Catalyzed synthesis method for anisole

A synthesis method and technology of anisole, which is applied in the field of catalytic synthesis of anisole, can solve the problems of low yield of anisole product, high equipment operation cost, incomplete phenol conversion, etc., so as to facilitate recycling and reuse , energy economy, and the effect of not easy to lose ingredients

Inactive Publication Date: 2019-01-04
阜新汉道化工有限责任公司
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  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Although most of the catalysts developed at present can be successfully applied to the process of synthesizing anisole from phenol and dimethyl carbonate, there are more or less problems respectively, such as high reaction temperature, or incomplete conversion of phenol, Or the yield of anisole product is not high, etc., these problems will inevitably lead to high energy consumption in production, high unit consumption of raw materials, high equipment operating costs, all of which will increase production costs

Method used

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  • Catalyzed synthesis method for anisole
  • Catalyzed synthesis method for anisole
  • Catalyzed synthesis method for anisole

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preparation example Construction

[0036] The preparation condition of table 1 catalyst

[0037]

[0038] The embodiment of the present invention uses gas chromatography to detect anisole, and the conditions are as follows:

[0039] GC Agilent 6890 equivalent instrument

[0040] FID detector, chromatography workstation

[0041] ZB-5 (30m×0.32mm×0.25μm) equivalent chromatographic column

[0042] Hydrogen flow rate: 30ml / min

[0043] Air flow rate: 300ml / min

[0044] Carrier gas (high purity nitrogen) flow rate: 1.0ml / min

[0045] Gasification chamber temperature: 260°C

[0046] Detector temperature: 260°C

[0047] Initial column temperature: 100°C

[0048] End column temperature: 280°C

[0049] Heating rate: 30°C / min

Embodiment 1

[0050] The preparation of embodiment 1 anisole

[0051] ① Catalyzed reaction: Put 95g (1mol) of phenol, 190g (2mol) of dimethyl carbonate and 47.5g of No. 1 catalyst into a 0.5L three-necked flask equipped with a thermometer, stirring, fractionating column, condenser and receiving bottle, and stir to raise the temperature Reflux begins to appear at about 90°C. After that, pay attention to controlling the heating rate, and maintain the extraction temperature of the fractionation column at 60-65°C to collect the methanol produced by the reaction. As the reaction continues, the temperature of the kettle will gradually increase. When the temperature reaches 120°C, almost no methanol is produced, and the reaction is nearly complete. A sample from the kettle is taken for gas phase detection and no phenol remains, and the reaction is over.

[0052] ② Recovery of dimethyl carbonate: ① After the reaction, replace the receiving bottle, gradually increase the temperature of the kettle fr...

Embodiment 2

[0055] The preparation of embodiment 2 anisole

[0056] Reaction process is with embodiment 1, and difference with embodiment 1 is, in embodiment 1, dimethyl carbonate consumption is changed into 142.5g (1.5mol), replaces No. 1 catalyst with No. 2 catalyst 47.5g simultaneously, other not Change. During the reaction process, the reaction temperature rose up to 130° C., and 49.3 g of the catalyst was recovered after the reaction to obtain 104 g of 99.3% anisole, the product yield was 96.3%, and the distillation residue was 0.9 g.

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Abstract

The invention discloses a preparation method of anisole. The preparation method of the anisole comprises the steps of carrying out etherification reaction on phenol and dimethyl carbonate under the effect of a self-made catalyst; recycling methanol generated in a reaction process and the unreacted dimethyl carbonate by fractionation; after reaction is finished, separating and recycling a catalyst;and rectifying a coarse product to obtain an anisole product. By the process, the phenol can be transformed completely, the yield of the anisole reaches 99% or above, and the content of the anisole reaches up to 99.5% or above. The provided method has the environmentally friendly excellent characteristics of small toxicity of reaction raw materials, gentle reaction conditions, simple and speedy process, less waste water, waste gas and solid wastes and the like, and thus is suitable for industrial large-scale production.

Description

technical field [0001] The invention relates to a catalytic synthesis method of anisole, belonging to the technical field of organic synthesis. Background technique [0002] Anisole is also known as anisole, its English name is Anisole, its molecular formula is C7H8O, its relative molecular weight is 108.13, and it is a colorless liquid. Found naturally in the oil of tarragon, it has a pleasant anise-like aroma. For organic synthesis, also used as solvents, spices and insect repellants. The existing mature production technology is prepared by reacting dimethyl sulfate and phenol in alkaline solution. When synthesizing anisole, it is generally necessary to use highly toxic dimethyl sulfate, which has a high risk of damage to the human body and the production environment, and there is also a large amount of waste sulfate produced, which is extremely unfavorable to environmental protection. As the country pays more and more attention to environmental protection, the use of a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C41/16C07C43/205B01J31/02
CPCB01J31/0244B01J2231/40C07C41/16C07C43/205Y02P20/584
Inventor 侯光刘影刘军杨领军吴金江张长林黄泽祎张晓宇于旭东陶金辉陈宝昌韩韬
Owner 阜新汉道化工有限责任公司
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