CN219156794U - Malic acid edulcoration acid purification's device - Google Patents
Malic acid edulcoration acid purification's device Download PDFInfo
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- CN219156794U CN219156794U CN202223175575.6U CN202223175575U CN219156794U CN 219156794 U CN219156794 U CN 219156794U CN 202223175575 U CN202223175575 U CN 202223175575U CN 219156794 U CN219156794 U CN 219156794U
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Abstract
The utility model discloses a malic acid impurity removal acid purification device, which comprises a feeding zone, an after-adsorption washing zone, a regeneration washing zone, a fresh acid zone and a product recovery zone which are sequentially arranged, wherein the feeding zone is respectively provided with an anion exchange resin column; the material is malic acid in the material feeding area, and the material discharging area is connected with a product tank; the water washing area after adsorption is fed with water, and the discharging is connected with a product tank; the regeneration zone is also internally provided with an intermediate tank connected in series between adjacent columns, and the feed is dilute alkali solution; the feed of the regeneration water washing area is water; the feed of the inlet light acid zone is a dilute product, and the feed is reversed; the feeding of the product recovery area is the discharging of the water washing area after adsorption, the discharging is connected with a product tank, and the reverse feeding is performed; the device also comprises a control system and a distribution valve which is in butt joint with the anion exchange resin column, wherein the control system is connected with the distribution valve and controls the switching of the anion exchange resin column in each zone. The device reduces the production cost, simplifies the production method, shortens the production period and improves the total yield.
Description
Technical Field
The utility model relates to a malic acid impurity removal and purification technology, in particular to a malic acid impurity removal and purification device adopting a continuous fluid device and a separation technology.
Background
Malic acid, also known as 2-hydroxysuccinic acid, has two stereoisomers due to one asymmetric carbon atom in the molecule. In nature, there are three forms, namely D-malic acid, L-malic acid and their mixtures DL-malic acid. Malic acid is white crystal or crystalline powder, has strong hygroscopicity, is easy to dissolve in water and ethanol, and has special pleasant sour taste. The main application of the DL-malic acid can be divided into edible and non-edible aspects, and is mainly prepared by a chemical synthesis method, and the DL-malic acid solution obtained by the reaction contains some impurities such as maleic acid which does not completely react, isomerized fumaric acid, colored substances generated by side reaction, metal ions and the like besides the target product DL-malic acid. Therefore, the purification of the DL-malic acid solution is a key for influencing the quality of the product.
Disclosure of Invention
Aiming at the defects of complicated operation, low yield, high cost, large wastewater amount, and the like of the prior malic acid impurity removal by adopting a fixed bed, the utility model provides the malic acid impurity removal and purification device based on the continuous fluid separation device, so as to achieve the purposes of reducing the production cost, simplifying the production method, shortening the production period, and improving the total yield.
In order to achieve the above purpose, the present utility model adopts the following technical scheme:
the device comprises a feeding zone, an after-adsorption washing zone, a regeneration washing zone, a fresh acid zone and a product recovery zone which are sequentially arranged according to a circulation switching direction, wherein each zone comprises at least one anion exchange resin column;
the anion exchange resin column in the feeding area is fed with malic acid, and the discharging is connected with a product tank;
the anion exchange resin column of the water washing area after adsorption is an anion exchange resin column with the hetero acid adsorbed, and the feed of the water washing area after adsorption is water;
the anion exchange resin column in the regeneration zone is an anion exchange resin column which is subjected to water washing and is adsorbed with the mixed acid, the anion exchange resin columns in the regeneration zone are connected in series, an intermediate tank which is connected between the adjacent anion exchange resin columns in series is also arranged in the regeneration zone, and the feed of the regeneration zone is dilute alkali solution;
the anion exchange resin column of the regenerated water washing area is a regenerated anion exchange resin column, the feed of the regenerated water washing area is water, and the discharge of the regenerated water washing area is connected with the intermediate tank;
the anion exchange resin column of the inlet fade-out area is an anion exchange resin column which is subjected to regeneration water washing, the feed of the inlet fade-out area is a dilute product, and the inlet fade-out area is a reverse feed;
the anion exchange resin column of the product recovery zone is an anion exchange resin column subjected to light acid treatment, the feed of the product recovery zone is the discharge of the water washing zone after adsorption, and the discharge of the product recovery zone is connected with the product tank; the product recovery zone is fed in reverse;
the malic acid impurity removal acid purification device further comprises a control system and a distribution valve, wherein the distribution valve is in butt joint with the anion exchange resin column, and the control system is connected with the distribution valve and controls the switching of the anion exchange resin column in each zone.
The dilute product is used as the feed in the acid inlet area to directly wash out the water left in the resin column with the dilute product, so that the resin is fully expanded to prevent a large amount of heat from being released, and the ejected water can be recycled to the system.
Preferably, the anion exchange resin column is packed with a weakly basic macroporous anion exchange resin.
Preferably, the feed zone is provided with three sets of anion exchange resin columns connected in series, each set of anion exchange resin columns containing 2 anion exchange resin columns in parallel.
Preferably, the anion exchange resin columns in the post-adsorption water washing area, the regeneration water washing area and the regeneration area are all connected in series.
Preferably, the post-adsorption water washing zone contains 4 anion exchange resin columns, the regeneration zone contains 5 anion exchange resin columns, the regeneration water washing zone contains 4 anion exchange resin columns, the fresh acid zone contains 1 anion exchange resin column, and the product recovery zone contains 1 anion exchange resin column.
Preferably, in the regeneration zone, according to the flow direction of the liquid, the intermediate tank is connected with 2 anion exchange resin columns in series before and 3 anion exchange resin columns in series after.
Preferably, the dilute alkali solution is a dilute sodium hydroxide solution.
Preferably, the dilute alkali solution is sodium hydroxide solution with the mass fraction of 7%.
Preferably, the feed to the regeneration water wash zone is the discharge of the inlet fade-acid zone.
In the anion exchange resin column of the device designed by the utility model, the hetero acid ions and hydroxyl ions on the resin are exchanged, the effluent is a purified product, the exchanged resin sequentially enters a post-adsorption water washing area, a regeneration water washing area, a fresh acid area and a feeding area along with the switching of a system, and the regeneration area is subjected to the regeneration and activation of alkali, so that the regenerated resin reenters the feeding area to continuously purify malic acid.
The device designed by the utility model realizes each step of time-lapse exchange, water washing, regeneration and the like in the traditional production in a continuous production method, continuously feeds and continuously outputs products, and completely innovates the traditional fixed bed technology. Inside the continuous separation process: washing water, chemical reagents and the like are recycled in the system, and large intermediate tanks-batch-to-batch application of the traditional fixed bed method is not needed. Meanwhile, due to the continuous operation of the continuous fluid separation device, the fluid distribution valves are sequentially switched, and each separation unit sequentially pumps liquid with different media according to the method design, such as: raw materials, water, different chemical reagents, etc.
The device designed by the utility model replaces the traditional fixed bed purification process and has the advantages that:
(1) The sodium hydroxide consumption in the traditional fixed bed purification process is large, the utilization rate is low, and the device can reduce the cost.
(2) The device can continuously run, so that the components and the concentration of the product are kept stable, and the downstream working section is convenient to match.
(3) The device adopts the distributing valve to realize continuous production, the transfer tank and the matching are very small, the device is compact, the device is easy to be installed at any position, the device is easy to be matched with the old production process and device, and the occupied area is only about 10 percent of the same scale.
(4) The device can reduce the resin consumption by about 40 percent relative to a fixed bed system; the amount of wash water can be reduced by up to about 50%.
(5) The device can simultaneously remove or separate substances with different properties, thus simplifying the complex process.
(6) The rotating speed can be automatically adjusted according to the change of the mass and the flow of the flowing fluid according to the requirement of the production process; thus ensuring an economically optimal operation.
(7) The flow direction of the fluid may be coupled in a counter-current or co-current manner, depending on the convenience of the production process.
(8) Because a plurality of separation units are adopted, the production method flow can be flexibly changed.
Drawings
Fig. 1 is a schematic view of the structure of the device of example 1. Wherein # 1 to # 20 are anion exchange resin columns, and 21 is a middle tank. The direction of the arrow in the figure indicates the direction of liquid flow, and the direction of switching of the anion exchange resin column is from right to left in the figure.
Detailed Description
Example 1
The following is a detailed description of the embodiment in conjunction with fig. 1:
adopts a malic acid impurity-removing acid purifying device independently developed by the applicant, adopts weak-alkaline macroporous anion exchange resin, and has a design treatment capacity of 5.2m 3 And/h, the filling amount of each resin is 240L according to the characteristics of malic acid. The following segmentation areas are sequentially arranged according to the cyclic switching direction:
the device comprises a feeding zone, an after-adsorption water washing zone, a regeneration water washing zone, a fresh acid zone and a product recovery zone, wherein each zone comprises at least one anion exchange resin column;
the anion exchange resin column in the feeding area is fed with malic acid, and the discharging is connected with a product tank; through flow rate control, the raw materials firstly enter the columns of the zone through two groups of parallel pipelines, most of the mixed acid is adsorbed by the resin, and the other part of the mixed acid enters the columns connected in series at the back for re-adsorption, and the final product is discharged from the outlet of the zone, wherein the feeding speed is 5.2m 3 /h。
The anion exchange resin column of the water washing area after adsorption is an anion exchange resin column with the hetero acid adsorbed, the feed of the water washing area after adsorption is water, and the water inlet speed is 1.7m 3 /h。
The anion exchange resin column in the regeneration zone is an anion exchange resin column which is subjected to water washing and is adsorbed with hetero acid, the anion exchange resin columns in the regeneration zone are connected in series, an intermediate tank which is connected between the adjacent anion exchange resin columns in series is also arranged in the regeneration zone, the feed of the regeneration zone is dilute alkali solution, and the feed speed is 1m 3 /h。
The anion exchange resin column in the regeneration washing zone is a regenerated anion exchange resin column, the feed of the regeneration washing zone is water, and the discharge of the regeneration washing zone is connected with the intermediate tank. The acid remaining in the resin tank was washed with water and returned directly to the intermediate tank at a feed rate of 1.7m 3 /h。
The anion exchange resin column of the inlet fade-out area is an anion exchange resin column which is subjected to regeneration water washing, the feed of the inlet fade-out area is a dilute product, and the inlet fade-out area is a reverse feed;
the anion exchange resin column of the product recovery zone is an anion exchange resin column subjected to light acid treatment, the feed of the product recovery zone is the discharge of the water washing zone after adsorption, and the discharge of the product recovery zone is connected with the product tank; the product recovery zone is fed in reverse;
the dilute product is used as the feed in the acid inlet area to directly wash out the water left in the resin column with the dilute product, so that the resin is fully expanded to prevent a large amount of heat from being released, and the ejected water can be recycled to the system. The flow rate of the inlet light acid is 2m 3 /h。
The device for purifying the malic acid impurity removal acid further comprises a switching system, and the switching system controls the switching of the anion exchange resin column in each zone.
The anion exchange resin column is filled with a weak base macroporous anion exchange resin.
The feeding zone is provided with 6 anion exchange resin columns which are connected in parallel in pairs, and the three anion exchange resin columns are connected in series.
The anion exchange resin columns in the water washing area after adsorption, the regeneration water washing area and the regeneration area are all connected in series.
The dilute alkali solution is dilute sodium hydroxide solution.
The dilute alkali solution is sodium hydroxide solution with the mass fraction of 7%.
And the feeding of the regeneration water washing zone is the discharging of the inlet light acid zone.
The method comprises the following steps:
(1) Purity of the product
The device replaces the original fixed bed, the two process resin consumption and the produced wastewater and water consumption pair ratio are shown in table 1:
table 1 and Table 1 comparing production costs of conventional fixed bed Process
Two pairs of process product metrics are shown in table 2:
table 2 and Table 2 comparing product index of conventional fixed bed Process
As can be seen from the comparison, the index difference of the two devices relative to the raw material product is not large, but the resin consumption of the device is reduced by 43% compared with that of the original fixed bed, and the wastewater production is reduced by 59%.
Claims (9)
1. The device for purifying the malic acid impurity-removing acid is characterized by comprising a feeding zone, an adsorbed water washing zone, a regeneration zone, a regenerated water washing zone, a fresh acid zone and a product recovery zone which are sequentially arranged according to a circulation switching direction, wherein each zone comprises at least one anion exchange resin column;
the anion exchange resin column in the feeding area is fed with malic acid, and the discharging is connected with a product tank;
the anion exchange resin column of the water washing area after adsorption is an anion exchange resin column with the hetero acid adsorbed, and the feed of the water washing area after adsorption is water;
the anion exchange resin column in the regeneration zone is an anion exchange resin column which is subjected to water washing and is adsorbed with the mixed acid, the anion exchange resin columns in the regeneration zone are connected in series, an intermediate tank which is connected between the adjacent anion exchange resin columns in series is also arranged in the regeneration zone, and the feed of the regeneration zone is dilute alkali solution;
the anion exchange resin column of the regenerated water washing area is a regenerated anion exchange resin column, the feed of the regenerated water washing area is water, and the discharge of the regenerated water washing area is connected with the intermediate tank;
the anion exchange resin column of the inlet fade-out area is an anion exchange resin column which is subjected to regeneration water washing, the feed of the inlet fade-out area is a dilute product, and the inlet fade-out area is a reverse feed;
the anion exchange resin column of the product recovery zone is an anion exchange resin column subjected to light acid treatment, the feed of the product recovery zone is the discharge of the water washing zone after adsorption, and the discharge of the product recovery zone is connected with the product tank; the product recovery zone is fed in reverse;
the malic acid impurity removal acid purification device further comprises a control system and a distribution valve, wherein the distribution valve is in butt joint with the anion exchange resin column, and the control system is connected with the distribution valve and controls the switching of the anion exchange resin column in each zone.
2. The apparatus for purifying malic acid according to claim 1, wherein the anion exchange resin column is packed with a weakly basic macroporous anion exchange resin.
3. The apparatus for purifying malic acid according to claim 1, wherein the feed zone is provided with three groups of anion exchange resin columns connected in series, each group of anion exchange resin columns containing 2 anion exchange resin columns connected in parallel.
4. The apparatus for purifying malic acid according to claim 1, wherein the anion exchange resin columns in the post-adsorption washing zone, the regeneration washing zone and the regeneration zone are all connected in series.
5. The apparatus for purifying malic acid according to claim 4, wherein the post-adsorption washing zone comprises 4 anion exchange resin columns, the regeneration zone comprises 5 anion exchange resin columns, the regeneration washing zone comprises 4 anion exchange resin columns, the inlet acid zone comprises 1 anion exchange resin column, and the product recovery zone comprises 1 anion exchange resin column.
6. The apparatus for purifying a malic acid according to claim 5, wherein in the regeneration zone, 2 anion exchange resin columns are connected in series before the intermediate tank and 3 anion exchange resin columns are connected in series after the intermediate tank according to the flow direction of the liquid.
7. The apparatus for purifying malic acid according to claim 1, wherein the dilute alkali solution is a dilute sodium hydroxide solution.
8. The apparatus for purifying malic acid according to claim 7, wherein the diluted alkaline solution is a sodium hydroxide solution with a mass fraction of 7%.
9. The apparatus for purifying malic acid according to claim 1, wherein the feed to the regeneration water wash zone is the discharge from the inlet acid zone.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202223175575.6U CN219156794U (en) | 2022-11-29 | 2022-11-29 | Malic acid edulcoration acid purification's device |
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| CN202223175575.6U CN219156794U (en) | 2022-11-29 | 2022-11-29 | Malic acid edulcoration acid purification's device |
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| CN202223175575.6U Active CN219156794U (en) | 2022-11-29 | 2022-11-29 | Malic acid edulcoration acid purification's device |
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