A device for recovering and processing mother liquor in a D-chiro-inositol preparation process
Patent Information
- Application Number
- CN202522530568.0
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2025-11-28
- Publication Date
- 2026-10-16
- Estimated Expiration
- 2035-11-28
AI Technical Summary
[0003]目前，D-手性肌醇制备过程中会产生大量的母液，其中约含乙醇40%、D-手性肌醇10%、肌醇4%、其他杂质5%，其余为水，目前多通过蒸馏回收乙醇，脱醇后的料液因杂质的影响，回收困难，导致原料的浪费，同时后期产生废水比较多导致环保压力大
[0015]This invention relates to a mother liquor recovery and treatment device in the preparation of D-chiral inositol, comprising a mother liquor tank, an outlet of which is connected via a pipeline to a dealcoholization tank, an outlet of which is connected via a pipeline to an acidification tank, an outlet of which is connected via a pipeline to a macroporous adsorption resin column, and an outlet of which is connected via a pipeline to a column chromatography tank; an outlet of which is connected via a pipeline to a first crystallization tank, an inlet of which is connected via a pipeline to a first ethanol tank, an outlet of which is connected via a pipeline to a first filter, an outlet of which is connected via a pipeline to a first filtrate tank, an outlet of which is connected via a pipeline to a second crystallization tank, an inlet of which is connected via a pipeline to a second ethanol tank, an outlet of which is connected via a pipeline to a second filter, and an outlet of which is connected via a pipeline to a crude D-chiral inositol tank. After the mother liquor enters the dealcoholization tank, a large amount of ethanol solvent is removed, avoiding interference from the solvent with subsequent acidification reactions and adsorption effects. The acidification tank adjusts the pH to convert acidic impurities in the mother liquor into easily adsorbable forms, while protecting the stability of the target product, D-chiral inositol. The macroporous adsorption resin column specifically adsorbs pigments, high molecular weight impurities, and some byproducts, achieving efficient separation of impurities from the target product. Finally, the column chromatography solution is stored in the column chromatography tank, providing a low-impurity, high-purity raw material base for subsequent crystallization processes. The entire series design avoids the risk of contamination caused by process interruptions, significantly reduces manual intervention, improves production continuity and automation, and provides a stable process foundation for large-scale production.
Smart Images
Figure CN224854223U_ABST
Abstract
Description
Technical Field
[0001] This utility model relates to the field of D-chiral inositol production technology, specifically to a device for recovering and treating mother liquor during the preparation of D-chiral inositol. Background Technology
[0002] D-Chiro Inositol (DCI) is one of the nine isomers of inositol that is optically active. It is also the bioactive isomer of vitamin B8. It exists in relatively high levels in buckwheat seeds, soybeans, and some insects, mostly in the form of methylated or glycosylated derivatives. It is a biodegradation product of buckwheat glycosides. It has insulin-sensitizing effects and promotes liver fat metabolism. It can significantly reduce blood glucose levels and has a significant therapeutic effect on diabetes.
[0003] Currently, the preparation of D-chiral inositol generates a large amount of mother liquor, which contains approximately 40% ethanol, 10% D-chiral inositol, 4% inositol, 5% other impurities, and the remainder is water. Ethanol is currently mostly recovered by distillation. However, the liquid after alcohol removal is difficult to recover due to the influence of impurities, resulting in waste of raw materials. At the same time, a large amount of wastewater is generated in the later stage, which puts great pressure on environmental protection. Summary of the Invention
[0004] The technical problem to be solved by this utility model is to provide a mother liquor recovery and treatment device in the preparation process of D-chiral inositol, which improves economic efficiency and is environmentally friendly, in order to address the shortcomings of the existing technology.
[0005] To solve the above-mentioned technical problems, the technical solution of this utility model is as follows:
[0006] A mother liquor recovery and treatment device in the preparation of D-chiral inositol includes a mother liquor tank, the outlet of which is connected to a dealcoholization tank via a pipeline, the outlet of which is connected to an acidification tank via a pipeline, the outlet of which is connected to a macroporous adsorption resin column via a pipeline, and the outlet of which is connected to a column chromatography tank via a pipeline.
[0007] The outlet of the column chromatography tank is connected to a first crystallization tank via a pipeline. The inlet of the first crystallization tank is connected to a first ethanol tank via a pipeline. The outlet of the first crystallization tank is connected to a first filter via a pipeline. The outlet of the first filter is connected to a first filtrate tank via a pipeline. The outlet of the first filtrate tank is connected to a second crystallization tank via a pipeline. The inlet of the second crystallization tank is connected to a second ethanol tank via a pipeline. The outlet of the second crystallization tank is connected to a second filter via a pipeline. The outlet of the second filter is connected to a crude D-chiral inositol tank via a pipeline.
[0008] As an improved technical solution, the top gas phase outlet of the dealcoholization tank is connected to an ethanol recovery tank via a pipeline.
[0009] As an improved technical solution, the inlet of the acidification tank is connected to a glacial acetic acid tank via a pipeline.
[0010] As an improved technical solution, the inlet of the macroporous adsorption resin column is connected to a third ethanol tank, a sodium hydroxide tank, and a deionized water tank via pipelines.
[0011] As an improved technical solution, the outlet of the column tank is connected to a concentration tank via a pipeline, and the outlet of the concentration tank is connected to the first crystallization tank via a pipeline.
[0012] As an improved technical solution, the outlet of the first filter is connected to a first filter cake tank via a pipeline, the outlet of the first filter cake tank is connected to a dissolving tank via a pipeline, the inlet of the dissolving tank is connected to a fourth ethanol tank via a pipeline, the outlet of the dissolving tank is connected to a third filter via a pipeline, the liquid phase outlet of the third filter is connected to a second filtrate tank via a pipeline, and the outlet of the second filtrate tank is connected to a second crystallization tank via a pipeline.
[0013] As a preferred technical solution, the solid phase outlet of the third filter is connected to an inositol recovery tank via a pipeline.
[0014] Due to the adoption of the above technical solution, the beneficial effects of this utility model are:
[0015] This invention relates to a mother liquor recovery and treatment device in the preparation of D-chiral inositol, comprising a mother liquor tank, an outlet of which is connected via a pipeline to a dealcoholization tank, an outlet of which is connected via a pipeline to an acidification tank, an outlet of which is connected via a pipeline to a macroporous adsorption resin column, and an outlet of which is connected via a pipeline to a column chromatography tank; an outlet of which is connected via a pipeline to a first crystallization tank, an inlet of which is connected via a pipeline to a first ethanol tank, an outlet of which is connected via a pipeline to a first filter, an outlet of which is connected via a pipeline to a first filtrate tank, an outlet of which is connected via a pipeline to a second crystallization tank, an inlet of which is connected via a pipeline to a second ethanol tank, an outlet of which is connected via a pipeline to a second filter, and an outlet of which is connected via a pipeline to a crude D-chiral inositol tank. After the mother liquor enters the dealcoholization tank, a large amount of ethanol solvent is removed, avoiding interference from the solvent with subsequent acidification reactions and adsorption effects. The acidification tank adjusts the pH to convert acidic impurities in the mother liquor into easily adsorbable forms, while protecting the stability of the target product, D-chiral inositol. The macroporous adsorption resin column specifically adsorbs pigments, high molecular weight impurities, and some byproducts, achieving efficient separation of impurities from the target product. Finally, the column chromatography solution is stored in the column chromatography tank, providing a low-impurity, high-purity raw material base for subsequent crystallization processes. The entire series design avoids the risk of contamination caused by process interruptions, significantly reduces manual intervention, improves production continuity and automation, and provides a stable process foundation for large-scale production.
[0016] The top vapor phase outlet of the dealcoholization tank of this invention is connected to an ethanol recovery tank via a pipeline. Utilizing the volatile nature of ethanol, the dealcoholization tank vaporizes the ethanol in the mother liquor through heating or pressure reduction. The vapor phase ethanol is then piped into the ethanol recovery tank, where it is condensed and separated to obtain high-purity recovered ethanol, which can be directly reused in crystallization, analysis, and other processes, thus saving costs.
[0017] The inlet of the acidification tank is connected to a glacial acetic acid tank via a pipeline. Glacial acetic acid, as a weak acid, has the characteristics of precise pH adjustment and mild reaction. By connecting the glacial acetic acid tank and the acidification tank through the pipeline, a metering pump can be used to achieve quantitative and uniform addition of glacial acetic acid, accurately controlling the pH value of the mother liquor to 3-4. This avoids incomplete adsorption of impurities due to excessively high pH values, or loss due to isomerization of D-chiral inositol caused by excessively low pH values. At the same time, glacial acetic acid reacts with alkaline impurities in the mother liquor to form water-soluble salts, which are easily removed in subsequent adsorption processes, further improving the purification effect of the mother liquor and ensuring the stability of subsequent processes and the consistency of product quality.
[0018] The inlet of the macroporous adsorption resin column is connected to a third ethanol tank, a sodium hydroxide tank, and a deionized water tank via pipelines. The macroporous adsorption resin column is first regenerated with ethanol, then with sodium hydroxide, and then washed with water until neutral before being fed. This process can more effectively adsorb impurities in the feed solution, resulting in more thorough regeneration and effectively increasing the service life of the resin.
[0019] The outlet of the column chromatography tank is connected to a concentration tank via a pipeline, and the outlet of the concentration tank is connected to the first crystallization tank via a pipeline. The concentration of D-chiral inositol in the column chromatography solution is low; direct crystallization would result in high solvent consumption, long crystallization time, and low yield. By adding a concentration tank between the column chromatography tank and the first crystallization tank, the column chromatography solution is concentrated to a solid content of 50% w / w, significantly increasing the concentration of the target product. During concentration, a small amount of residual low-boiling-point impurities can be further removed, improving the purity of the raw material. The concentrated solution enters the first crystallization tank, reducing the amount of ethanol solvent added, shortening the crystallization time, significantly improving production efficiency and unit equipment capacity, and reducing energy consumption and production costs.
[0020] The outlet of the first filter is connected to a first filter cake tank via a pipeline. The outlet of the first filter cake tank is connected to a dissolving tank via a pipeline. The inlet of the dissolving tank is connected to a fourth ethanol tank via a pipeline. The outlet of the dissolving tank is connected to a third filter via a pipeline. The liquid phase outlet of the third filter is connected to a second filtrate tank via a pipeline. The outlet of the second filtrate tank is connected to a second crystallization tank via a pipeline. Although the filter cake after the first crystallization filtration has a high purity, it still contains a small amount of impurities that have not been completely removed. Through this series design, the filter cake is first collected in the first filter cake tank to avoid the filter cake being exposed to air and absorbing moisture or becoming contaminated. Then, the filter cake is sent to the dissolving tank to completely dissolve it. It is then filtered through the third filter to remove the trace solid impurities that were not dissolved after dissolution. The filtered clear liquid enters the second crystallization tank for secondary crystallization and purification.
[0021] The solid phase outlet of the third filter is connected to an inositol recovery tank via a pipeline. The solid phase product of the third filter is mainly inositol, which can be recovered and reused for the conversion of chiral inositol, avoiding the waste of resources caused by discarding the target product with the filter residue, reducing production losses, and improving the overall economic benefits of the project. Attached Figure Description
[0022] The present invention will be further described below with reference to the accompanying drawings and embodiments.
[0023] Figure 1 This is a structural schematic diagram of an embodiment of the present utility model;
[0024] The tank consists of: 1. Mother liquor tank; 2. De-alcoholization tank; 3. Acidification tank; 4. Macroporous adsorption resin column; 5. Column buffer tank; 6. First crystallization tank; 7. First ethanol tank; 8. First filter; 9. First filtrate tank; 10. Second crystallization tank; 11. Second ethanol tank; 12. Second filter; 13. D-chiral inositol crude product tank; 14. Ethanol recovery tank; 15. Glacial acetic acid tank; 16. Third ethanol tank; 17. Sodium hydroxide tank; 18. Deionized water tank; 19. Concentration tank; 20. First filter cake tank; 21. Dissolving tank; 22. Third filter; 23. Second filtrate tank; 24. Inositol recovery tank; 25. Fourth ethanol tank. Detailed Implementation
[0025] The present invention will be further described below with reference to the accompanying drawings and embodiments.
[0026] like Figure 1 As shown, a mother liquor recovery and treatment device in the preparation of D-chiral inositol includes a mother liquor tank 1. The outlet of the mother liquor tank 1 is connected to a dealcoholization tank 2 via a pipeline. The outlet of the dealcoholization tank 2 is connected to an acidification tank 3 via a pipeline. The outlet of the acidification tank 3 is connected to a macroporous adsorption resin column 4 via a pipeline. The outlet of the macroporous adsorption resin column 4 is connected to a column chromatography tank 5 via a pipeline. The outlet of the column chromatography tank 5 is connected to a first crystallization tank 6 via a pipeline. The inlet of the first crystallization tank 6 is connected to a first ethanol tank 7 via a pipeline. The outlet of the first crystallization tank 6 is connected to a first filter 8 via a pipeline. The outlet of the first filter 8 is connected to a first filtrate tank 9 via a pipeline. The outlet of the first filtrate tank 9 is connected to a second crystallization tank 10 via a pipeline. The inlet of the second crystallization tank 10 is connected to a second ethanol tank 11 via a pipeline. The outlet of the second crystallization tank 10 is connected to a second filter 12 via a pipeline. The outlet of the second filter 12 is connected to a crude D-chiral inositol tank 13 via a pipeline. After the mother liquor enters the dealcoholization tank 2, a large amount of ethanol solvent is removed, avoiding interference from the solvent with subsequent acidification reactions and adsorption effects. The acidification tank 3 adjusts the pH to convert acidic impurities in the mother liquor into easily adsorbable forms, while simultaneously protecting the stability of the target product, D-chiral inositol. The macroporous adsorption resin column 4 specifically adsorbs pigments, high-molecular-weight impurities, and some byproducts, achieving efficient separation of impurities from the target product. Finally, the column chromatography solution is stored in the column chromatography solution tank 5, providing a low-impurity, high-purity raw material base for subsequent crystallization processes. This series design avoids the risk of contamination caused by process interruptions, significantly reduces manual intervention, improves production continuity and automation, and provides a stable process foundation for large-scale production.
[0027] The top vapor outlet of the dealcoholization tank 2 is connected to the ethanol recovery tank 14 via a pipeline. Taking advantage of the volatile nature of ethanol, the dealcoholization tank 2 vaporizes the ethanol in the mother liquor by heating or reducing pressure. The vapor ethanol is then introduced into the ethanol recovery tank 14 via a pipeline. After condensation and separation, high-purity recovered ethanol is obtained, which can be directly reused in crystallization, analysis and other processes, saving costs.
[0028] The inlet of the acidification tank 3 is connected to the glacial acetic acid tank 15 via a pipeline. Glacial acetic acid, as a weak acid, has the characteristics of precise pH adjustment and mild reaction. By connecting the glacial acetic acid tank 15 to the acidification tank 3 via a pipeline, the metering pump can be used to achieve quantitative and uniform addition of glacial acetic acid, accurately controlling the pH value of the mother liquor to 3-4. This avoids incomplete adsorption of impurities due to excessively high pH value, or loss due to isomerization reaction of D-chiral inositol caused by excessively low pH value. At the same time, glacial acetic acid reacts with alkaline impurities in the mother liquor to form water-soluble salts, which are easily removed in subsequent adsorption processes, further improving the purification effect of the mother liquor and ensuring the stability of subsequent processes and the consistency of product quality.
[0029] The inlet of the macroporous adsorption resin column 4 is connected to a third ethanol tank 16, a sodium hydroxide tank 17, and a deionized water tank 18 via pipelines. The macroporous adsorption resin column 4 is first regenerated with ethanol, then with sodium hydroxide, and then washed with water until neutral before being fed. This process can more effectively adsorb impurities in the feed solution, resulting in more thorough regeneration and effectively increasing the service life of the resin.
[0030] The outlet of the column chromatography tank 5 is connected to a concentration tank 19 via a pipeline, and the outlet of the concentration tank 19 is connected to the first crystallization tank 6 via a pipeline. The concentration of D-chiral inositol in the column chromatography solution is low; direct crystallization would result in high solvent consumption, long crystallization time, and low yield. By adding a concentration tank 19 between the column chromatography tank 5 and the first crystallization tank 6, the column chromatography solution is concentrated to a solid content of 50% w / w, significantly increasing the concentration of the target product. During concentration, a small amount of residual low-boiling-point impurities can be further removed, improving the purity of the raw materials. The concentrated solution enters the first crystallization tank 6, reducing the amount of ethanol solvent added, shortening the crystallization time, significantly improving production efficiency and unit equipment capacity, and reducing energy consumption and production costs.
[0031] The outlet of the first filter 8 is connected to a first filter cake tank 20 via a pipe. The outlet of the first filter cake tank 20 is connected to a dissolving tank 21 via a pipe. The inlet of the dissolving tank 21 is connected to a fourth ethanol tank 25 via a pipe. The outlet of the dissolving tank 21 is connected to a third filter 22 via a pipe. The liquid phase outlet of the third filter 22 is connected to a second filtrate tank 23 via a pipe. The outlet of the second filtrate tank 23 is connected to a second crystallization tank 10 via a pipe. Although the filter cake after the first crystallization filtration has a high purity, it still contains a small amount of impurities that have not been completely removed. Through this series design, the filter cake is first collected in the first filter cake tank 20 to avoid the filter cake being exposed to air and absorbing moisture or becoming contaminated. Then, the filter cake is sent to the dissolving tank 21 to completely dissolve the filter cake. It is then filtered through the third filter 22 to remove the trace solid impurities that were not dissolved after dissolution. The filtered clear liquid enters the second crystallization tank 10 for secondary crystallization and purification.
[0032] The solid phase outlet of the third filter 22 is connected to an inositol recovery tank 24 via a pipeline. The solid phase product of the third filter 22 is mainly inositol, which can be recycled for the conversion of chiral inositol after recovery, avoiding the waste of resources caused by discarding the target product with the filter residue, reducing production losses, and improving the overall economic benefits of the project.
[0033] It should be understood that these embodiments are for illustrative purposes only and are not intended to limit the scope of the present invention. Furthermore, it should be understood that after reading the teachings of this invention, those skilled in the art can make various alterations or modifications to the invention, and these equivalent forms also fall within the scope defined by the appended claims.
Claims
1. A device for recovering and processing mother liquor during the preparation of D-chiral inositol, comprising a mother liquor tank, characterized in that: The outlet of the mother liquor tank is connected to a dealcoholization tank via a pipeline, the outlet of the dealcoholization tank is connected to an acidification tank via a pipeline, the outlet of the acidification tank is connected to a macroporous adsorption resin column via a pipeline, and the outlet of the macroporous adsorption resin column is connected to a column chromatography tank via a pipeline. The outlet of the column chromatography tank is connected to a first crystallization tank via a pipeline. The inlet of the first crystallization tank is connected to a first ethanol tank via a pipeline. The outlet of the first crystallization tank is connected to a first filter via a pipeline. The outlet of the first filter is connected to a first filtrate tank via a pipeline. The outlet of the first filtrate tank is connected to a second crystallization tank via a pipeline. The inlet of the second crystallization tank is connected to a second ethanol tank via a pipeline. The outlet of the second crystallization tank is connected to a second filter via a pipeline. The outlet of the second filter is connected to a crude D-chiral inositol tank via a pipeline.
2. The mother liquor recovery and treatment device in the preparation process of D-chiral inositol as described in claim 1, characterized in that: The top gas phase outlet of the dealcoholization tank is connected to an ethanol recovery tank via a pipeline.
3. The mother liquor recovery and treatment device in the preparation process of D-chiral inositol as described in claim 1, characterized in that: The inlet of the acidification tank is connected to a glacial acetic acid tank via a pipe.
4. The mother liquor recovery and treatment device in the preparation process of D-chiral inositol as described in claim 1, characterized in that: The inlet of the macroporous adsorption resin column is connected to a third ethanol tank, a sodium hydroxide tank, and a deionized water tank via pipes.
5. The mother liquor recovery and treatment device in the preparation process of D-chiral inositol as described in claim 1, characterized in that: The outlet of the column chromatography tank is connected to a concentration tank via a pipeline, and the outlet of the concentration tank is connected to the first crystallization tank via a pipeline.
6. The mother liquor recovery and treatment device in the preparation process of D-chiral inositol as described in claim 1, characterized in that: The outlet of the first filter is connected to a first filter cake tank via a pipe. The outlet of the first filter cake tank is connected to a dissolving tank via a pipe. The inlet of the dissolving tank is connected to a fourth ethanol tank via a pipe. The outlet of the dissolving tank is connected to a third filter via a pipe. The liquid phase outlet of the third filter is connected to a second filtrate tank via a pipe. The outlet of the second filtrate tank is connected to a second crystallization tank via a pipe.
7. The mother liquor recovery and treatment device in the preparation process of D-chiral inositol as described in claim 6, characterized in that: The solid phase outlet of the third filter is connected to an inositol recovery tank via a pipeline.