Catalyst for preparing anisole from phenol and dimethyl carbonate

A dimethyl carbonate and catalyst technology, applied in the chemical field, can solve the problems of limiting the conversion rate of raw materials and production and processing capacity, and achieve good industrial application prospects, expand the spacing between laminates, and have the effect of no equipment corrosion

Active Publication Date: 2022-05-17
CHINA UNIV OF MINING & TECH (BEIJING)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

According to the characteristics of this reaction, low temperature is beneficial to the selectivity of anisole, but it limits the conversion rate and production and processing capacity of raw materials from a kinetic point of view.

Method used

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  • Catalyst for preparing anisole from phenol and dimethyl carbonate
  • Catalyst for preparing anisole from phenol and dimethyl carbonate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] In beaker A, make 100ml solution A with 0.12mol magnesium nitrate hexahydrate and 0.03mol aluminum nitrate nonahydrate with deionized water, and make 100ml solution with 0.255mol sodium hydroxide and 0.0648mol anhydrous sodium carbonate with deionized water B, add 100ml deionized water to beaker C. After stirring and dissolving, use a peristaltic pump to pump solution A and solution B into beaker C at a certain rate. After the end, continue to stir the solution in beaker C at room temperature for 10 h, and maintain the pH between 9-11. After the stirring, the slurry in the beaker C was filtered and washed with deionized ion until neutral. Dry the obtained precipitate in an oven at 110°C for 12 hours, and the product is a hydrotalcite-like material, which is denoted as Mg4Al-LDH. Reserved for subsequent experiments.

[0030] Put the Mg4Al-LDH into the muffle furnace for calcination at a heating rate of 3°C / min, from room temperature to 450°C and then calcine for 5h. ...

Embodiment 2

[0033] Take 1g of Mg4Al-LDH and add 50ml of 0.1mol / L ammonium fluoroaluminate solution. Stirring was carried out at room temperature for 6h. After the stirring is finished, filter with suction, wash, dry, and roast, and the product is marked as Mg4Al-LDO-0.1FAl. A 0.1 g sample was taken for gas-phase alkylation of phenol and dimethyl carbonate under the same reaction conditions as in Example 1. The product was analyzed by gas chromatography, and the conversion rate was 99.22%, and the selectivity was 69.98%. The acid-base TPD of the obtained catalyst is shown in figure 2 , the amount of weak base is 0.21mmol / g, the amount of strong base is 0.408mmol / g, the amount of weak acid is 0.084mmol / g, and the amount of strong acid is 0.305mmol / g.

Embodiment 3

[0035]Take 1g of Mg4Al-LDH, add 50ml of 0.025mol / L ammonium fluoroaluminate solution, stir at room temperature for 6h, then suction filter, wash, dry, and roast. The product is marked as Mg4Al-LDO-0.025FAl. A 0.1 g sample was taken for the gas-phase alkylation reaction of phenol and dimethyl carbonate. The reaction conditions were the same as in Example 1. The product was analyzed by gas chromatography, and the conversion rate was 99.04%, and the selectivity was 83.4%.

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PUM

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Abstract

The invention provides a catalyst for preparing anisole from phenol and dimethyl carbonate, which utilizes IIA group alkaline earth metal salt and aluminum nitrate to form hydrotalcite through co-precipitation of sodium hydroxide and sodium carbonate, and then adds fluorosilicate and / or obtained by intercalation modification of fluoroaluminate.

Description

technical field [0001] The invention relates to a catalyst for preparing anisole from phenol and dimethyl carbonate, belonging to the field of chemistry. Background technique [0002] Anisole is an important organic chemical raw material, and has important applications in dyes, medicines, spices, resins, and synthetic fibers. [0003] At present, anisole is mainly produced in industry with phenol and dimethyl sulfate as raw materials. Dimethyl sulfate is a highly toxic substance, which produces a large amount of highly toxic wastewater and solid waste. The environmental pollution is very serious, and some manufacturers have been forced to limit production. , Suspension of production has seriously affected the healthy development of downstream related industries. Dimethyl carbonate is a new green chemical raw material with low pollution and environmental friendliness. As a process of methylating reagent and phenol to synthesize anisole, it is harmless, non-toxic and non-poll...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J37/03B01J27/232B01J27/24B01J27/25B01J27/125C07C41/16C07C43/205
CPCB01J37/03B01J27/232B01J27/24B01J27/25B01J27/125C07C41/16C07C43/205Y02P20/584
Inventor 张海永张璐王永刚许德平
Owner CHINA UNIV OF MINING & TECH (BEIJING)
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