CN114507119A - Method for purifying n-butanol solvent in diammonium glycyrrhizinate production - Google Patents
Method for purifying n-butanol solvent in diammonium glycyrrhizinate production Download PDFInfo
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- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 title claims abstract description 230
- 239000002904 solvent Substances 0.000 title claims abstract description 85
- SPPIIOPGDLITJE-VLQRKCJKSA-N diazanium;(2s,3s,4s,5r,6s)-6-[[(3s,4ar,6ar,6bs,8as,11s,12ar,14ar,14bs)-11-carboxylato-4,4,6a,6b,8a,11,14b-heptamethyl-14-oxo-2,3,4a,5,6,7,8,9,10,12,12a,14a-dodecahydro-1h-picen-3-yl]oxy]-5-[(2r,3r,4s,5s,6s)-6-carboxy-3,4,5-trihydroxyoxan-2-yl]oxy-3,4-dihy Chemical compound N.N.O([C@@H]1[C@@H](O)[C@H](O)[C@H](O[C@@H]1O[C@H]1CC[C@]2(C)[C@H]3C(=O)C=C4[C@@H]5C[C@](C)(CC[C@@]5(CC[C@@]4(C)[C@]3(C)CC[C@H]2C1(C)C)C)C(O)=O)C(O)=O)[C@@H]1O[C@H](C(O)=O)[C@@H](O)[C@H](O)[C@H]1O SPPIIOPGDLITJE-VLQRKCJKSA-N 0.000 title claims abstract description 28
- 238000000034 method Methods 0.000 title claims abstract description 23
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 22
- 238000003756 stirring Methods 0.000 claims abstract description 31
- 238000006243 chemical reaction Methods 0.000 claims abstract description 27
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 24
- 238000010438 heat treatment Methods 0.000 claims abstract description 15
- 238000001914 filtration Methods 0.000 claims abstract description 12
- 239000012535 impurity Substances 0.000 claims abstract description 11
- 238000005086 pumping Methods 0.000 claims abstract description 11
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000008213 purified water Substances 0.000 claims abstract description 9
- 230000007935 neutral effect Effects 0.000 claims abstract description 8
- 239000012141 concentrate Substances 0.000 claims abstract description 5
- 238000007599 discharging Methods 0.000 claims abstract description 5
- 210000003298 dental enamel Anatomy 0.000 claims description 2
- 238000000746 purification Methods 0.000 abstract description 6
- 239000000243 solution Substances 0.000 description 20
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 12
- 239000007788 liquid Substances 0.000 description 12
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 6
- 229960000583 acetic acid Drugs 0.000 description 6
- 235000011114 ammonium hydroxide Nutrition 0.000 description 6
- 239000007864 aqueous solution Substances 0.000 description 6
- 238000000605 extraction Methods 0.000 description 6
- 239000012362 glacial acetic acid Substances 0.000 description 6
- 239000002699 waste material Substances 0.000 description 5
- 238000002425 crystallisation Methods 0.000 description 4
- 230000008025 crystallization Effects 0.000 description 4
- 239000002920 hazardous waste Substances 0.000 description 4
- 238000003860 storage Methods 0.000 description 4
- 239000003814 drug Substances 0.000 description 3
- 239000012528 membrane Substances 0.000 description 3
- 239000011259 mixed solution Substances 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 238000004321 preservation Methods 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 229940079593 drug Drugs 0.000 description 2
- 229940088597 hormone Drugs 0.000 description 2
- 239000005556 hormone Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- DKPFZGUDAPQIHT-UHFFFAOYSA-N Butyl acetate Natural products CCCCOC(C)=O DKPFZGUDAPQIHT-UHFFFAOYSA-N 0.000 description 1
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000001299 aldehydes Chemical class 0.000 description 1
- 239000003242 anti bacterial agent Substances 0.000 description 1
- 229940088710 antibiotic agent Drugs 0.000 description 1
- CQEYYJKEWSMYFG-UHFFFAOYSA-N butyl acrylate Chemical compound CCCCOC(=O)C=C CQEYYJKEWSMYFG-UHFFFAOYSA-N 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000013064 chemical raw material Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 239000006184 cosolvent Substances 0.000 description 1
- 239000012024 dehydrating agents Substances 0.000 description 1
- 239000002274 desiccant Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- DOIRQSBPFJWKBE-UHFFFAOYSA-N dibutyl phthalate Chemical compound CCCCOC(=O)C1=CC=CC=C1C(=O)OCCCC DOIRQSBPFJWKBE-UHFFFAOYSA-N 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000003995 emulsifying agent Substances 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000003205 fragrance Substances 0.000 description 1
- 239000004519 grease Substances 0.000 description 1
- FUZZWVXGSFPDMH-UHFFFAOYSA-M hexanoate Chemical compound CCCCCC([O-])=O FUZZWVXGSFPDMH-UHFFFAOYSA-M 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 229910000027 potassium carbonate Inorganic materials 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- 235000013599 spices Nutrition 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- STCOOQWBFONSKY-UHFFFAOYSA-N tributyl phosphate Chemical compound CCCCOP(=O)(OCCCC)OCCCC STCOOQWBFONSKY-UHFFFAOYSA-N 0.000 description 1
- 229940088594 vitamin Drugs 0.000 description 1
- 239000011782 vitamin Substances 0.000 description 1
- 229930003231 vitamin Natural products 0.000 description 1
- 235000013343 vitamin Nutrition 0.000 description 1
- 239000010887 waste solvent Substances 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a method for purifying an n-butanol solvent in diammonium glycyrrhizinate production, which comprises the following steps: s1: adjusting the pH value of the used n-butanol solvent to be neutral by using dilute hydrochloric acid; s2: pumping the n-butanol-soluble solvent adjusted in the step S1 into a single-effect concentration reaction kettle, heating the single-effect concentration reaction kettle, and then starting to concentrate under reduced pressure, wherein the reduced pressure is-0.1 to-0.07 MPa; s3: filtering the n-butanol solvent decompressed in the step S2 to remove impurities to obtain a pretreated n-butanol solvent; s4: pumping the n-butanol solvent pretreated in the step S3 into a reaction kettle, adding purified water under the condition of stirring, stirring for 30-40min, standing for 1-2 h for layering, and discharging a water layer to obtain a clear and transparent n-butanol layer. The n-butanol solvent purification method has the advantages of simplicity, short time consumption, low cost and the like, and the obtained n-butanol solvent has few impurities and high purity, has no difference with a new n-butanol solvent in diammonium glycyrrhizinate production, and has good market prospect.
Description
Technical Field
The invention relates to a purification method, in particular to a method for purifying an n-butanol solvent in diammonium glycyrrhizinate production, and belongs to the technical field of chemical industry.
Background
The n-butyl alcohol is mainly used as a solvent, a dehydrating agent, an anti-emulsifying agent, an extracting agent of grease, a spice drug, hormone and the like, is used as a condensing agent and a cosolvent in the chemical industry, and is used as a standard substance in chromatographic analysis and a high-purity reagent in scientific research experiments. N-butyl alcohol is an important organic chemical raw material, has very wide application, and is mainly used for n-butyl phthalate, fatty dibasic acid, butyl phosphate, butyl acrylate, butyl acetate and the like; they are widely used in medicine, organic synthesis, and as extractants for oils, drugs (such as antibiotics, hormones, and vitamins), and fragrances.
The Chinese patent with application number of 201210232200.0 discloses an invention patent named as a purification method of high-purity organic solvent n-butanol, which comprises the following steps: removing most of aldehyde, ketone and ester impurities from the raw material n-butyl alcohol through silica gel and a diatomite column, drying and dehydrating the raw material n-butyl alcohol by using anhydrous magnesium sulfate or anhydrous potassium carbonate serving as a drying agent, rectifying, filtering and packaging to obtain the high-purity organic solvent n-butyl alcohol product. However, the method is too complicated to operate, inconvenient to operate and needs further improvement.
At present, after the n-butyl alcohol solvent is used, the n-butyl alcohol solvent can be used as a waste solvent to be filled into a storage tank and then used as hazardous waste to be externally wrapped by hazardous waste manufacturers for treatment. The waste n-butanol solvent is used as hazardous waste, and the storage and transportation of the waste n-butanol solvent bring great potential safety hazards to workshops and can also cause waste to a certain extent.
In view of the above, in order to further reduce the production cost of diammonium glycyrrhizinate and reduce unnecessary potential safety hazards, it is urgently needed to improve the recovery and purification of the n-butanol solvent used in the production of diammonium glycyrrhizinate.
Disclosure of Invention
The invention aims to solve the problems in the prior art and provides a method for purifying an n-butanol solvent in diammonium glycyrrhizinate production.
In order to achieve the above object, the present invention adopts the following technical solutions:
a method for purifying an n-butanol solvent in diammonium glycyrrhizinate production is characterized by comprising the following steps:
s1: adjusting the pH value of the used n-butanol solvent to be neutral by using dilute hydrochloric acid;
s2: pumping the n-butanol-soluble solvent adjusted in the step S1 into a single-effect concentration reaction kettle, heating the single-effect concentration reaction kettle, and then carrying out reduced pressure concentration;
s3: filtering the n-butanol solvent decompressed in the step S2 by using a filter to remove impurities to obtain a pretreated n-butanol solvent;
s4: and (4) carrying out back extraction on the n-butanol solvent pretreated in the step S3 through purified water to obtain the high-purity n-butanol solvent.
Preferably, in the step S1, the concentration of the dilute hydrochloric acid is 18% to 19%, in the step S2, the single-effect concentration reaction kettle is an enamel single-effect concentration reaction kettle, the pH of the n-butanol solvent is adjusted to be neutral to 7.0, and meanwhile, the ceramic single-effect concentration reaction kettle is used as the reaction kettle, so that corrosion of the n-butanol solvent to the reaction kettle can be reduced, and the reaction kettle is protected.
More preferably, in the step S2, the temperature of the single-effect concentration reactor is increased to 65 to 75 ℃.
Still preferably, in the step S2, the temperature of the single-effect concentration reactor is raised to 70 ℃.
Further preferably, in the step S2, the mesh number of the filter is one or more of 1000 meshes, 1300 meshes and 1500 meshes.
Still more preferably, in the step S2, the mesh number of the filter is 1000 meshes.
Still more preferably, in the step S3, the pretreated n-butanol is mixed with a certain amount of water, and the mixture is not slightly milky, and the main purpose of the filtration is: removing fine and invisible particulate matters in the production process.
In step S4, the mass ratio of the n-butanol solvent to the purified water after the pretreatment is: (2-4) to 1.
The invention has the advantages that:
(1) the method for purifying the n-butyl alcohol solvent has the advantages that the n-butyl alcohol solvent used in the diammonium glycyrrhizinate production is subjected to adjustment to be neutral by dilute hydrochloric acid, reduced pressure concentration, impurity removal by filtration and back extraction to obtain the high-purity n-butyl alcohol solvent, the used n-butyl alcohol solvent is recycled and purified by the method, waste of the n-butyl alcohol solvent is avoided, the production cost of the diammonium glycyrrhizinate can be further reduced, and potential safety hazards of the used n-butyl alcohol solvent in storage and transportation can be reduced;
(2) the n-butanol solvent purification method has the advantages of being simple, short in time consumption, low in cost and the like, the obtained n-butanol solvent is few in impurities and high in purity, has no difference with a new n-butanol solvent in diammonium glycyrrhizinate production, and has a good market prospect.
Drawings
FIG. 1 is a diagram showing a comparison of the crystallization state of diammonium glycyrrhizinate by using different n-butanol solvents according to the present invention.
Detailed Description
The present invention is further illustrated by the following examples, which are not intended to limit the scope of the invention.
Example 1
S1: the pH of 1300kg of the used n-butanol solvent was adjusted to neutral 7.0 with 50kg of 18% dilute hydrochloric acid;
s2: pumping the n-butanol-soluble solvent adjusted in the step S1 into a single-effect concentration reaction kettle, heating the single-effect concentration reaction kettle to 65 ℃, and then starting to concentrate under reduced pressure, wherein the reduced pressure is 0.1 MPa;
s3: filtering the n-butanol solvent decompressed in the step S2 through a 1000-mesh filter to remove impurities to obtain a pretreated n-butanol solvent;
s4: pumping the n-butanol solvent pretreated in the step S3 into a reaction kettle, adding 650kg of purified water under the condition of stirring, stirring for 30min, standing for 1 hour for layering, and discharging a water layer to obtain 1010kg of clear and transparent n-butanol solvent.
Example 2
S1: adjusting the pH value of the used 1280kg of n-butanol solvent to be neutral 7.0 by 45kg of 18% diluted hydrochloric acid;
s2: pumping the n-butanol-soluble solvent adjusted in the step S1 into a single-effect concentration reaction kettle, heating the single-effect concentration reaction kettle to 70 ℃, and then starting to concentrate under reduced pressure, wherein the reduced pressure is 0.09 MPa;
s3: filtering the n-butanol solvent decompressed in the step S2 through a 1300-mesh filter to remove impurities to obtain a pretreated n-butanol solvent;
s4: pumping the n-butanol solvent pretreated in the step S3 into a reaction kettle, adding 430kg of purified water under the condition of stirring, stirring for 35min, standing for 1.5 hours for layering, and discharging a water layer to obtain 980kg of clear and transparent n-butanol solvent.
Example 3
S1: the pH of the used 1250kg of n-butanol solvent was adjusted to neutral 7.0 with 48kg of 19% dilute hydrochloric acid;
s2: pumping the n-butanol-soluble solvent adjusted in the step S1 into a single-effect concentration reaction kettle, heating the single-effect concentration reaction kettle to 75 ℃, and then starting to concentrate under reduced pressure, wherein the reduced pressure is 0.07 MPa;
s3: filtering the n-butanol solvent decompressed in the step S2 through a 1500-mesh filter to remove impurities to obtain a pretreated n-butanol solvent;
s4: pumping the n-butanol solvent pretreated in the step S3 into a reaction kettle, adding 625g of purified water under the stirring condition, stirring for 40min, standing for 2 hours for layering, and discharging a water layer to obtain 950kg of clear and transparent n-butanol solvent.
Sample detection
Selecting new n-butanol solvent, new and old n-butanol solvent and the n-butanol solvent purified in the embodiment 2, wherein the new and old n-butanol solvent is n-butanol solvent without back extraction by purified water, and the preparation process of the sample according to the diammonium glycyrrhizinate process comprises the following steps:
(1) dividing the acidified solution into three parts equally in a beaker, adding a new n-butanol solvent with the volume of 1/3 of the acidified solution, stirring and extracting for 3 hours, standing and layering for 3 hours, and separating an upper solution (n-butanol layer); and adding water with the volume of n-butyl alcohol of 1/4 into the upper layer solution for back extraction, stirring and extracting for 3 hours, standing and layering for 3 hours, and separating to obtain n-butyl alcohol extract.
Keeping the temperature of the solution at 30 ℃, slowly adding 14 volume percent concentrated ammonia water of n-butyl alcohol into the n-butyl alcohol extract, continuously stirring for 7 at 30 ℃, standing for 2 hours, separating out lower-layer aqueous solution, and filtering by a 1000-mesh filter membrane.
Placing the filtered ammoniated solution in a beaker, stirring, heating in water bath until the temperature of the internal liquid is 73 ℃, adding an ethanol glacial acetic acid mixed solution (obtained by mixing 90% ethanol with 4.5 times of volume of the lower-layer aqueous solution and glacial acetic acid with the same volume of ammonia water and stirring uniformly) while stirring; after the addition, the water bath heating is continued until the temperature of the internal liquid is 73 ℃, the heat preservation is carried out for 4 hours, the heating is stopped, the stirring and the temperature reduction are continued until a large amount of white solid is separated out, and the time is more than 12 hours. And (3) putting the crystallization liquid in a Buchner funnel until no liquid flows out basically, and obtaining the diammonium glycyrrhizinate wet product.
(2) Dividing the acidified solution into three parts equally in a beaker, adding new and old n-butanol solvents with the volume of 1/3 of the acidified solution, stirring and extracting for 3 hours, standing and layering for 3 hours, and separating the upper solution (n-butanol layer); and adding water with the volume of n-butyl alcohol of 1/4 into the upper layer solution for back extraction, stirring and extracting for 3 hours, standing and layering for 3 hours, and separating to obtain n-butyl alcohol extract.
Keeping the temperature of the solution at 30 ℃, slowly adding 14 volume percent concentrated ammonia water of n-butyl alcohol into the n-butyl alcohol extract, continuously stirring for 7 at 30 ℃, standing for 2 hours, separating out lower-layer aqueous solution, and filtering by a 1000-mesh filter membrane.
Placing the filtered ammoniated solution in a beaker, stirring, heating in water bath until the temperature of the internal liquid is 73 ℃, adding an ethanol glacial acetic acid mixed solution (obtained by mixing 90% ethanol with 4.5 times of volume of the lower-layer aqueous solution and glacial acetic acid with the same volume of ammonia water and stirring uniformly) while stirring; after the addition, the water bath heating is continued until the temperature of the internal liquid is 73 ℃, the heat preservation is carried out for 4 hours, the heating is stopped, the stirring and the temperature reduction are continued until a large amount of white solid is separated out, and the time is more than 12 hours. And (3) putting the crystallization liquid in a Buchner funnel until no liquid flows out basically, and obtaining the diammonium glycyrrhizinate wet product.
(3) Dividing the acidified solution into three parts equally in a beaker, adding the n-butanol solvent purified in example 2 with the volume of the acidified solution being 1/3, stirring and extracting for 3 hours, standing and layering for 3 hours, and separating the upper solution (n-butanol layer); and adding water with the volume of n-butyl alcohol of 1/4 into the upper layer solution for back extraction, stirring and extracting for 3 hours, standing and layering for 3 hours, and separating to obtain n-butyl alcohol extract.
Keeping the temperature of the solution at 30 ℃, slowly adding 14 volume percent concentrated ammonia water of n-butyl alcohol into the n-butyl alcohol extract, continuously stirring for 7 at 30 ℃, standing for 2 hours, separating out lower-layer aqueous solution, and filtering by a 1000-mesh filter membrane.
Placing the filtered ammoniated solution in a beaker, stirring, heating in water bath until the temperature of the internal liquid is 73 ℃, adding an ethanol glacial acetic acid mixed solution (obtained by mixing 90% ethanol with 4.5 times of volume of the lower-layer aqueous solution and glacial acetic acid with the same volume of ammonia water and stirring uniformly) while stirring; after the addition, the water bath heating is continued until the temperature of the internal liquid is 73 ℃, the heat preservation is carried out for 4 hours, the heating is stopped, the stirring and the temperature reduction are continued until a large amount of white solid is separated out, and the time is more than 12 hours. And (3) putting the crystallization liquid in a Buchner funnel until no liquid flows out basically, and obtaining the diammonium glycyrrhizinate wet product.
The clarity and yield of the sample meet the quality standard of internal control (see table 1)
TABLE 1
After detection, the state of the sample when diammonium glycyrrhizinate is crystallized is shown in fig. 1, and in fig. 1, from left to right, the new n-butanol solvent, the n-butanol solvent purified in example 2 and the new n-butanol solvent are used.
In conclusion, the n-butanol solvent purification method has the advantages of being simple, short in time consumption, low in cost and the like, the obtained n-butanol solvent is few in impurities and high in purity, has no difference with a new n-butanol solvent in diammonium glycyrrhizinate production, and has a good market prospect. The method is used for recovering and purifying the used n-butyl alcohol solvent, avoids waste, can further reduce the production cost of the diammonium glycyrrhizinate, and can also reduce the potential safety hazard of the diammonium glycyrrhizinate as hazardous waste in storage and transportation.
In the description herein, references to the description of the term "one embodiment," "some embodiments," "an example," "a specific example," or "some examples," etc., mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The foregoing illustrates and describes the principles, general features, and advantages of the present invention. It should be understood by those skilled in the art that the above embodiments do not limit the present invention in any way, and all technical solutions obtained by using equivalent alternatives or equivalent variations fall within the scope of the present invention.
Claims (7)
1. A method for purifying an n-butanol solvent in diammonium glycyrrhizinate production is characterized by comprising the following steps:
s1: adjusting the pH value of the used n-butanol solvent to be neutral by using dilute hydrochloric acid;
s2: pumping the n-butanol-soluble solvent adjusted in the step S1 into a single-effect concentration reaction kettle, heating the single-effect concentration reaction kettle, and then starting to concentrate under reduced pressure, wherein the reduced pressure is-0.1 to-0.07 MPa;
s3: filtering the n-butanol solvent decompressed in the step S2 by using a filter to remove impurities to obtain a pretreated n-butanol solvent;
s4: pumping the n-butanol solvent pretreated in the step S3 into a reaction kettle, adding purified water under the condition of stirring, stirring for 30-40min, standing for 1-2 h for layering, and discharging a water layer to obtain a clear and transparent n-butanol layer.
2. The method for purifying the n-butanol solvent in the production of diammonium glycyrrhizinate, according to claim 1, wherein in step S1, the concentration of dilute hydrochloric acid is 18% to 19%, and in step S2, the single-effect concentration reaction kettle is an enamel single-effect concentration reaction kettle.
3. The method for purifying the n-butanol solvent in the production of diammonium glycyrrhizinate, according to claim 1, wherein in step S2, the temperature of the single-effect concentration reaction kettle is increased to 65-75 ℃.
4. The method for purifying the n-butanol solvent in the production of diammonium glycyrrhizinate, according to claim 3, wherein in step S2, the temperature of the single-effect concentration reaction kettle is raised to 70 ℃.
5. The method for purifying the n-butanol solvent in the production of diammonium glycyrrhizinate according to claim 1, wherein the mesh number of the filter is one or more of 1000 meshes, 1300 meshes and 1500 meshes.
6. The method for purifying the n-butanol solvent in the production of diammonium glycyrrhizinate, according to claim 5, wherein the mesh number of the filter is 1000 meshes.
7. The method for purifying the n-butanol solvent in the diammonium glycyrrhizinate production according to claim 1, wherein in step S4, the mass ratio of the n-butanol solvent to the purified water after the pretreatment is: (2-4) to 1.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4507176A (en) * | 1984-05-07 | 1985-03-26 | Lloyd Berg | Separation of n-butyl acetate from n-butanol by extractive distillation |
| CN1743338A (en) * | 2004-09-01 | 2006-03-08 | 天津市资福医药科技开发有限公司 | Method for preparing diammonium glycyrhetate |
| CN102731251A (en) * | 2012-07-06 | 2012-10-17 | 天津市康科德科技有限公司 | Purification method of highly pure organic solvent n-butanol |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4507176A (en) * | 1984-05-07 | 1985-03-26 | Lloyd Berg | Separation of n-butyl acetate from n-butanol by extractive distillation |
| CN1743338A (en) * | 2004-09-01 | 2006-03-08 | 天津市资福医药科技开发有限公司 | Method for preparing diammonium glycyrhetate |
| CN102731251A (en) * | 2012-07-06 | 2012-10-17 | 天津市康科德科技有限公司 | Purification method of highly pure organic solvent n-butanol |
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