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Sulfolene crystallization wastewater recovery method

A recovery method and sulfolene technology are applied in the field of recovery of sulfolene crystallization wastewater, which can solve the problems of unrecoverable sulfolene and waste of resources, and achieve the effects of inhibiting decomposition and making the reaction process safe.

Active Publication Date: 2019-01-01
PETROCHINA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The main purpose of the present invention is to provide a recovery method for sulfolene crystallization wastewater, to solve the problem that sulfolene in the existing sulfolene crystallization wastewater cannot be recycled, resulting in waste of resources

Method used

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  • Sulfolene crystallization wastewater recovery method
  • Sulfolene crystallization wastewater recovery method
  • Sulfolene crystallization wastewater recovery method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] Take 200g of sulfolene crystallization wastewater and place it in a 1000mL beaker, and use the chemical classification method to detect the content of sulfur dioxide and sulfolene in the wastewater. The test results showed that the sulfur dioxide content was 230ppm, and the sulfolene content was 18.5wt%.

[0041] Take by weighing 20g calcium carbonate and mix with above-mentioned sulfolane crystallization waste water, and constantly stir, feed air into above-mentioned crystallization waste water simultaneously, filter, obtain filtrate and filter residue, analyze the content of sulfur dioxide in the filtrate.

[0042] The above filtrate was mixed with sulfolene to prepare a sulfolene solution with a concentration of 60 wt%. Then, the above sulfolane solution was subjected to hydrogenation reaction at a reaction temperature of 55° C. and a reaction pressure of 3.0 MPa to obtain a crude sulfolane product. The content of sulfolene in the crude sulfolane product was analyze...

Embodiment 2

[0044] The difference with Example 1 is: change the calcium carbonate used to remove sulfur dioxide in waste water into barium carbonate. As a result, the sulfolene content in the crude product was 0.35%, and the recovery rate of sulfolene in the waste water was 98.1 wt%. The results are shown in Table 1.

Embodiment 3

[0046] The difference from Example 1 is: the calcium carbonate used to remove sulfur dioxide in the waste water is changed to barium carbonate, and the air introduced into the waste water is changed to oxygen. As a result, the content of sulfolene in the crude product was 0.26wt%, and the recovery rate of sulfolene in waste water was 98.6wt%. The results are shown in Table 1.

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Abstract

The invention provides a sulfolene crystallization wastewater recovery method, wherein sulfolene crystallization wastewater contains sulfur dioxide. The sulfolene crystallization wastewater recovery method comprises: carrying out a reaction on sulfolene crystallization wastewater and a carbonate to convert sulfur dioxide into a sulfite, wherein the carbonate is slightly soluble or insoluble in water; carrying out an oxidation reaction on the sulfite and an oxidant to obtain a sulfate precipitate and desulfurization wastewater; and dissolving sulfolene in the desulfurization wastewater, and carrying out a hydrogenation reaction to obtain sulfolane. According to the present invention, with the recovery method, sulfur dioxide in the wastewater can be effectively removed, and the used carbonate is the slightly soluble or insoluble compound, such that the reaction process is safe and stable, a large amount of heat cannot be released during the reaction so as to easily inhibit the decomposition of sulfolene, and the sulfolene in the wastewater is effectively recovered.

Description

technical field [0001] The invention relates to the field of recovery of sulfolene in industrial waste water, in particular to a recovery method of sulfolene crystallization waste water. Background technique [0002] Sulfolane is an essential intermediate for the industrial synthesis of green solvent sulfolane. Sulfolane is an excellent high temperature resistant, aprotic polar solvent, which is miscible with water, acetone, toluene, etc. It is an ideal solvent in the extraction process of aromatics. Sulfolane can also be used for acid gas purification and recovery, extraction and distillation solvents, polymer solvents and various reaction solvents. In addition, it is also used in paper industry, oil industry, electronics industry and textile industry. It is a widely used fine chemicals. [0003] There are many synthetic routes of sulfolene, and the relatively mature and only industrialized route is the Diels–Alder reaction of butadiene and sulfur dioxide to prepare sulfo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D333/48C02F1/58C02F103/36
CPCC02F1/58C02F2103/36C07D333/48
Inventor 袁清国张玉东孙士勇韩红霞刘瑛伊东李华王中平
Owner PETROCHINA CO LTD