Membrane decolorizing device for recovering acidizing fluid
By designing a decolorization device for recycling acidified liquid membranes, high-pressure nanofiltration membrane and filtration technology are used to remove impurities and pigments in the second mother liquor, the problems of unforming and acidification and centrifugation of the second mother liquor are solved, and the effects of reducing energy consumption, reducing COD emissions and increasing yields are achieved.
Patent Information
- Application Number
- CN202420586335.5
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2024-03-25
- Publication Date
- 2025-03-28
- Estimated Expiration
- 2034-03-25
AI Technical Summary
In the prior art, the second mother dry product is not formed, the yield is low, the third mother liquid waste discharge COD value is high, and the acidification and centrifugation are difficult, and the decolorization effect is poor.
A device for recycling acidified liquid membrane decolorization is designed to intercept impurities and pigments with molecular weight exceeding 1000 through high-pressure nanofiltration membrane, and combine bag filtration and 5μm microporous filtration to remove particles and decolorization of the acidified liquid.
The two-main crystallization and plate-frame filtration operation were abolished, which reduced energy consumption and COD emissions, improved yields, and significantly reduced the use of activated carbon.
Smart Images
Figure CN222677435U_ABST
Abstract
Description
Technical Field
[0001] The utility model relates to the technical field of synthetic production of raw material medicine vitamin C, in particular to a recycling acidified liquid membrane decolorization device. Background Art
[0002] The existing treatment process is to separate the second mother liquor through concentration and crystallization to obtain the second mother dry product for esterification, and the produced third mother liquor is discharged. The problems of the second mother dry product and esterification are as follows:
[0003] (1) Due to the high impurities and poor crystal form of the second master batch, the citric acid and impurities cannot be effectively separated by crystallization separation, resulting in the second master batch dry product being unformed and having a low yield. The COD value of the third master liquid discharged to the environment is high;
[0004] (2) The labor intensity of esterification of the second mother dry product is high, and the Vc-Na wet product produced by plate and frame filtration after adding alkali to the reaction is low in content and poor in quality.
[0005] Vc-Na wet product is acidified, and the problems due to the large number of impurities are as follows:
[0006] (1) Difficulty in acidification centrifugation: It is difficult to recover the acidified liquid and centrifuge it separately. The feed is small and the machine is frequently shaken. It can only be mixed with the genuine product and centrifuged, resulting in overall deviation in material quality.
[0007] (2) Too much activated carbon is used for decolorization and the effect is poor: the amount of carbon added to the recovered acidified liquid is more than 5 times that of the genuine product, and the decolorization effect is poor. Utility Model Content
[0008] In view of the above deficiencies in the prior art, the purpose of the utility model is to provide a membrane decolorization device for recovering acidified liquid, which reduces the energy consumption of the device, reduces COD emissions, and greatly improves the yield through improvements on the device.
[0009] The utility model is realized by adopting the following technical solutions:
[0010] The recycling acidified liquid membrane decolorization device comprises two mother liquid storage tanks, which are connected to a secondary microfilter through a primary filter, the secondary microfilter is connected to a concentration pot through a dialysate tank, the concentration pot is connected to a freezing tank through a primary esterification tank, the freezing tank is connected to a secondary acidification tank through a plate and frame filter press, and the secondary acidification tank is connected to a high-pressure nanofilter through a centrifuge.
[0011] The secondary microfilter is connected with a flushing water inlet pipeline, and the secondary microfilter is connected with a miscellaneous liquid collection tank through a pipeline.
[0012] The primary filter, the secondary microfilter, the dialysate tank and the miscellaneous liquid collection tank constitute a high-pressure nanofiltration membrane decolorization device.
[0013] The primary esterification tank is connected with a sodium carbonate inlet pipeline and a methanol inlet pipeline.
[0014] The secondary acidification tank is provided with an activated carbon feed port, and is connected with a dilute sulfuric acid pipeline and a methanol pipeline with water.
[0015] Between the secondary acidification tank and the centrifuge, there are bag filters and 5μm microporous filters. The filters contain nanofiltration membranes.
[0016] The lower part of the centrifuge is connected with a sodium carbonate outlet pipeline, and the lower part of the plate and frame filter press is provided with a mother liquor outlet pipeline.
[0017] The two ends of the high-pressure nanofilter are respectively connected with a high-concentration impurity pipeline and a deconcentration pipeline.
[0018] The working principle of the utility model is:
[0019] 1. The second mother liquor is decolorized by a high-pressure nanofiltration membrane to intercept impurities such as proteins and pigments with a molecular weight exceeding 1000. This device consists of a primary filter, a secondary micro-pass, a high-pressure pump, a high-pressure nanofiltration membrane group, a dialysate tank, and a miscellaneous liquid collection tank to purify the second mother liquor. 2. After the second mother liquor is purified, due to the improvement of quality, it is directly put into esterification after being concentrated to remove water, and the crystallization and plate and frame filter pressing operations are cancelled, shortening the process route, reducing energy consumption, reducing COD emissions, and improving the yield. 3. The recovery esterification operation adopts the method of distilling out methanol with water to reduce water and improve the yield and quality. 4. The second mother plate and frame increase the flow channel mother liquor separation and impurity removal device to improve the quality of the material entering the acidification. 5. The recovered acidified liquid produced by the acidification reaction is first filtered by bag filtration and 5μm microporous filtration to remove particles and impurities, and then enters the nanofiltration membrane through a high-pressure pump. Impurities and pigments in the recovered acidified liquid are retained by the nanofiltration membrane due to their large molecular weight, and substances with lower molecular weights such as Vc, methanol, and water pass through the nanofiltration membrane to achieve the purpose of decolorization of impurity pigments. The impurities and pigments in the retained liquid are concentrated and crystallized to recover the Vc because they contain materials, and the mother liquor is sold out. The dialysate after membrane decolorization directly enters the concentration process to produce vitamin C. The nanofiltration membrane is equipped with a backwash pump for online cleaning to extend the service life of the membrane group.
[0020] Compared with the prior art, the beneficial effects of the utility model are:
[0021] (1) The second mother crystallization and plate and frame filter pressing operations were cancelled, saving 200,000 kcal / h of power ice brine cooling capacity and 150,000 kWh of electricity per year; the plate and frame filter pressing of the second mother dry product was cancelled, saving 50,000 yuan in consumable filter cloth costs and 200,000 yuan in labor costs per year; the yield is expected to increase by 0.5%, with an annual benefit of 480,000 yuan.
[0022] (2) Membrane decolorization can greatly reduce the cost of activated carbon. The unit consumption of activated carbon is expected to drop from the current 30 kg per ton to 15 kg per ton, with an annual benefit of 7.35 million yuan. BRIEF DESCRIPTION OF THE DRAWINGS
[0023] Figure 1 This is a schematic diagram of the structure of the utility model's acidified liquid recovery membrane decolorization device;
[0024] In the figure: 1. Second mother liquor storage tank; 2. Primary filter; 3. Secondary microfilter; 4. Dialysate tank; 5. Miscellaneous liquid collection tank; 6. Concentrator; 7. Primary esterification tank; 8. Freezing tank; 9. Plate and frame filter press; 10. Secondary acidification tank; 11. Centrifuge; 12. High-pressure nanofilter; 13. Flushing water inlet pipeline; 14. Sodium carbonate inlet pipeline; 15. Methanol inlet pipeline; 16. Mother liquor outlet pipeline of filter press; 17. Dilute sulfuric acid pipeline; 18. Methanol with water pipeline; 19. Sodium carbonate outlet pipeline; 20. High-concentration impurity pipeline; 21. Deconcentration pipeline. DETAILED DESCRIPTION
[0025] In order to make the purpose and technical solution of the utility model more clear, the utility model is further described in detail below in conjunction with the accompanying drawings.
[0026] Example 1
[0027] like Figure 1 As shown, the membrane decolorization device for recovering acidified liquid includes two mother liquid storage tanks 1, which are connected to the secondary microfilter 3 through the primary filter 2, the secondary microfilter 3 is connected to the concentration pot 6 through the dialyzate tank 4, the concentration pot 6 is connected to the freezing pot 8 through the primary esterification tank 7, the freezing tank 8 is connected to the secondary acidification tank 10 through the plate-frame filter press 9, and the secondary acidification tank 10 is connected to the high-pressure nanofilter 12 through the centrifuge 11. The secondary microfilter 3 is connected to the flushing water inlet pipeline 13, and the secondary microfilter 3 is connected to the impurity collection tank 5 through the pipeline. The primary esterification tank 7 is connected to the sodium carbonate inlet pipeline 14 and the methanol inlet pipeline 15. The secondary acidification tank 10 is provided with an activated carbon feed port, and the secondary acidification tank 10 is connected with a dilute sulfuric acid pipeline 17 and a methanol pipeline with water 18. The lower part of the centrifuge 11 is connected with a sodium carbonate outlet device pipeline 19, and the lower part of the plate-frame filter press 9 is provided with a mother liquid outlet filter press pipeline 16. The two ends of the high-pressure nanofilter 12 are respectively connected to a high-concentration impurity pipeline 20 and a deconcentration pipeline 21. The recovered acidified liquid produced by the acidification reaction is first filtered by bag filter and 5μm microporous filtration to remove particles and impurities, and then enters the nanofiltration membrane through a high-pressure pump. Impurities and pigments in the recovered acidified liquid are retained by the nanofiltration membrane due to their large molecular weight, and substances with lower molecular weights such as Vc, methanol, and water pass through the nanofiltration membrane to achieve the purpose of decolorization of impurity pigments.
[0028] The above-mentioned recovery acidified liquid membrane decolorization device, when in operation, comprises the following steps:
[0029] (1) The second mother liquor is decolorized by a high-pressure nanofiltration membrane to intercept impurities such as proteins and pigments with a molecular weight exceeding 1000. This device is composed of a primary filter 2, a secondary microfilter 3, a high-pressure pump, a high-pressure nanofiltration membrane group, a dialysate tank 4, and a miscellaneous liquid collection tank 5 to achieve the purification of the second mother liquor; (2) After the second mother liquor is purified, the quality is improved and it is directly put into esterification after removing water by concentration; (3) The recovery esterification operation adopts the method of distilling out the methanol with water to reduce the water content and improve the yield and quality; (4) The second mother plate frame increases the flow channel mother liquor separation and impurity removal device to improve the quality of the material entering the acidification; (5) The recovered acidified liquid produced by the acidification reaction is first filtered through a bag filter and a 5μm microporous filter to remove particles and impurities, and then enters the nanofiltration membrane through a high-pressure pump. Impurities and pigments in the recovered acidified liquid are retained by the nanofiltration membrane due to their large molecular weight, while substances with lower molecular weight such as Vc, methanol, and water pass through the nanofiltration membrane to achieve the purpose of decolorization of impurities and pigments; the retained liquid containing impurities and pigments is concentrated and crystallized to recover Vc because it contains materials, and the mother liquor is sold out; the dialysate after membrane decolorization directly enters the concentration process to produce vitamin C; the nanofiltration membrane is equipped with a backwash pump for online cleaning to extend the service life of the membrane group.
Claims
1. A membrane decolorization device for recovering acidified liquid, characterized in that: The invention comprises two mother liquid storage tanks (1), wherein the two mother liquid storage tanks (1) are connected to a secondary microfilter (3) via a primary filter (2), the secondary microfilter (3) is connected to a concentration pot (6) via a dialysate tank (4), the concentration pot (6) is connected to a freezing tank (8) via a primary esterification tank (7), the freezing tank (8) is connected to a secondary acidification tank (10) via a plate and frame filter press (9), and the secondary acidification tank (10) is connected to a high-pressure nanofilter (12) via a centrifuge (11).
2. The membrane decolorization device for recovering acidified liquid according to claim 1, characterized in that: The secondary microfilter (3) is connected to a flushing water inlet pipeline (13), and the secondary microfilter (3) is connected to a miscellaneous liquid collection tank (5) via a pipeline.
3. The membrane decolorization device for recovering acidified liquid according to claim 1, characterized in that: The primary esterification tank (7) is connected to a sodium carbonate inlet pipeline (14) and a methanol inlet pipeline (15).
4. The membrane decolorization device for recovering acidified liquid according to claim 1, characterized in that: The secondary acidification tank (10) is provided with an activated carbon feed port, and the secondary acidification tank (10) is connected with a dilute sulfuric acid pipeline (17) and a methanol-with-water pipeline (18).
5. The membrane decolorization device for recovering acidified liquid according to claim 1, characterized in that: A sodium carbonate outlet pipe (19) is connected below the centrifuge (11), and a mother liquor outlet pipe (16) is provided below the plate-frame filter press (9).
6. The membrane decolorization device for recovering acidified liquid according to claim 1, characterized in that: The two ends of the high-pressure nanofilter (12) are respectively connected to a high-concentration impurity pipeline (20) and a deconcentration pipeline (21).