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Synthesis process of methylparaben

A technology for the synthesis of methyl paraben esters, which is applied in the preparation of carboxylic acid esters, the preparation of organic compounds, and organic chemistry. It can solve problems such as poor product quality, long reaction time, and waste liquid corrosion of equipment, and achieve stable properties. , Simple operation, short time-consuming effect

Inactive Publication Date: 2013-04-10
魏晓婧
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  • Abstract
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Problems solved by technology

[0007] The synthesis of parabens is usually based on concentrated sulfuric acid as a catalyst and esterification of alcohol and p-hydroxybenzoic acid as raw materials. This method has the disadvantages of poor product quality, difficult product separation, waste liquid corrosion equipment, and environmental pollution.
In recent years, there has been a method of catalyzing the synthesis of solid superacids and insoluble heteropolyacids, but the preparation of catalysts in this method is complicated and the reaction time is long

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  • Synthesis process of methylparaben
  • Synthesis process of methylparaben
  • Synthesis process of methylparaben

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Embodiment Construction

[0017] The process steps of the present invention are: adding p-hydroxybenzoic acid and methanol with a molar ratio of 1: 1.5 to 1: 4.0 in a round bottom flask, and then adding 0.1 to 0.6 g / g of catalyst sodium bisulfate; placing the flask in a cavity of a microwave oven In the process, the flask is connected to the external stirring and water separating and condensing device through the three-port connecting pipe placed at the hole on the top of the microwave oven; preheat to dissolve the raw materials, and after the dissolution, adjust the microwave output power to 450W to continue heating. When the water separator starts Start timing when the distillate appears; after reacting for 3 to 18 minutes, pour out the reaction solution, and the catalyst remains in the flask as a solid; distill the reaction solution to remove excess methanol, and pour 5% sodium bicarbonate into it while it is hot Aqueous solution, the ester is separated from the water; the crude ester is obtained by ...

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Abstract

The invention relates to a synthesis process of food preservative, and in particular relates to a synthesis process of methylparaben. The synthesis process of methylparaben is simple in operation, short in time consumption and low in pollution. The synthesis process comprises the steps of: adding p-hydroxybenzoic acid and methanol into a round-bottom flask according to the molar ratio of (1: 1.5)-(1: 4.0), and then adding 0.1-0.6g / g of catalyst sodium hydrogen sulfate into the mixture; putting the round-bottom flask into a microwave oven; preheating to dissolve the raw materials, adjusting the microwave output power to 450W after dissolving and further heating; timing when distillate appears in a water separator; carrying out reaction for 3-18minuest, then pouring out reaction liquid, and leaving the catalyst in a solid state in the round-bottom flask; distilling the reaction liquid, evaporating out excessive methanol, pouring 5% of sodium hydrogen carbonate while hot, and separating out ester from water; and filtering, washing and drying to obtain the finished product.

Description

Technical field: [0001] The present invention relates to a kind of synthesis technique of food preservative, more specifically, relate to the synthesis technique of methylparaben. Background technique: [0002] Methylparaben, also known as methyl p-hydroxybenzoate, the molecular formula is C 8 h 8 o 3 , the structural formula is shown in the figure below. [0003] [0004] Methylparaben [0005] Paraben is an internationally recognized broad-spectrum high-efficiency food preservative. The United States, Europe, Japan, Canada, South Korea, Russia and other countries allow paraben to be used in food. It is widely used in condiments such as soy sauce and vinegar, pickled products, baked food, sauce products, beverages, rice wine, and preservation of fruits and vegetables. my country's GB2760 stipulates that ethylparaben, propylparaben and sodium methylparaben, sodium ethylparaben and sodium propylparaben can be used as food preservatives. [0006] Due to its phenolic h...

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Application Information

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IPC IPC(8): C07C69/84C07C67/08
Inventor 魏晓婧
Owner 魏晓婧
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