrylamide and 0.2g sodium persulfate, stirred at 60°C for 20min to obtain a porous resin solution, octavinyl POSS was purchased from Angxing New Carbon Materials Changzhou Co., Ltd. company.

Embodiment 3

[0032] Preparation of bilayer porous composite silicon:

[0033] (1), 8g triblock copolymer (F127, EO 106 PO 70 EO 106, BASF company)) was dissolved in 200 mL of deionized aqueous solution containing 13.78 g of anhydrous sodium acetate, stirred for 6 h to form stable micelles, and then added 0.08 mol of 1,2-bistrimethoxysilylethane, at 20 The pre-hydrolysis was carried out at ℃ for 6h, and then 0.02mol aminopropyltriethoxysilane was slowly added dropwise to the above solution. The above solution was stirred at 20℃ for 24h, transferred to an autoclave, crystallized at 100℃ for 24h, and taken out. Cool, filter, and dry at room temperature to obtain powder material. The method for extracting the template agent is as follows: each 1.0 g of the above powder material is mixed with 200 mL of absolute ethanol and 1.5 g of concentrated hydrochloric acid (mass fraction 36%), and refluxed for 24 hours. 0.5 g was added to 20 mL of triethylamine, stirred at room temperature for 20 min, ...

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Abstract

The invention relates to a preparation method of 2-methyltetrahydrofuran, which belongs to the technical field of fine chemical production, and comprises the following steps: step 1, immersing double-layer porous composite silicon in 0.1 M nickel nitrate solution, ultrasonically dispersing and oscillating for 24 hours at room temperature, and then centrifuging and washing to obtain a composite catalyst; and 2, uniformly mixing the reaction substrate, n-hexane and a composite catalyst, and carrying out a reaction for 2-6 h at 120-210 DEG C in a hydrogen atmosphere to obtain the 2-methyltetrahydrofuran. The inner layer of the composite catalyst is copper-loaded mesoporous silica, and the outer layer of the composite catalyst is nickel-loaded porous resin, so that due to the multilayer structure, the volatilization and enrichment of copper are reduced, and the stability of the catalytic activity of the composite catalyst is improved; and the composite catalyst has the characteristics of high copper and nickel loading quantity, low surface and efficient catalysis.

Description

technical field [0001] The invention belongs to the technical field of fine chemical production, and in particular relates to a preparation method of 2-methyltetrahydrofuran. Background technique [0002] 2-Methyltetrahydrofuran (hereinafter referred to as 2-Me-THF) is an important organic intermediate and an excellent solvent. In organic synthesis, it is mainly used to synthesize chloroquine phosphate, primaquine phosphate and thiamine. At the same time, due to its moderate boiling point (80.2°C), low solubility in water, easy separation from water, and Lewis basicity similar to that of tetrahydrofuran (THF), it can be applied to many organometallic reactions, in many respects It is superior to the current "universal solvent" tetrahydrofuran, which enables it to develop rapidly in the field of solvent replacement applications: (1) used to replace tetrahydrofuran, ether, etc. Toxic halogenated hydrocarbons, benzenes, etc. are used as reaction reagents or extraction solvent...

Claims

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Application Information

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IPC IPC(8): C07D307/06B01J35/10B01J31/22
CPCC07D307/06B01J31/1815B01J2531/847B01J2531/16B01J35/60Y02P20/584
Inventor 洪建敏朱良德程上飞方斌程典武
Owner ANHUI JIXI COUNTY HUIHUANG CHEM
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