CN108358774B - Method and apparatus for multiple recovery of components using pervaporation-crystallization coupling - Google Patents

Method and apparatus for multiple recovery of components using pervaporation-crystallization coupling Download PDF

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CN108358774B
CN108358774B CN201810029101.XA CN201810029101A CN108358774B CN 108358774 B CN108358774 B CN 108358774B CN 201810029101 A CN201810029101 A CN 201810029101A CN 108358774 B CN108358774 B CN 108358774B
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crystallization
raw material
liquid
pervaporation
membrane
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CN108358774A (en
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李砚硕
陈晨
吴大朋
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Ningbo University
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Ningbo University
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    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C51/00Preparation of carboxylic acids or their salts, halides or anhydrides
    • C07C51/42Separation; Purification; Stabilisation; Use of additives

Abstract

The invention discloses a method and a device for recovering components in multiple ways by utilizing pervaporation-crystallization coupling, wherein the method comprises the following steps: heating the raw material liquid to the pervaporation temperature, introducing the raw material liquid into a pervaporation membrane separation unit, and enriching the raw material liquid into a permeate on the downstream side of a membrane by a separation membrane which is selectively penetrated by one component in the recovered solvent; the retentate on the upstream side of the membrane is introduced into a crystallization unit, and after crystallization, crystals and a raffinate are obtained by solid-liquid separation. By utilizing the device and the method for recycling the industrial waste liquid, disclosed by the invention, a plurality of components in the industrial waste liquid can be effectively recycled, the waste of products with high added values is avoided, the cost for processing a large amount of waste liquid and purchasing a new solvent is saved, and great economic benefits are generated.

Description

Method and apparatus for multiple recovery of components using pervaporation-crystallization coupling
Technical Field
The invention relates to solvent recovery treatment and cyclic application, in particular to the recovery treatment and utilization of a solvent to be recovered, which is subjected to fine chemical and pharmaceutical production by an alcohol precipitation process and also contains a crystallizable component. Belongs to the technical field of environmental protection.
Background
The water extraction and alcohol precipitation method (water-alcohol method) is a method in which ethanol is added into a concentrated water extraction solution of traditional Chinese medicines or a product water solution obtained by a chemical synthesis method to make the alcohol content different, the solubility of some product compositions in an alcohol solution is reduced, precipitate is separated out, and solid-liquid separation is carried out to obtain the product. Generally, the solvent to be recovered obtained by solid-liquid separation is subjected to separation of alcohol and water by a conventional rectification process or the like, so as to recover the alcohol solvent. However, the solvent to be recovered still contains some crystallizable active components, so that the direct rectification treatment loses this part of the product. If the water content in the solvent to be recovered can be reduced at a lower temperature (lower than the heat-resistant temperature of the effective component), the effective component can be caused to continue to crystallize, thereby achieving its recovery.
Take sodium pyruvate production as an example. Sodium pyruvate is the most common pyruvate, namely sodium pyroglutamate and 2-carbonyl sodium propionate, is an endogenous small molecular substance, naturally exists in human bodies, and participates in the metabolism of all tissues and organs of the whole body. The sodium pyruvate has wide application in the fields of medicine, diagnostic reagents and medical instruments and has extremely high market value.
In the prior art, the method for industrially producing sodium pyruvate mainly adopts pyruvic acid as a raw material, and the pyruvic acid reacts with alkaline substances such as sodium hydroxide or sodium bicarbonate to prepare sodium pyruvate, and the sodium pyruvate is further crystallized by an alcohol precipitation method to obtain high-purity sodium pyruvate. In the production process, centrifugal mother liquor obtained after centrifugal separation of sodium pyruvate crystals is used as a solvent to be recovered for rectification treatment. The centrifugal mother liquor contains about 75-90% of alcohol and 10-25% of water. The solubility of sodium pyruvate in water was 47g/100g water at room temperature. As such, the rectification treatment of the centrifugal mother liquor causes a great amount of sodium pyruvate loss, greatly increases the production cost and causes the waste of social resources. In addition, the distillation and recovery of the solvent are also very difficult due to the complex components in the waste liquid.
Based on the current situation, a comprehensive treatment scheme aiming at the mixed solution with complex components is expected to be found so as to establish a more efficient and economic production flow and realize the sustainable output of environmental protection.
Disclosure of Invention
The object of the present invention is to provide an integrated process scheme for industrial solvents to be recovered with complex composition, by which efficient recovery of various components in the solvent to be recovered is expected to be achieved in a compact and efficient manner.
First, the present invention discloses a method for recovering components in multiple ways by using pervaporation-crystallization coupling, which comprises the following steps: heating the raw material liquid to the pervaporation temperature, introducing the raw material liquid into a pervaporation membrane separation unit, and enriching the raw material liquid into a permeate on the downstream side of a membrane by a separation membrane which is selectively penetrated by one component in the recovered solvent; the retentate on the upstream side of the membrane is introduced into a crystallization unit, and after crystallization (cooling to a crystallization temperature to precipitate crystals) is subjected to solid-liquid separation to obtain crystals and a crystallization raffinate.
Secondly, the invention discloses a device for recovering components by multiple coupling of pervaporation and crystallization, which comprises a heating unit (1), a pervaporation separation membrane unit (2) and a crystallization unit (3);
the heating unit (1) heats the raw material liquid to the pervaporation temperature;
the pervaporation membrane unit (2) receives the heated raw material liquid and separates the raw material liquid into a permeate and a retentate;
the crystallization unit (3) receives a retentate.
By utilizing the device and the method for recycling the industrial waste liquid, disclosed by the invention, a plurality of components in the industrial waste liquid can be effectively recycled, the waste of products with high added values is avoided, the cost for processing a large amount of waste liquid and purchasing a new solvent is saved, and great economic benefits are generated.
Drawings
The invention is shown in figure 2:
FIG. 1 is an apparatus for multiple recovery of components using pervaporation-crystallization coupling.
FIG. 2 is a recovery processing device for multi-component in the waste liquid of sodium pyruvate production.
In the figure: 1 heating unit, 101 heater, 2 pervaporation separation membrane unit, 201 molecular sieve membrane module, 3 crystallization unit, 301 retentate condenser, 302 crystallization vessel, 4 feed pump, 5 permeate condenser, 6 permeate storage tank.
Detailed Description
The invention firstly provides a method for recovering components in multiple ways by utilizing pervaporation-crystallization coupling, which comprises the following steps: heating the raw material liquid to the pervaporation temperature, introducing the raw material liquid into a pervaporation membrane separation unit, and enriching the raw material liquid into a permeate on the downstream side of a membrane by a separation membrane which is selectively penetrated by one component in the recovered solvent; the retentate on the upstream side of the membrane is introduced into a crystallization unit, and after crystallization (cooling to a crystallization temperature to precipitate crystals) is subjected to solid-liquid separation to obtain crystals and a crystallization raffinate.
Wherein, the raw material liquid refers to a mixed solution containing a plurality of recoverable components to be treated. Generally, the process preferably employs a feed solution for treatment that is a mixed solution comprising a solvent, water and a crystallizable component, wherein the solvent and water are miscible and the crystallizable component has a greater solubility in water than in the solvent. It is possible to achieve a transition from an unsaturated to a supersaturated state of the crystallizable component in the system as the water content is reduced, and thereby to crystallize out.
When applied to the above aqueous feed solution, in a preferred embodiment, the pervaporation membrane is a selectively permeable membrane. More preferably a selectively permeable molecular sieve membrane. Examples include, but are not limited to, type a molecular sieve membranes.
In more specific application, the raw material liquid is an unsaturated solution of a crystallizable component, the water content of the retentate obtained by dehydrating the raw material liquid is greatly reduced, but crystals are still not precipitated at the pervaporation temperature or in a flowing state of the retentate, and the crystals can be precipitated when the temperature of the retentate is reduced or the flowing state is changed into a standing state. Thus, there are various alternative ways of crystallizing the retentate, and crystallization by lowering the temperature is preferred. Of course, in fact, in industrial applications, both approaches tend to coexist. The retentate flows out of the membrane module, flows through the retentate condenser and then enters the crystallization storage tank, and stands still and/or is further cooled to completely separate out crystals. E.g. crystallization, by cooling the retentate to the crystallization temperature; the pervaporation temperature is below the maximum refractory temperature of the crystallizable component and above the crystallization temperature of the crystallizable component in the retentate. In a more specific embodiment, the retentate is an unsaturated solution for the crystallizable component at the pervaporation temperature and is a supersaturated solution for the crystallizable component at the crystallization temperature.
By the process, the recovery of the solvent and the recovery of the crystallizable component can be realized simultaneously.
The above-described process of the present invention can be applied independently or set to be performed cyclically to meet the requirements of different standards for products. In a specific embodiment, a common recycling mode can be to incorporate the crystallization raffinate into the feed solution for recycling operation, or to incorporate the crystallization raffinate into the raffinate for further crystallization.
Based on the content of the above-mentioned process, the skilled person can develop various specific processes according to the requirements of the product or the production process, and design the corresponding production device. Such variations are intended to be within the scope of the invention.
Such designs may be exemplified by, but not limited to: in the above method of multiple component recovery by pervaporation-crystallization coupling, the pervaporation process may be a single pass or a cyclic process. The pervaporation-crystallization coupling process can be a single-pass process or a circulating process.
In the aspect of raw material liquid selection, in the more specific application of the invention, the raw material liquid is a solution to be recovered generated in the alcohol precipitation process, and comprises water and C1-4Alcohol and a crystallizable component, the crystallizable component having a solubility in water greater than that of C1-4Solubility in alcohol. The solution to be recovered generated in the representative alcohol precipitation process is the mother liquor remaining after sodium pyruvate crystals are obtained by crystallization in the alcohol precipitation process in the sodium pyruvate production process. The mother liquor typically comprises ethanol, water and sodium pyruvate, and in this particular example of use, the process of the invention comprises the steps of:
(1) heating the raw material liquid to the pervaporation temperature, introducing the raw material liquid into a separation membrane component, and enabling water to selectively permeate through the separation membrane to be enriched into a permeate at the downstream side of the membrane;
(2) guiding the residual solution which does not permeate through the separation membrane into a crystallization unit, cooling to crystallization temperature to precipitate crystals, and filtering after crystallization is completed to obtain sodium pyruvate crystals and crystallization residual solution; the crystallization residual liquid is a mixed solution containing a small amount of water, ethanol and part of unseparated sodium pyruvate;
further, the method may comprise the following steps of a cycle, namely:
(3) the crystallization residual liquid is merged into the raw material liquid, the operations of the steps (1) to (2) are circulated, or,
and (3) adding the crystallization residual liquid into the infiltration residual liquid, and circulating the operation of the step (2).
By way of preferred example, the invention provides a specific application of the method, namely a method for recovering and treating multiple components in sodium pyruvate production waste liquid, which comprises the following steps:
(1) heating the raw material waste liquid to 40-50 ℃, introducing the raw material waste liquid into a pervaporation separation membrane assembly, and enriching water in the waste liquid into a permeate through the separation membrane selectively at the downstream side of the separation membrane; of course, in a specific production process, some exploration and challenge are required for selecting the pervaporation temperature according to field raw materials and test conditions, and under the specific conditions of the embodiment, the temperature is most suitably controlled to be 45 +/-2 ℃.
(2) Introducing the residual solution into a crystallization unit, cooling to 0 +/-2 ℃, and filtering to obtain sodium pyruvate crystals and crude ethanol after the crystals are completely separated out;
(3) the crude ethanol is combined into raw material waste liquid, and the operations of the steps (1) to (2) are recycled, or
The crude ethanol is combined with the retentate and the operation of step (2) is recycled.
In order to cooperate with the above multiple recovery method, the invention further provides a device, namely a device for multiple recovery of components by utilizing pervaporation-crystallization coupling, which comprises a heating unit 1, a pervaporation separation membrane unit 2 and a crystallization unit 3; the heating unit 1 heats the raw material liquid to the pervaporation temperature; the pervaporation membrane unit 2 receives the heated raw material liquid and separates the raw material liquid into a permeate and a retentate; the crystallization unit 3 receives the retentate.
In connection with the method of the present invention utilizing pervaporation-crystallization coupled multiple recovery of components as described above, it is believed that the method of using the apparatus need not be described in further detail. By way of example and preferred method, the present invention provides a set of apparatus for recovering and treating multiple components in waste liquid from sodium pyruvate production, as shown in fig. 2, comprising: a heater 101, a feed pump 4 connected to the heater 101; a molecular sieve membrane module 201 connected to the heater 101, a permeate condenser 5 connected to the downstream side of the separation membrane, a retentate condenser 301 connected to the upstream side of the separation membrane, and a crystallization vessel 302 connected thereto.
In addition to the basic structure described above, the skilled person can achieve the object by adding connecting channels, material pumps and valves between the above-mentioned components according to the requirements of cyclic processing, batch/continuous production, and these technical means should be regarded as a simple combination of the present invention and the prior art and are covered by the scope of the present invention.
The following flight limiting examples are provided to further illustrate the present invention and should not be construed as limiting the scope of the present invention in any way.
Example 1
The typical production process of sodium pyruvate comprises the following steps:
(1) pumping 280kg of pyruvic acid into a sodium pyruvate reaction tank, stirring after pumping, slowly pressing the pretreated sodium carbonate solution (172kg of sodium carbonate is dissolved in 420kg of water) into the reaction tank, controlling the temperature in the reaction tank to be not more than 35 ℃, stopping feeding when the pH value of the reaction liquid reaches 4.8-5.3, and controlling the feeding time to be about 1 hour;
(2) after the reaction, 1440kg of 95% ethanol is slowly pumped into the reaction tank, and after the pumping, the mixture is centrifugally dried;
(3) and (3) conveying the solid product obtained by centrifugation into a drying room, carrying out vacuum drying, controlling the vacuum degree to be more than or equal to-0.09 Mpa and the temperature to be 65-70 ℃, keeping the temperature for 2 hours, cooling for about 20 minutes when the dry loss is less than or equal to 0.5%, and discharging.
After solid-liquid separation is carried out in the step (2), centrifugal mother liquor is obtained, and the composition of the centrifugal mother liquor is very typical through detection and contains: 60kg of sodium pyruvate, 1400kg of ethanol and 500kg of water. As a raw material liquid to be treated in the following test. The treatment aims to realize the dehydration recovery of ethanol and the crystallization recovery of sodium pyruvate in the same process flow.
S1: constructing a multi-component recovery processing device in the sodium pyruvate production waste liquid, as shown in the attached figure 2: the feed pump 4, the heater 101 and the molecular sieve membrane component 201 are sequentially connected; the molecular sieve membrane component 201 adopts an A-type molecular sieve membrane, and the filling area of the membrane component is 0.27 square meter. The downstream side of the separation membrane is connected to the permeate condenser 5, the upstream side of the separation membrane is connected to the retentate condenser 301, and the retentate condenser 301 is further connected to the crystallisation vessel 302.
S2: a typical process is as follows:
a. the raw material liquid is input into a heater 101 through a feed pump 4 and heated to 45 ℃;
b. the heated material is input into the molecular sieve membrane module 201 for dehydration: water selectively permeates the separation membrane, is enriched into permeate at the downstream side of the separation membrane, is condensed by a permeate condenser 5 and then is led into a permeate storage tank 6; the dehydrated raw material liquid remaining on the upstream side of the separation membrane is a retentate, condensed by a retentate condenser 301, and introduced into a crystallization vessel 302.
c. In the crystallization container 302, the retentate is kept stand at zero temperature, after the sodium pyruvate crystals are separated out, solid-liquid separation is carried out to obtain sodium pyruvate solids and crystallization raffinate. The crystallization residual liquid is a solution which takes ethanol as a main component and contains a small amount of water and dissolved sodium pyruvate.
And recording and detecting the substance content of each product obtained in the process, and calculating.
The experimental results are as follows:
(1) total feed rate: 13.5 Kg;
(2) the total discharge amount:
water discharge (permeate amount) on the downstream side of the separation membrane: 3.1 Kg;
crystal recovery amount: 0.15 Kg;
recovery of crystallization raffinate (crude ethanol): 10.0 Kg;
the total discharge amount: 13.25Kg
It can be seen that the mass balance is substantially balanced.
(3) And (3) material analysis results:
feed water content: 26 wt.%;
water content in the crystallized raffinate (crude ethanol): 4 wt.%;
the purity of the recovered sodium pyruvate crystals is 70%.
Therefore, the pervaporation-crystallization coupling process can realize the recovery and reuse of the ethanol solvent and the improvement of the yield of the sodium pyruvate product, and has obvious economic benefit.
Example 2
The production process of sodium pyruvate is the same as that in example 1, except that the centrifugal mother liquor is treated and recovered by rectification, ethanol with water content of 6 wt.% is obtained at the top of the tower, and wastewater is obtained at the bottom of the tower. The following table shows the production efficiency comparison of the rectification process (I) of this example with the pervaporation crystallization process (II) of example 1, as shown in Table 1.
TABLE 1
Description of the drawings: the cost accounting in this table is based on the feed water content of 26 wt.% and the recovered solvent water content of 4 wt.%:
b: 1.0mpa steam measured 320 yuan/ton
b: the circulating cooling water is calculated according to 0.5 yuan/ton
d: the electricity is measured as 1 yuan/KWh.
e, calculating according to 2000 tons of raw material liquid processed every year
f, calculating newly purchased ethanol according to 6000 yuan/ton
h, according to the calculation of the test results, 10kg of ethanol is recovered, 150g of sodium pyruvate crystals with the content of 69% are obtained, and therefore 150 x 0.69/10 to 10.35kg of sodium propyl can be obtained for every ton of ethanol. Sodium pyruvate was calculated as 80 yuan/kg.

Claims (6)

1. The method for multiple recovery of components by using pervaporation-crystallization coupling is characterized by comprising the following steps of: heating the raw material liquid to the pervaporation temperature, introducing the raw material liquid into a pervaporation membrane separation unit, and enriching the raw material liquid into a permeate on the downstream side of a membrane by a separation membrane which is selectively penetrated by one component in the recovered solvent; introducing the residual solution on the upstream side of the membrane into a crystallization unit, and performing solid-liquid separation after crystallization to obtain crystals and crystallization residual solution;
wherein:
the raw material liquid comprises a solvent, water and a crystallizable component, wherein the solvent is ethanol, and the crystallizable component is sodium pyruvate;
the pervaporation membrane is a selective water permeable membrane.
2. The method of claim 1, further comprising:
a step of merging the crystallization residual liquid into the raw material liquid for cycle operation, or,
and adding the crystallization residual liquid into the infiltration residual liquid to continue crystallization.
3. The process according to claim 1, characterized in that the crystallization is carried out by cooling the retentate to the crystallization temperature; the pervaporation temperature is below the maximum refractory temperature of the crystallizable component and above the crystallization temperature of the crystallizable component in the retentate.
4. The method of claim 1 wherein the retentate is an unsaturated solution for the crystallizable component at the pervaporation temperature and is a supersaturated solution for the crystallizable component at the crystallization temperature.
5. The method of claim 4, wherein the feed solution is a centrifuge mother liquor of a sodium pyruvate production process, the centrifuge mother liquor comprising ethanol, water and sodium pyruvate, the method comprising the steps of:
(1) heating the raw material liquid to the pervaporation temperature, introducing the raw material liquid into a separation membrane component, and enabling water to selectively permeate through the separation membrane to be enriched into a permeate at the downstream side of the membrane;
(2) guiding the residual solution which does not permeate through the separation membrane into a crystallization unit, cooling to crystallization temperature to precipitate crystals, and filtering after crystallization is completed to obtain sodium pyruvate crystals and crystallization residual solution;
(3) the crystallization residual liquid is added into the raw material liquid, the operation of the steps (1) to (2) is circulated, or,
and (3) adding the crystallization residual liquid into the infiltration residual liquid, and circulating the operation of the step (2).
6. The method of claim 5, comprising the steps of:
(1) heating the raw material waste liquid to 40-50 ℃, introducing the raw material waste liquid into a pervaporation separation membrane assembly, and enriching water in the waste liquid into a permeate through the separation membrane selectively at the downstream side of the separation membrane;
(2) introducing the residual solution into a crystallization unit, cooling to 0 +/-2 ℃, and filtering to obtain sodium pyruvate crystals and crude ethanol after the crystals are completely separated out;
(3) the crude ethanol is merged into the raw material waste liquid, and the operation of the steps (1) to (2) is circulated, or
The crude ethanol is combined with the retentate and the operation of step (2) is recycled.
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CN103910608A (en) * 2014-03-26 2014-07-09 太原理工大学 Phenol crystallization method and device by adopting pervaporation-crystallization coupling way

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