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Preparation method of sulfolene

A technology of sulfolene and butadiene, which is applied in the field of preparation of sulfolene, can solve the problem of low conversion rate of butadiene, and achieve the goals of increasing conversion rate, stable and controllable preparation process, and optimizing reaction process Effect

Inactive Publication Date: 2019-05-17
PETROCHINA CO LTD
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Problems solved by technology

[0005] The main purpose of the present invention is to provide a kind of preparation method of sulfolene, to solve the problem that the conversion rate of butadiene is relatively low in the existing process of adopting continuous reaction to prepare sulfolene

Method used

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  • Preparation method of sulfolene

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[0023] As described in the background art, the existing process of preparing sulfolene by continuous reaction has the problem of low conversion rate of butadiene. In order to solve the above technical problems, the application provides a preparation method for synthesizing sulfolene. The preparation method includes: using butadiene and sulfur dioxide as reaction raw materials; A chelation reaction occurs in the device to obtain a crude sulfolene product, wherein along the flow direction of the reaction raw materials, the reaction temperature in each reaction device decreases successively; and the above-mentioned crude sulfolene product is purified to obtain sulfolene .

[0024] A kind of "chelation reaction" cycloaddition reaction. In this reaction, one atom of one reactant adds to the atoms at both ends of the conjugated system of the other reactant, forming two new σ bonds. The reaction substrate reduces a π bond, and the coordination number of the atom increases.

[0025...

Embodiment 1

[0054] use figure 1 The shown sulfolene preparation apparatus prepares sulfolene. SO in the reaction raw material 2 The molar ratio to butadiene is 1.2:1, and the raw material enters the first reaction device 11. The reaction pressure in the first reaction device 11 is 3.0MPa, the reaction temperature is 110°C, and the space velocity is 0.5h -1 . The reaction pressure in the second reaction device 12 is 1.8MPa, the reaction temperature is 85°C, and the space velocity is 0.5h -1 . The reaction pressure in the third reaction device 13 is 0.8MPa, the reaction temperature is 70°C, and the space velocity is 0.25h -1 . The sulfolene crude product is discharged from the sulfolene crude product outlet of the third reaction device 13, and it is transported to the flash unit 20, wherein the conversion rate of butadiene is 96.2%, and the sulfolene crude product SO 2 The concentration of butadiene is 17.91wt%, and the concentration of butadiene is 1.06wt%.

[0055] In the flash u...

Embodiment 2

[0061] The difference from Example 1 is: the SO in the reaction raw material passed into the first reaction device 2 The molar ratio to butadiene is 1.5:1. The conversion rate of butadiene in the third reaction device is 97.5%, and the SO in the crude product of sulfolene 2 The concentration was 25.3 wt%, and the butadiene concentration was 0.66 wt%. SO in the mixed gas material evaporated from the flash unit 20 2 The content of butadiene is 96.58wt%, and the content of butadiene is 2.58wt%. The sulfur dioxide content of the flash tower bottom material and the stripping tower bottom material is the same as in Example 1.

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Abstract

The invention provides a preparation method of sulfolene. The preparation method comprises the following steps: butadiene and sulfur dioxide are taken as reaction raw materials; the reaction raw materials are introduced into a plurality of reaction devices which are sequentially connected in series for chelation reaction, and a crude sulfolene product is obtained, wherein the reaction temperaturesin the reaction devices are reduced sequentially in the flow direction of the reaction raw materials; the crude sulfolene product is purified, and sulfolene is obtained. Sulfolene generated in the former reaction device can act as a diluent in the latter reaction device, and thus, the preparation process of sulfolene is more stable and controllable. Meanwhile, exothermic intensity of the continuous reaction process is about one tenth of the maximum exothermic intensity of the batch process, so that the reaction temperature can be controlled by adoption of the continuous reaction process. Synthesis of sulfolene is an exothermic reversible reaction, and the reaction temperatures in the three reaction devices are reduced sequentially, so that the conversion rate of the reaction raw materialsis increased, and the reaction process is optimized.

Description

technical field [0001] The invention relates to the field of organic synthesis, in particular to a preparation method of sulfolene. Background technique [0002] The first to apply for a patent for the synthesis of sulfolene was the German BASF company. Staudinger discovered that the effect of a polymerization inhibitor can synthesize sulfolene with high selectivity. With the emergence of pyrolysis technology, major petrochemical companies have applied for patents for the synthesis of sulfolene by mixing C4 and sulfur dioxide, but this reaction separation technology of conjugated dienes was eventually replaced by extractive distillation technology. [0003] With the emergence of natural gas desulfurization technology and aromatics separation technology using sulfolane as a solvent, the synthesis of sulfolane has become a prerequisite step for sulfolane production. Most of the existing sulfolene synthesis reactions are carried out in kettle-type batch reactions, but there ar...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D333/48
Inventor 张玉东宋立红田存轩伊东李华王家杰袁清国苗勇
Owner PETROCHINA CO LTD