Intermediate organic impurity removing device for 1, 3-propane sultone production

By combining an intermediate material production vessel, a filter, and an ethanol solvent tank with vacuum distillation and ethanol washing, the problem of impurity removal in the production of 1,3-propanesulfonate lactone was solved, enabling the preparation of high-purity products that meet the high-purity requirements for lithium batteries.

CN224252816UActive Publication Date: 2026-05-19SHANDONG YONGHAO NEW MATERIAL TECH CO LTD
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Patent Information

Authority / Receiving Office
CN · China
Patent Type
Utility models(China)
Current Assignee / Owner
SHANDONG YONGHAO NEW MATERIAL TECH CO LTD
Filing Date
2025-06-11
Publication Date
2026-05-19

AI Technical Summary

Technical Problem

In the existing production process of 1,3-propanesulfonate lactone, it is difficult to efficiently remove organic impurities from intermediates, resulting in significant product losses and failing to meet the high purity requirements for lithium batteries.

Method used

The process involves using intermediate materials in a production vessel, filter, ethanol solvent tank, and related pipelines and stirring equipment. Salting out and separating impurities from sodium 3-hydroxypropane-1-sulfonate are achieved through vacuum distillation, ethanol washing, and hydrochloric acid treatment.

Benefits of technology

The purity of 1,3-propanesulfonate lactone was increased from 99.0% to over 99.95%, meeting the high purity requirements for lithium batteries and reducing product loss.

✦ Generated by Eureka AI based on patent content.

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Abstract

The utility model relates to the technical field of chemical reaction equipment, in particular to an intermediate organic impurity removal device for 1, 3-propane sultone production, which comprises an intermediate material production kettle and an ethanol solvent tank, and the bottom output end of the intermediate material production kettle is connected with the top of a filter through a pipeline. A filter screen is arranged at the lower part in the filter; a filter stirring paddle is connected in the filter; the top of the filter is connected with a nitrogen inlet line; and the bottom of the filter is connected with an ethanol receiving tank through a pipeline, and is also connected with a salt treatment pipeline and a distillation dehydration pipeline. After being deacidified, the intermediate treated by the device is esterified and cyclized to generate 1, 3PS, the 1, 3PS is distilled to obtain a crude product, and the purity is improved from 99.0 to more than 99.95.
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Description

Technical Field

[0001] This utility model relates to the field of chemical reaction equipment technology, specifically a device for removing organic impurities from intermediates used in the production of 1,3-propanesulfonate lactone. Background Technology

[0002] 1,3-Propanesulfonate lactone (hereinafter referred to as 1,3-PS) is an important chemical intermediate, mainly used as a surfactant, and also used in the formulation of cosmetics and as a pharmaceutical intermediate in the pharmaceutical industry. It is also used as a sulfonating agent in the synthesis of leather, inks and colorants. It is widely used in pharmaceutical and chemical industries, photosensitive materials, lithium batteries, biochemistry, textiles, lubrication, wastewater treatment, surface treatment and other industries.

[0003] In recent years, due to continuous technological advancements, the development scale of lithium batteries has grown significantly, and the use of 1,3-PS in lithium batteries has increased daily. It can improve the thermal stability and safety of lithium-ion batteries. The quality requirements for 1,3-PS used in batteries are extremely high: its content ≥99.90%, color number ≤30 (platinum-cobalt colorimetric), moisture ≤100ppm, acid value ≤100ppm, turbidity ≤10NTU, and sodium ion ≤20ppm. Only 1,3-PS that meets all these requirements can be used in lithium battery electrolytes.

[0004] Currently, in the production process of 1,3-PS, in order to obtain products that meet all the requirements, it is often necessary to go through a complicated refining and purification process, such as distillation and crystallization. Inevitably, a large amount of product is lost during the purification process. Utility Model Content

[0005] The technical problem to be solved by this utility model is to overcome the defects of the prior art and provide an intermediate organic impurity removal device for the production of 1,3-propanesulfonate lactone.

[0006] To solve the above-mentioned technical problems, this utility model provides the following technical solution:

[0007] An organic impurity removal device for intermediates in the production of 1,3-propanesulfonate lactone includes an intermediate material production vessel, the bottom output end of which is connected to the top of a filter via a pipeline, an ethanol solvent tank, the bottom output end of which is connected to the top of the filter via a pipeline, a filter screen is installed in the lower part of the filter, a filter stirring paddle is connected inside the filter, a nitrogen inlet is connected to the top of the filter, an ethanol receiving tank is connected to the bottom of the filter via a pipeline, and a salt treatment pipeline and a distillation dehydration pipeline are also connected to the bottom of the filter.

[0008] The above-mentioned structural operation process is as follows: the sodium 3-hydroxypropane-1-sulfonate solution is distilled and concentrated into a slurry through the intermediate material production kettle, and then sent to the filter. Ethanol solvent is then introduced into this slurry, and after stirring for a certain period of time, the sodium 3-hydroxypropane-1-sulfonate and ethanol solvent are separated, thus completing the "washing and impurity removal" process of sodium 3-hydroxypropane-1-sulfonate.

[0009] The bottom output end of the intermediate material production reactor is connected to the intermediate material feed pump via a pipeline, and the output end of the intermediate material feed pump is connected to the filter via a pipeline. The concentrated slurry in the intermediate material production reactor is transported into the filter by the intermediate material feed pump.

[0010] The bottom output of the ethanol solvent tank is connected to an ethanol feed pump via a pipeline, and the output of the ethanol feed pump is connected to a filter via a pipeline, so that the ethanol solvent is delivered to the filter by the ethanol feed pump.

[0011] The intermediate material production vessel is equipped with a stirring mechanism, and the intermediate material production vessel is capable of vacuum distillation of the internal materials.

[0012] The stirring mechanism includes a reaction stirring paddle and a reaction stirring motor.

[0013] The filter stirring paddle is connected to the filter stirring motor.

[0014] The beneficial effects achieved by this utility model are:

[0015] This invention provides an organic impurity removal device for intermediates used in the production of 1,3-propanesulfonate lactone. The intermediates processed by this device are deacidified, then esterified and cyclized to generate 1,3PS. Distillation yields the crude product, increasing the purity from 99.0% to over 99.95%. Attached Figure Description

[0016] The accompanying drawings are provided to further illustrate the present invention and form part of the specification. They are used together with the embodiments of the present invention to explain the present invention, but do not constitute a limitation thereof. In the drawings:

[0017] Figure 1 This is a schematic diagram of the structure of this utility model;

[0018] In the diagram: 1. Reaction stirring motor; 2. Intermediate material production vessel; 3. Ethanol solvent tank; 4. Intermediate feed pump; 5. Ethanol feed pump; 6. Filter stirring motor; 7. Filter; 8. Filter screen; 9. Distillation and dehydration pipeline; 10. Salt treatment pipeline; 11. Ethanol receiving tank. Detailed Implementation

[0019] The preferred embodiments of the present invention will be described below with reference to the accompanying drawings. It should be understood that the preferred embodiments described herein are for illustration and explanation only and are not intended to limit the present invention.

[0020] Example:

[0021] like Figure 1 As shown, an intermediate organic impurity removal device for the production of 1,3-propanesulfonate lactone includes an intermediate material production vessel 2, the bottom output end of which is connected to the top of a filter 7 via a pipe, and an ethanol solvent tank 3, the bottom output end of which is connected to the top of the filter 7 via a pipe.

[0022] A filter screen 8 is installed in the lower part of the filter 7. A filter stirring paddle is connected inside the filter 7, and the filter stirring paddle is connected to a filter stirring motor 6. A nitrogen inlet line is connected to the top of the filter 7, which supplies nitrogen (not shown in the attached figure) to the top of the filter 7 for pressure filtration. An ethanol receiving tank 11 is connected to the bottom of the filter 7 through a pipe. A salt treatment pipeline 10 and a distillation dehydration pipeline 9 are also connected to the bottom of the filter 7.

[0023] The bottom output end of the intermediate material production vessel 2 is connected to the intermediate material feed pump 4 through a pipeline, and the output end of the intermediate material feed pump 4 is connected to the filter 7 through a pipeline. The concentrated slurry in the intermediate material production vessel 2 is transported into the filter 7 by the intermediate material feed pump 4.

[0024] The bottom output end of the ethanol solvent tank 3 is connected to the ethanol feed pump 5 through a pipe, and the output end of the ethanol feed pump 5 is connected to the filter 7 through a pipe, so that the ethanol feed pump 5 delivers ethanol solvent to the filter 7.

[0025] The intermediate material production vessel 2 is equipped with a stirring mechanism, and the intermediate material production vessel 2 can perform vacuum distillation on the internal materials. Existing equipment with vacuum distillation function can be selected for the intermediate material production vessel 2.

[0026] The stirring mechanism includes a reaction stirring paddle and a reaction stirring motor 1.

[0027] This invention provides a device for removing organic impurities from the intermediate "sodium 3-hydroxypropane-1-sulfonate". The operation of the device includes the following steps:

[0028] In the production of 1,3PS, after the reaction of allyl alcohol and sodium bisulfite to produce sodium 3-hydroxypropane-1-sulfonate, an aqueous solution of sodium 3-hydroxypropane-1-sulfonate, i.e., the reaction solution, is obtained and is located in intermediate material production kettle 2. In intermediate material production kettle 2, 80% of the water is distilled off under reduced pressure.

[0029] The remaining slurry is conveyed to the filter 7 with stirring via the intermediate feed pump 4. During this process, the material needs to be continuously stirred in the intermediate material production vessel 2.

[0030] Ethanol is pumped from ethanol solvent tank 3 to filter 7 by ethanol feed pump 5. The intermediate sodium 3-hydroxypropane-1-sulfonate undergoes "salting out" in the presence of ethanol solvent and becomes a solid precipitate.

[0031] After the ethanol solvent and intermediate slurry are stirred in the stirred filter 7 for two hours, and after all the sodium 3-hydroxypropane-1-sulfonate has precipitated, the material is filtered by nitrogen pressure, and the filtrate enters the ethanol receiving tank 11 to remove impurities.

[0032] After filtration, hydrochloric acid aqueous solution is added to filter 7 through intermediate material production reactor 2. The concentration of hydrochloric acid aqueous solution is above 30%.

[0033] In filter 7, the intermediate sodium 3-hydroxypropane-1-sulfonate reacts with hydrochloric acid aqueous solution to generate 3-hydroxypropane-1-sulfonic acid, which dissolves in hydrochloric acid aqueous solution, and a certain amount of sodium chloride precipitates out.

[0034] The 3-hydroxypropane-1-sulfonic acid solution is filtered through nitrogen pressure and then filtered into distillation and dehydration line 9 for subsequent distillation and dehydration treatment.

[0035] After adding distilled water to intermediate material production reactor 2 to dissolve the precipitated sodium chloride, it is then pressurized with nitrogen and discharged to salt treatment pipeline 10 for subsequent sodium chloride salt treatment processes.

Claims

1. A device for removing organic impurities from intermediates used in the production of 1,3-propanesulfonate lactone, characterized in that, The system includes an intermediate material production vessel (2), the bottom output of which is connected to the top of a filter (7) via a pipe, and an ethanol solvent tank (3), the bottom output of which is connected to the top of a filter (7) via a pipe. A filter screen (8) is installed in the lower part of the filter (7). A filter stirring paddle is connected inside the filter (7). A nitrogen inlet line is connected to the top of the filter (7). An ethanol receiving tank (11) is connected to the bottom of the filter (7) via a pipe. A salt treatment pipeline (10) and a distillation and dehydration pipeline (9) are also connected to the bottom of the filter (7).

2. The apparatus for removing organic impurities from intermediates in the production of 1,3-propanesulfonate lactone according to claim 1, characterized in that, The bottom output end of the intermediate material production vessel (2) is connected to the intermediate feed pump (4) through a pipe, and the output end of the intermediate feed pump (4) is connected to the filter (7) through a pipe.

3. The apparatus for removing organic impurities from intermediates used in the production of 1,3-propanesulfonate lactone according to claim 1, characterized in that, The bottom output end of the ethanol solvent tank (3) is connected to the ethanol feed pump (5) through a pipe, and the output end of the ethanol feed pump (5) is connected to the filter (7) through a pipe.

4. The apparatus for removing organic impurities from intermediates in the production of 1,3-propanesulfonate lactone according to claim 1, characterized in that, The intermediate material production vessel (2) is equipped with a stirring mechanism, and the intermediate material production vessel (2) is capable of vacuum distillation of the internal materials.

5. The apparatus for removing organic impurities from intermediates in the production of 1,3-propanesulfonate lactone according to claim 4, characterized in that, The stirring mechanism includes a reaction stirring paddle and a reaction stirring motor (1).

6. The apparatus for removing organic impurities from intermediates used in the production of 1,3-propanesulfonate lactone according to claim 1, characterized in that, The filter stirring paddle is connected to the filter stirring motor (6).