NaOH-Al2O3/GO catalyst and anisole catalytic synthesis thereof

A catalyst and technology of anisole, applied in the field of NaOH-Al2O3/GO catalyst and its catalytic synthesis of anisole, can solve the problems of low yield of anisole, low preparation cost, low self-toxicity, etc., and improve catalytic activity , large specific surface area, the effect of preventing agglomeration

Active Publication Date: 2020-02-14
YULIN UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] Dimethyl carbonate (DMC) is also a kind of common methylation reagent, because it also contains active groups such as methyl group and carbonyl group, and the preparation cost is relatively low, its own toxicity is low, and safety is higher, so it can be used as an ideal Alternatives, but the problem is that compared with dimethyl sulfate or methyl iodide, although it has advantages in terms of economy and environmental protection, its reactivity is lower and the yield of anisole is lower

Method used

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  • NaOH-Al2O3/GO catalyst and anisole catalytic synthesis thereof
  • NaOH-Al2O3/GO catalyst and anisole catalytic synthesis thereof
  • NaOH-Al2O3/GO catalyst and anisole catalytic synthesis thereof

Examples

Experimental program
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Embodiment 1

[0020] Weigh 0.12g of graphite oxide and add it to a 250mL beaker, add 120mL of deionized water to the beaker, stir evenly, put the beaker into an ultrasonic cleaner for ultrasonication for 2 hours, and mechanically peel off to form a brown transparent graphene oxide dispersion. Then, 1.5 g of aluminum nitrate and 1.3 g of urea were sequentially added to the graphene oxide dispersion, and the beaker was placed on a magnetic stirrer and stirred at room temperature for 2 hours to form a uniform dark brown mixture. Pour the dark brown mixture into a 200mL polytetrafluoroethylene-lined reaction kettle, then add 2mL N-methylpyrrolidone, stir evenly, put it into a blast drying oven, and react at 300°C for 12 hours under airtight conditions. After the reaction, cool to room temperature, wash the black solid by centrifugation, and dry at 70°C to obtain 0.3 g loaded Al 2 o 3 Nanoparticles of graphene oxide, denoted as Al 2 o 3 / GO. 0.3g Al 2 o 3 / GO was added to 10 mL of aqueous ...

Embodiment 2

[0022] Add dimethyl carbonate and phenol into the hydrothermal reaction kettle in different molar ratios, and add the NaOH-Al prepared in Example 1 with different mass contents of dimethyl carbonate and phenol total mass 2 o 3 / GO catalyst, and then reacted at different temperatures for different times under airtight conditions. The conversion rate of phenol and the proportion of anisole in the product were measured by gas chromatography-mass spectrometry (GC-MS). The specific reaction conditions and reaction results are shown in Table 1.

[0023] Table 1

[0024]

[0025] As can be seen from Table 1, the catalyst of the present invention is used to catalyze the reaction of dimethyl carbonate and phenol to synthesize anisole, and the conversion rate of phenol and the selectivity of anisole can reach more than 80%, which greatly improves the productive rate of anisole .

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Abstract

The invention discloses a NaOH-Al2O3 / GO catalyst and anisole catalytic synthesis thereof. Graphene oxide (GO) prepared by a modified Hummrs method serves as a carrier, hydrothermal method is used forloading Al2O3 nanoparticles, and then NaOH is loaded at a high temperature to prepare the NaOH-Al2O3 / GO catalyst. The GO in the catalyst can effectively prevent the agglomeration of the Al2O3 nanoparticles, the nanoparticles can in turn reduce the interlayer force of the GO, the GO has a large specific surface area, so that the loaded catalytic active components are greatly increased, and catalytic activity is further improved; and meanwhile the NaOH loaded in the catalyst provides alkalinity for the catalyst (dimethyl carbonate accelerates the reaction with phenol under alkaline conditions).Therefore, the catalyst is used for catalyzing the reaction between the dimethyl carbonate and the phenol, the yield of the anisole is greatly increased, the environmental protection pressure is reduced, the cost of raw materials can also be lowered, and the environmental protection and economic requirements of industrial anisole production are met.

Description

technical field [0001] The invention belongs to the technical field of preparation of anisole, in particular to a kind of NaOH-Al 2 o 3 / GO catalyst and its catalytic method for synthesizing anisole. Background technique [0002] Anisole has an anise-like aromatic odor and is widely used in organic synthesis reactions. Anisole is prepared from phenol and a methylating reagent under alkaline conditions. Traditionally, anisole is prepared by reacting methylating reagents such as dimethyl sulfate, methanol, and methyl iodide with phenol. Wherein, although the production process with dimethyl sulfate as raw material has good reactivity, a large amount of acid will be produced in the reaction process, which will not only pollute the environment, but also increase the processing cost, and dimethyl sulfate itself is a highly toxic substance . Using methyl iodide as a raw material has high reactivity, but methyl iodide itself is expensive, so it is not the first choice in terms ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/04C07C41/16C07C43/205
CPCB01J23/04B01J35/0013C07C41/16C07C43/205Y02P20/584
Inventor 张智芳任旭徐路路张璐王万庆毕文强侯锦涛舒军政
Owner YULIN UNIV
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