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Method for preparing anisole from phenol and methanol

A technology for the preparation of methanol and anisole, applied in the dehydration of hydroxyl-containing compounds to prepare ethers, ether preparations, chemical instruments and methods, etc., can solve the problems of being difficult to be market competitive, low catalyst service life, high production costs, etc. Low cost, long service life, and less by-products

Pending Publication Date: 2021-08-10
BAOJI UNIV OF ARTS & SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Although some breakthroughs have been obtained in the above researches, and the catalysts have shown high catalytic activity, most of the catalysts have C-alkylation and O-alkylation at the same time, and there is a gradual increase in catalyst activity as the reaction progresses. Defects such as attenuation and low service life of catalysts will inevitably lead to problems such as high production costs, high energy consumption, and difficulty in becoming competitive in the market

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] 1. Add 100g γ-Al 2 o 3 Add to 1000g of deionized water, add 3g of ammonium acetate, stir at 70°C for 6h, filter, wash, dry at 70°C, grind into powder and place in a tube furnace, blow in argon at 50mL / min, at 500°C Calcined at ℃ for 4h to prepare the catalyst carrier.

[0024] 2. Add 7.2g of ferric nitrate to 72g of deionized water, then add 100g of catalyst carrier, stir evenly, ultrasonicate for 20min, leave to stand at room temperature for 10h, dry at 60°C, grind into powder, and then mix it with 1.98g of ammonium fluoride Add it into 78g of deionized water, stir evenly, ultrasonicate for 20min, stand at room temperature and age for 10h, dry at 60°C, grind it into powder, put it in a tube furnace, feed argon gas at 50mL / min, and roast at 500°C 4h, the catalyst was prepared.

[0025]3. The catalyst obtained in step 2 is granulated and shaped into cylindrical particles with a diameter of 4mm and a height of 4mm, and packed into a fixed bed reactor. The catalyst load...

Embodiment 2

[0027] 1. Add 100g γ-Al 2 o 3 Add it to 1000g deionized water, add 2g ammonium acetate and 2.78g magnesium acetate, stir at 70°C for 6h, filter, wash, dry at 70°C, grind it into powder, place it in a tube furnace, and feed it at 50mL / min Argon, calcined at 500°C for 4h to obtain a catalyst carrier.

[0028] 2. Add 4.58g of magnesium nitrate to 72g of deionized water, then add 100g of catalyst carrier, stir evenly, ultrasonicate for 20min, leave it at room temperature for 10h, dry at 60°C, grind it into powder, and mix it with 1.32g of ammonium fluoride Add it into 78g of deionized water, stir evenly, ultrasonicate for 20min, stand at room temperature and age for 10h, dry at 60°C, grind it into powder, put it in a tube furnace, feed argon gas at 50mL / min, and roast at 500°C 4h, the catalyst was prepared.

[0029] 3. This step is the same as that in Example 1. After 200 hours of reaction, the conversion rate of phenol is 88.9%, and the selectivity of anisole is 91.4%.

Embodiment 3

[0031] 1. Add 100g γ-Al 2 o 3 Add it to 1000g deionized water, add 2g ammonium acetate and 2.06g calcium acetate, stir at 70°C for 6h, filter, wash, dry at 70°C, grind it into powder, place it in a tube furnace, and feed it at 50mL / min Argon, calcined at 500°C for 4h to obtain a catalyst carrier.

[0032] 2. Add 4.22g of calcium nitrate to 72g of deionized water, then add 100g of catalyst carrier, stir evenly, ultrasonicate for 20min, leave it at room temperature for 10h, dry at 60°C, grind it into powder, and mix it with 1.32g of ammonium fluoride Add it into 78g of deionized water, stir evenly, ultrasonicate for 20min, stand at room temperature and age for 10h, dry at 60°C, grind it into powder, put it in a tube furnace, feed argon gas at 50mL / min, and roast at 500°C 4h, the catalyst was prepared.

[0033] 3. This step is the same as in Example 1. After 200 hours of reaction, the conversion rate of phenol is 86.6%, and the selectivity of anisole is 93.4%.

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Abstract

The invention discloses a method for preparing anisole from phenol and methanol. The method is characterized in that a fixed bed reactor is adopted, and active components such as sodium acetate, potassium acetate, calcium acetate, magnesium acetate or ammonium acetate modified gamma-Al2O3 loaded ammonium fluoride, sodium fluoride, potassium fluoride, ferric fluoride, magnesium fluoride, calcium fluoride and the like are used as catalysts to catalyze phenol and methanol to prepare anisole. The modification of the ferric fluoride, the magnesium fluoride and the calcium fluoride is prepared by dipping corresponding nitrate and ammonium fluoride on gamma-Al2O3 for two times. Efficient synthesis of anisole is achieved, the phenol conversion rate is high, anisole selectivity is high, the catalyst is simple in preparation process, low in cost, high in stability and long in service life, and the application requirement of an industrial catalyst is met.

Description

technical field [0001] The invention belongs to the technical field of preparation of anisole, in particular to a method for preparing anisole by using phenol and methanol. Background technique [0002] Anisole, also known as anisole or methoxybenzene, is found naturally in tarragon oil. Because of its unique fragrance, anisole is widely used in perfumes, insect pheromones, phenolic resins, soaps, insect repellents and additives, etc. Because of its active ether bond, it can be used as a raw material for industrial organic synthesis. Moreover, anisole can increase the octane number of gasoline and can be used as a gasoline additive instead of methyl tert-butyl ether. Because of its high dielectric constant and high boiling point, it can be used as an initiator, thermostat filler, etc., and is an important organic chemical raw material and intermediate. In recent years, the market demand for anisole has increased dramatically. Anisole is used as a solvent in the printing ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C41/09C07C43/205B01J27/25B01J37/08B01J37/02B01J35/02B01J35/00
CPCC07C41/09B01J27/25B01J37/082B01J37/0201B01J35/50B01J35/40C07C43/205
Inventor 王伟张凡李少晶冯国栋罗小林
Owner BAOJI UNIV OF ARTS & SCI