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Method used for preparing diethyl sulfate

A technology of diethyl sulfate and sulfuric acid, which is applied in the chemical industry, can solve the problems of low reuse value and pollution, and achieve the effects of fast evaporation speed, increased yield, and large liquid evaporation area

Active Publication Date: 2015-07-15
TAIAN HAVAY CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Due to being heated in the kettle for a long time, the obtained waste sulfuric acid contains many carbonized substances, which makes this waste sulfuric acid a sticky brown shape, and the value of reuse is very low. Generally, it can only be discarded as waste, which will cause very polluted
Therefore, so far, there is no one in China that can prepare diethyl sulfate on a large scale.

Method used

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  • Method used for preparing diethyl sulfate
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  • Method used for preparing diethyl sulfate

Examples

Experimental program
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Effect test

Embodiment 1

[0035] 1) At room temperature, slowly drop 100 grams of 98% sulfuric acid into 92 grams of absolute ethanol, and stir for 30 minutes after the addition to obtain a pre-reaction mixture, which includes sulfuric acid, ethyl hydrogen sulfate, water, and ethanol ;

[0036] 2) figure 2 It is a process flow diagram for the preparation of diethyl sulfate. The pre-reaction liquid obtained in step 1) is added to the pre-reaction liquid dripping device 1, and enters the planar reaction section 2 in a laminar flow along the heating surface, and the planar reaction The A-A section of section 2 is a plane, such as image 3 As shown, the planar reaction section 2 maintains the temperature at 150-160°C, and the time for 1g of the pre-reaction liquid to flow through the heated planar reaction section is 0.5min. When the pre-reaction liquid flows through the planar reaction section 2, the pre-reaction Ethyl hydrogen sulfate in the liquid is continuously converted into diethyl sulfate, and d...

Embodiment 2

[0039] 1) 43 grams of ethylene are slowly passed into 75 grams of 98% sulfuric acid to obtain a reaction pre-reactant, which mainly contains diethyl sulfate, ethyl hydrogen sulfate and sulfuric acid in the reaction mixture;

[0040] 2) figure 2 It is a process flow diagram for the preparation of diethyl sulfate. The pre-reaction liquid obtained in step 1) is added to the pre-reaction liquid dripping device 1, and enters the planar reaction section 2 in a laminar flow along the heating surface, and the planar reaction The A-A section of section 2 is tubular, such as Figure 4 As shown, the planar reaction section 2 maintains the temperature at 145-155° C., and the time for 1 g of the pre-reaction solution to flow through the heated planar reaction section is 10 minutes. When the pre-reaction solution flows through the planar reaction section 2, the pre-reaction solution The ethyl hydrogen sulfate in the reaction system is continuously converted into diethyl sulfate, and dieth...

Embodiment 3

[0042] 1) At room temperature, slowly drop 100 grams of 98% sulfuric acid into 92 grams of absolute ethanol, and stir for 30 minutes after the addition to obtain a pre-reaction mixture, which includes sulfuric acid, ethyl hydrogen sulfate, water, and ethanol ;

[0043] 2) figure 2 It is a process flow diagram for the preparation of diethyl sulfate. The pre-reaction liquid obtained in step 1) is added to the pre-reaction liquid dripping device 1, and enters the planar reaction section 2 in a laminar flow along the heating surface, and the planar reaction The A-A section of section 2 is a plane, such as image 3 As shown, the planar reaction section 2 maintains the temperature at 130-150°C, and the time for 1g of the pre-reaction solution to flow through the heated planar reaction section is 4min. When the pre-reaction solution flows through the planar reaction section 2, the pre-reaction solution Ethyl hydrogen sulfate in the process is continuously converted into diethyl su...

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Abstract

The invention provides a method used for preparing diethyl sulfate. According to the method, a mixed solution containing ethyl hydrogen sulfate and / or diethyl sulfate is delivered through reaction distillation surface at a certain temperature, and at the same time, reduced pressure distillation is carried out, so that diethyl sulfate in the mixed solution and generated on the reaction distillation surface is separated rapidly, waste sulfuric acid in the mixed solution and generated on the reaction distillation surface is collected in a waste liquid collector, and ethanol is collected in a tail gas collector. Recycling of waste sulfuric acid and collected ethanol can be realized; the method is low in cost; and no waste acid is discharged.

Description

technical field [0001] The invention belongs to the field of chemical industry and relates to a novel method for preparing 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] There are many ways to prepare diethyl sulfate, and they can be summed up as follows: sulfuryl chloride-ethanol method, chlorosulfonic acid-ethanol method, ether-concentrated sulfuric acid method, sulfuryl chloride-ethanol-sodium chloride method, sulfuryl chloride-sulfuric acid method Sulfuryl chloride-ethanol method, sulfuric acid-ethylene method, sulfuric acid-ethanol method. Most of the above methods all need diethyl sulfate to be distilled out with underpressure distillation operation, and the ...

Claims

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Application Information

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IPC IPC(8): C07C305/08C07C303/24C07C303/44
Inventor 王加旺李贺存付俊
Owner TAIAN HAVAY CHEM
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