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Environmentally-friendly diethyl sulfate production process,

A diethyl sulfate, green production technology, applied in the direction of sulfuric acid ester preparation, organic compound preparation, chemical instruments and methods, etc., can solve the problem of inability to realize large-scale production of diethyl sulfate, low yield, large sodium sulfate and other problems, to achieve the effect of easy industrial production, lower production cost, and low production cost

Pending Publication Date: 2020-01-03
TAIAN HAVAY CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method needs too much amount of sodium sulfate, can't stir in the whole reaction, distillation process, only relies on sodium sulfate solid heat transfer, and heat is accumulated locally, and yield is not high, and a few grams or tens of grams of diethyl sulfate are prepared at a time. It is barely possible, but the large-scale production of diethyl sulfate cannot be realized

Method used

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  • Environmentally-friendly diethyl sulfate production process,

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Add 1000g of diethyl sulfate intermediate in the three-necked flask, and add 880g of anhydrous sodium sulfate; under stirring conditions, the temperature in the bottle is raised to 80°C for 4 hours; the temperature in the bottle is raised to 100°C, and the reaction is for 8 hours; Put the flask into cold water and cool down to 0°C in the bottle; add 900g of water at a temperature of 10°C and stir to dissolve. After all the dissolution in the bottle, let stand and separate the liquids to obtain 398.1g of the upper ester phase (crude diethyl sulfate); the crude product After re-distillation, 382.2 g of diethyl sulfate was obtained, with a yield of 68.5% (calculated as ethanol). The purity was 99.82% as detected by gas chromatography.

Embodiment 2

[0026] Add 50kg of diethyl sulfate intermediate in the reaction kettle, add 22kg of anhydrous sodium sulfate; under the condition of stirring, the temperature in the kettle is raised to 60°C for 2 hours; the temperature in the kettle is raised to 90°C, and the reaction is for 2 hours; ℃, react for 2 hours; after the reaction is completed, cool to 20 ℃ in the kettle; add 60 kg of water with a temperature of 5 ℃ and stir to dissolve, and after all the dissolution in the kettle, stand still and separate liquids to obtain 20.78 kg of the upper ester phase; the obtained ester After phase distillation, 19.95kg of diethyl sulfate was obtained, with a yield of 71.5% (in terms of ethanol), and detected by gas chromatography, the purity was 99.76%.

Embodiment 3

[0028] Add 2000kg of diethyl sulfate intermediate in the reaction kettle, add 700kg of anhydrous sodium sulfate; under stirring conditions, the temperature in the kettle is raised to 90°C for 2 hours; the temperature in the kettle is raised to 130°C, and the reaction is for 2 hours; after the reaction is completed, cool to 50°C in the kettle; add 3,000kg of water at a temperature of 10°C and stir to dissolve, and after all the dissolution in the kettle, stand still and separate liquids to obtain 785.8kg of the upper ester phase; obtain 754.4kg of diethyl sulfate after distillation of the obtained ester phase, The yield is 67.6% (calculated as ethanol), and the purity is 99.84% as detected by gas chromatography.

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Abstract

The invention belongs to the field of chemical synthesis, and specially relates to an environmentally-friendly diethyl sulfate production process, which comprises: carrying out a reaction on a diethylsulfate intermediate (ethyl hydrogen sulfate or a mixture containing ethyl hydrogen sulfate) and sulfate or hydrochloride for 4-12 h at a temperature of 60-130 DEG C to generate a mixture of diethylsulfate and disulfate, cooling the mixture, dissolving with water, separating to obtain a disulfate solution and a diethyl sulfate crude product, and refining the diethyl sulfate crude product to obtain diethyl sulfate. According to the process of the invention, the reactants cannot be carbonized in the reaction process, the waste acid difficultly recycled is not generated, the product quality ishigh, the industrial production is easy to realize, and the process is an environmentally-friendly diethyl sulfate production process.

Description

technical field [0001] The invention belongs to the field of chemical synthesis, and in particular relates to a green production process of diethyl sulfate. Background technique [0002] Diethyl sulfate is an important ethylating reagent, and also an important intermediate in organic chemical industry, pesticide, pharmaceutical and other industries. Due to its high boiling point, high pressure is not required for the ethylation reaction, so it can be used as an ideal ethylating reagent. [0003] According to the literature ([1] Li Zhongming. Synthesis of diethyl sulfate [J]. Hubei Chemical Industry, 1997 (01): 31-32, [2] Zhu Jianjun, Feng Lei, Lu Hongwen. Synthesis of diethyl sulfate [J] .Chemical Design, 1994(02):43-45+51, [3] Wu Zhiguang, Zou Zhichen, Huang Ruqi. Study on the Synthesis of Diethyl Sulfate[J]. Chemical Reagents, 1991(03):190+144, [4 ] Yang Qinglin. Synthesis of diethyl sulfate by sulfuric acid-ethanol method [J]. Liaoning Chemical Industry, 1991 (01): 22-2...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C303/24C07C303/44C07C305/08
CPCC07C303/24C07C303/44C07C305/08
Inventor 孙桂彬张荣楠李贺存胡蕾张学德边炳辉王家旺
Owner TAIAN HAVAY CHEM
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