CN116348185A - Method and device for back-extraction purification of crude product after sublimation of maltol or ethyl maltol - Google Patents
Method and device for back-extraction purification of crude product after sublimation of maltol or ethyl maltol Download PDFInfo
- Publication number
- CN116348185A CN116348185A CN202180065864.XA CN202180065864A CN116348185A CN 116348185 A CN116348185 A CN 116348185A CN 202180065864 A CN202180065864 A CN 202180065864A CN 116348185 A CN116348185 A CN 116348185A
- Authority
- CN
- China
- Prior art keywords
- maltol
- kettle
- ethyl
- ethyl maltol
- crude product
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- XPCTZQVDEJYUGT-UHFFFAOYSA-N 3-hydroxy-2-methyl-4-pyrone Chemical compound CC=1OC=CC(=O)C=1O XPCTZQVDEJYUGT-UHFFFAOYSA-N 0.000 title claims abstract description 166
- HYMLWHLQFGRFIY-UHFFFAOYSA-N Maltol Natural products CC1OC=CC(=O)C1=O HYMLWHLQFGRFIY-UHFFFAOYSA-N 0.000 title claims abstract description 83
- 229940043353 maltol Drugs 0.000 title claims abstract description 83
- YIKYNHJUKRTCJL-UHFFFAOYSA-N Ethyl maltol Chemical compound CCC=1OC=CC(=O)C=1O YIKYNHJUKRTCJL-UHFFFAOYSA-N 0.000 title claims abstract description 76
- 229940093503 ethyl maltol Drugs 0.000 title claims abstract description 76
- 238000000034 method Methods 0.000 title claims abstract description 34
- 239000012043 crude product Substances 0.000 title claims abstract description 29
- 238000000859 sublimation Methods 0.000 title claims abstract description 25
- 230000008022 sublimation Effects 0.000 title claims abstract description 25
- 238000000746 purification Methods 0.000 title claims abstract description 14
- 238000000605 extraction Methods 0.000 title claims abstract description 9
- 239000012535 impurity Substances 0.000 claims abstract description 36
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 36
- 239000000463 material Substances 0.000 claims abstract description 28
- 239000007864 aqueous solution Substances 0.000 claims abstract description 16
- 238000010438 heat treatment Methods 0.000 claims abstract description 10
- 239000013078 crystal Substances 0.000 claims abstract description 9
- 238000004090 dissolution Methods 0.000 claims description 29
- 238000007710 freezing Methods 0.000 claims description 19
- 230000008014 freezing Effects 0.000 claims description 18
- 210000003298 dental enamel Anatomy 0.000 claims description 9
- 239000000047 product Substances 0.000 abstract description 5
- 239000012452 mother liquor Substances 0.000 description 21
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 10
- 239000002904 solvent Substances 0.000 description 10
- 238000001816 cooling Methods 0.000 description 9
- 239000000203 mixture Substances 0.000 description 8
- 238000007599 discharging Methods 0.000 description 6
- 238000000926 separation method Methods 0.000 description 6
- 238000001514 detection method Methods 0.000 description 5
- 238000011084 recovery Methods 0.000 description 5
- 238000002425 crystallisation Methods 0.000 description 4
- 230000008025 crystallization Effects 0.000 description 4
- 238000004821 distillation Methods 0.000 description 4
- 238000006460 hydrolysis reaction Methods 0.000 description 4
- 239000003513 alkali Substances 0.000 description 3
- 238000004042 decolorization Methods 0.000 description 3
- 239000000413 hydrolysate Substances 0.000 description 3
- 238000002844 melting Methods 0.000 description 3
- 230000008018 melting Effects 0.000 description 3
- 239000012074 organic phase Substances 0.000 description 3
- 239000012071 phase Substances 0.000 description 3
- 238000005086 pumping Methods 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 229910001615 alkaline earth metal halide Inorganic materials 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 230000007062 hydrolysis Effects 0.000 description 2
- 239000002085 irritant Substances 0.000 description 2
- 231100000021 irritant Toxicity 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 238000003747 Grignard reaction Methods 0.000 description 1
- 238000007259 addition reaction Methods 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 229910001508 alkali metal halide Inorganic materials 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- 239000008346 aqueous phase Substances 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000005660 chlorination reaction Methods 0.000 description 1
- 230000032798 delamination Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 235000013312 flour Nutrition 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 150000004820 halides Chemical class 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 239000002798 polar solvent Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 238000005092 sublimation method Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- 238000003911 water pollution Methods 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D309/00—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only ring hetero atom, not condensed with other rings
- C07D309/34—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only ring hetero atom, not condensed with other rings having three or more double bonds between ring members or between ring members and non-ring members
- C07D309/36—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only ring hetero atom, not condensed with other rings having three or more double bonds between ring members or between ring members and non-ring members with oxygen atoms directly attached to ring carbon atoms
- C07D309/40—Oxygen atoms attached in positions 3 and 4, e.g. maltol
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/04—Solvent extraction of solutions which are liquid
- B01D11/0492—Applications, solvents used
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Saccharide Compounds (AREA)
Abstract
The application discloses a crude product back extraction purification method after maltol or ethyl maltol sublimates, which comprises the following steps: step 1: heating the crude product after the sublimation of the maltol or the ethyl maltol and water to 80+/-5 ℃ for dissolving; step 2: layering and standing the material obtained in the step 1, separating an upper layer aqueous solution, and then reducing the temperature of the upper layer aqueous solution layer to 10-15 ℃; step 3: centrifuging to obtain the maltol or ethyl maltol crystal after impurity removal. A purification device is also disclosed. The purification technical scheme has high yield and high product purity.
Description
The application requires priority of China patent application with the application number of 202011442712.0 and the name of a crude product back extraction purification method after sublimation of ethyl maltol on the application day of 2020, 12 and 11.
The invention relates to a method and a device for stripping and purifying crude products after maltol and ethyl maltol are sublimated.
During the production reaction of the maltol and the ethyl maltol, a large amount of byproducts are generated, wherein part of impurities with pungent odor, which have the boiling points close to those of the maltol and the ethyl maltol, are evaporated along with the maltol and the ethyl maltol in a sublimation purification section, are extremely soluble with the maltol and the ethyl maltol, are difficult to separate, and the quality of the maltol and the ethyl maltol is difficult to improve.
Chinese patent document CN108299362a discloses a method for separating impurities from crude maltol, comprising: a. filtering the hydrolyzed material, and cooling to 35 ℃ of 30 ℃; b. pumping the hydrolysate into an extraction mixer, and pumping chloroform at the same time to fully mix the hydrolysate and the chloroform; c. feeding the mixed solution into a layering device, feeding the layered light phase into a hydrolysate collecting tank, feeding the lower heavy phase into a chloroform collecting tank, putting the chloroform collecting tank into a distillation kettle for distillation to recover chloroform, and feeding the distilled material into a sublimation kettle for sublimation; d. pumping the light phase material in the hydrolysis collecting tank into a neutralization kettle, regulating the PH to 2.5 and 3.5, reducing the temperature to 45 ℃ of 40 ℃, putting the material into a crystallizer for freezing crystallization, and delivering the material into a sublimation kettle for sublimation after centrifugal drying. Chinese patent document CN101993428B discloses a purification method of ethyl maltol, which is characterized by comprising the following sequential steps: (1) sublimating the ethyl maltol crude product; (2) dissolving; (3) cooling; (4) solid-liquid separation; and (5) drying to obtain a finished product. In this patent document, after the ethyl maltol is dissolved, a mixed solution of ethanol and water is used as a solvent for dissolving ethyl maltol, and since the solvent is miscible with other organic substances, the delamination operation cannot be completed, which results in the subsequent failure to separate impurities from the mixture. Chinese patent document CN105085457A discloses an ethyl maltol sublimation crystallization process, wherein a crude product receiving kettle is heated in an ethyl maltol sublimation working section, so that the temperature in the crude product receiving kettle is controlled between 90 ℃ and 92 ℃, materials in the kettle are in a molten liquid state and are directly sent to a crystallization kettle for crystallization, and two procedures of freezing and centrifugal material throwing in the traditional process are omitted. Chinese patent document CN103113339B discloses a method for separating and purifying maltol, which comprises the steps of grignard reaction, addition reaction, hydrolysis reaction, chlorination hydrolysis reaction and sublimation separation, and is characterized in that: the sublimation step adopts a molecular distiller, the distillation vacuum degree is below 0.05Pa, the temperature is 110-120 ℃, and the maltol is distilled. Patent document US5440053a discloses a process for recovering maltol from a water-insoluble feedstock comprising maltol, comprising: contacting the feedstock with an aqueous solution of a solute material, wherein the solute material is an alkali or alkaline earth halide that increases the specific gravity of the water and increases the miscibility of the water with the alkali or alkali metal. Alkaline earth metal halides are more soluble in water than the maltol at low temperatures under conditions effective to extract the maltol from the feedstock into the solution; and separating the maltol from the solution and the alkali or alkaline earth metal halide.
In the above prior art, in separating crude maltol (or ethyl maltol), the object of treatment is a primary isolate comprising the hydrolysis product of maltol. After obtaining maltol by sublimation purification, since the melting point and the like of organic impurities are similar to those of maltol (or ethyl maltol), the difficulty of separation is great, and an effective means for separating a small amount of organic impurities in the maltol or ethyl maltol obtained by sublimation is lacking at low cost.
Disclosure of Invention
The invention aims to solve the technical problem of providing a method for stripping and purifying a crude product after maltol or ethyl maltol is sublimated, which can efficiently remove the irritant impurities in the crude product after maltol or ethyl maltol is sublimated.
In order to solve the technical problems, the invention provides a method for stripping and purifying a crude product after maltol or ethyl maltol is sublimated, which comprises the following steps:
(1) Adding maltol or ethyl maltol into a dissolution kettle, and then adding pure water, wherein the mass ratio of the maltol or ethyl maltol to the water is 1:6, heating to 80+/-5 ℃ by steam after the feeding is finished to dissolve materials;
(2) After the dissolution is finished, transferring the materials in the dissolution kettle to a layering tank for standing for 10min, layering, separating out impurities at the lower layer, putting the upper layer aqueous solution layer into a freezing kettle for cooling, cooling to 10-15 ℃, centrifuging by a centrifuge to obtain the purified maltol or ethyl maltol crystals, returning the centrifuged mother liquor to the step (1) for dissolution and application until the impurity content in the mother liquor exceeds the index, and discharging the mother liquor out of the system.
A method for stripping and purifying crude products after maltol or ethyl maltol sublimates comprises the following steps:
step 1: heating the crude product after the sublimation of the maltol or the ethyl maltol and water to 80+/-5 ℃ for dissolving;
step 2: layering and standing the material obtained in the step 1, separating an upper layer aqueous solution, and then reducing the temperature of the upper layer aqueous solution layer to 10-15 ℃;
step 3: centrifuging to obtain the maltol or ethyl maltol crystal after impurity removal.
Further, the mass ratio of the maltol or ethyl maltol to the water is 1:6.
further, the device comprises a dissolution kettle, a layering tank connected with the dissolution kettle, a freezing kettle connected with the layering tank, and a centrifuge connected with the freezing kettle.
Further, the material dissolving kettle is an enamel material dissolving kettle; the layering groove is an enamel layering groove, the upper part is a round end socket, and the bottom part is conical; the freezing kettle is an enamel freezing kettle.
For the sake of simple explanation, the method for purifying crude product after sublimation of maltol or ethyl maltol is hereinafter referred to as the method.
The method has the advantages that: 1. the characteristic that water and the irritant impurities are not mutually dissolved is utilized, and the water is utilized for back extraction, so that a large amount of impurities can be removed efficiently; 2. in order to increase the solubility of the maltol or the ethyl maltol in water, a heating mode is adopted, so that the water consumption is greatly reduced, and the maltol or the ethyl maltol can be realized: less used amount of water = 1:6; less water is used to facilitate subsequent separation and reduce water pollution and waste. 3. The water-soluble impurities in the maltol or ethyl maltol aqueous solution obtained after layering are less, so that the maltol or ethyl maltol aqueous solution can be reused for multiple times, and the treatment difficulty of mother liquor wastewater is reduced.
Fig. 1 is a flow chart of the present invention.
Wherein 1-a dissolution kettle; 2-layering grooves; 3-freezing the kettle; 4-a centrifuge; a-crude product; b-mother liquor recycling; c-mother liquor; d, sewage treatment; e-ethyl malt flour.
The maltol has a melting point of 159-162 ℃ and can volatilize with water vapor, sublimate at 93 ℃ and dissolve in water at normal temperature by about 1.2 weight percent. Ethyl maltol has a melting point of 89-93 ℃, is volatile at normal temperature, and is dissolved in water at about 1.6% by weight at normal temperature. Maltol and ethyl maltol have low solubility at normal temperature. The crude product obtained after sublimation is not high in absolute content of organic impurities, but these impurities lead to maltol which does not meet quality standards in terms of odor and color. These impurities are also difficult to remove by conventional means.
Maltol and ethyl maltol show good solubility in polar solvents such as acetone, alcohols, etc. However, these solvents are water-soluble and may dissolve not only maltol but also other organic impurities. Meanwhile, because of the easy volatilization, if the solvents are used for purifying the maltol and the ethyl maltol, the solvents can carry away more maltol and ethyl maltol during distillation separation, and more impurities can be introduced after the maltol and the ethyl maltol are condensed and crystallized.
Maltol and ethyl maltol are insoluble in non-polar hydrocarbons, which makes extraction of maltol and ethyl maltol using these solvents difficult.
In the practice of organizing the industrial production of maltol, the inventors found that impurities in maltol are mainly nonpolar impurities, and considering that the solubility difference between maltol and ethyl maltol in water is large at different high and low temperatures, maltol and ethyl maltol are firstly dissolved in hot water under stirring conditions, then kept at temperature, and after standing and layering, organic phases are removed, and then maltol and ethyl maltol aqueous solution are cooled and centrifugally separated by utilizing the solubility difference between maltol and ethyl maltol in water at different temperatures. This process is in fact a process in which maltol and ethyl maltol are returned from the loaded organic phase (or impurity) to the aqueous phase. The inventor obtains high-quality maltol and ethyl maltol products by the method, and has no new impurity introduced and low cost.
Embodiment one:
referring to fig. 1, a method for stripping and purifying a crude product after sublimation of ethyl maltol comprises the following steps:
(1) Adding ethyl maltol into a dissolution kettle 1, and adding pure water, wherein the mass ratio of the ethyl maltol to the water is 1:6, heating the mixture to 75 ℃ by opening steam after the material feeding is finished, and dissolving the mixture;
(2) After the dissolution is finished, transferring the materials in the dissolution kettle 1 to a layering tank 2, standing for 10min, layering, separating out impurities at the lower layer, putting an upper layer aqueous solution layer into a freezing kettle 3, cooling to 10 ℃, centrifuging by using a centrifuge 4 to obtain purified ethyl maltol crystals, returning the centrifuged mother liquor to the step (1) for dissolution and application, and discharging the mother liquor after the impurity content in the mother liquor exceeds the index.
The recovery rate of the recovered ethyl maltol is 93.2% and the purity of the recovered maltol is 99.2% after detection.
Embodiment two:
referring to fig. 1, a method for stripping and purifying a crude product after sublimation of ethyl maltol comprises the following steps:
(1) Adding ethyl maltol into a dissolution kettle 1, and adding pure water, wherein the mass ratio of the ethyl maltol to the water is 1:6, heating the mixture to 80 ℃ by opening steam after the material feeding is finished, and dissolving the mixture;
(2) After the dissolution is finished, transferring the materials in the dissolution kettle 1 to a layering tank 2, standing for 10min, layering, separating out impurities at the lower layer, putting an upper layer aqueous solution layer into a freezing kettle 3, cooling to 12.5 ℃, centrifuging by using a centrifuge 4 to obtain purified ethyl maltol crystals, returning the centrifuged mother liquor to the step (1) for dissolution and application, and discharging the mother liquor after the impurity content in the mother liquor exceeds the index.
The recovery rate of the recovered ethyl maltol is 94.5% and the purity of the recovered maltol is 99.3% after detection.
Embodiment III:
referring to fig. 1, a method for stripping and purifying a crude product after sublimation of ethyl maltol comprises the following steps:
(1) Adding ethyl maltol into a dissolution kettle 1, and adding pure water, wherein the mass ratio of the ethyl maltol to the water is 1:6, opening steam after the feeding is finished, and heating to 85 ℃ to dissolve the materials;
(2) After the dissolution is finished, transferring the materials in the dissolution kettle 1 to a layering tank 2, standing for 10min, layering, separating out impurities at the lower layer, putting an upper layer aqueous solution layer into a freezing kettle 3, cooling to 15 ℃, centrifuging by using a centrifuge 4 to obtain purified ethyl maltol crystals, returning the centrifuged mother liquor to the step (1) for dissolution and application, and discharging the mother liquor after the impurity content in the mother liquor exceeds the index.
The recovery rate of the recovered ethyl maltol is 94.3% and the purity of the recovered maltol is 99.1% after detection.
Embodiment four:
referring to fig. 1, a method for stripping and purifying a crude product after maltol sublimation comprises the following steps:
(1) Adding maltol into a dissolution kettle 1, and adding pure water, wherein the mass ratio of the maltol to the water is 1:6, heating the mixture to 75 ℃ by opening steam after the material feeding is finished, and dissolving the mixture;
(2) After the dissolution is finished, transferring the materials in the dissolution kettle 1 to a layering tank 2, standing for 10min, layering, separating out impurities at the lower layer, putting an upper layer aqueous solution layer into a freezing kettle 3, cooling to 12 ℃, centrifuging by using a centrifuge 4 to obtain maltol crystals after impurity removal, returning the centrifuged mother liquor to the step (1) for dissolution, and discharging the mother liquor after impurity content in the mother liquor exceeds the index.
The recovery rate of the recovered maltol is 92.5% and the purity of the recovered maltol is 99.2% after detection.
Fifth embodiment:
referring to fig. 1, a method for stripping and purifying a crude product after maltol sublimation comprises the following steps:
(1) Adding maltol into a dissolution kettle 1, and adding pure water, wherein the mass ratio of the maltol to the water is 1:6, opening steam after the feeding is finished, and heating to 85 ℃ to dissolve the materials;
(2) After the dissolution is finished, transferring the materials in the dissolution kettle 1 to a layering tank 2, standing for 10min, layering, separating out impurities at the lower layer, putting an upper layer aqueous solution layer into a freezing kettle 3, cooling to 14 ℃, centrifuging by a centrifuge 4 to obtain maltol crystals after impurity removal, returning the centrifuged mother liquor to the step (1) for dissolution, and discharging the mother liquor after impurity content in the mother liquor exceeds the index.
The recovery rate of the recovered maltol is 93.2% and the purity of the recovered maltol is 99.3% after detection.
In the above embodiment:
the material dissolving kettle adopts an enamel material dissolving kettle with a jacket and stirring; the layering groove adopts an enamel layering groove (an upper round seal head and a bottom cone); the freezing kettle adopts an enamel freezing kettle with a jacket and stirring.
In the prior art solvents are generally used to dissolve the sublimated products of maltol and ethyl maltol, followed by separation of the maltol and ethyl maltol in the water. The present invention differs from the prior art in that the present invention uses heated water to dissolve the maltol and ethyl maltol, does not use solvents that are possibly miscible with non-polar organics, and after stripping the maltol and ethyl maltol into the water, removes the organic phase. Compared with the solvent decolorization purification method, the method can perform decolorization purification, saves the use of a decolorizer, consumes energy and the like similar to the original method, and can perform innocent treatment after a small amount of impurities are separated; compared with the sublimated crude product, the method has low energy consumption. Compared with the solvent decolorization purification method or the sublimation method for processing the crude product, the method has high yield.
The foregoing is merely a specific implementation of the present application and other modifications and variations can be made by those skilled in the art based on the above-described examples in light of the above teachings. It is to be understood by persons skilled in the art that the foregoing detailed description is provided for the purpose of illustrating the present application and that the scope of the present application is to be controlled by the scope of the appended claims.
Furthermore, those skilled in the art will appreciate that while some embodiments described herein include some features but not others included in other embodiments, combinations of features of different embodiments are meant to be within the scope of the present application and form different embodiments. For example, in the following claims, any of the claimed embodiments can be used in any combination.
Claims (4)
- A method for stripping and purifying a crude product after subliming maltol or ethyl maltol is characterized by comprising the following steps:step 1: heating the crude product after the sublimation of the maltol or the ethyl maltol and water to 80+/-5 ℃ for dissolving;step 2: layering and standing the material obtained in the step 1, separating an upper layer aqueous solution, and then reducing the temperature of the upper layer aqueous solution layer to 10-15 ℃;step 3: centrifuging to obtain the maltol or ethyl maltol crystal after impurity removal.
- The method for purifying crude product back extraction after sublimation of maltol or ethyl maltol according to claim 1, wherein the mass ratio of maltol or ethyl maltol to water is 1:6.
- the purification device for crude product back extraction after maltol or ethyl maltol sublimates is characterized by comprising a dissolving kettle, a layering tank connected with the dissolving kettle, a freezing kettle connected with the layering tank and a centrifuge connected with the freezing kettle.
- A purification device for stripping crude products after subliming maltol or ethyl maltol according to claim 3, wherein the dissolution kettle is an enamel dissolution kettle; the layering groove is an enamel layering groove, the upper part is a round end socket, and the bottom part is conical; the freezing kettle is an enamel freezing kettle.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011442712.0 | 2020-12-11 | ||
| CN202011442712.0A CN112574156A (en) | 2020-12-11 | 2020-12-11 | Back extraction purification method for crude product after ethyl maltol sublimation |
| PCT/CN2021/137215 WO2022122028A1 (en) | 2020-12-11 | 2021-12-10 | Method and device for back-extraction purification of crude product obtained by sublimation of maltol or ethyl maltol |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN116348185A true CN116348185A (en) | 2023-06-27 |
Family
ID=75130762
Family Applications (2)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202011442712.0A Pending CN112574156A (en) | 2020-12-11 | 2020-12-11 | Back extraction purification method for crude product after ethyl maltol sublimation |
| CN202180065864.XA Pending CN116348185A (en) | 2020-12-11 | 2021-12-10 | Method and device for back-extraction purification of crude product after sublimation of maltol or ethyl maltol |
Family Applications Before (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202011442712.0A Pending CN112574156A (en) | 2020-12-11 | 2020-12-11 | Back extraction purification method for crude product after ethyl maltol sublimation |
Country Status (2)
| Country | Link |
|---|---|
| CN (2) | CN112574156A (en) |
| WO (1) | WO2022122028A1 (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112574156A (en) * | 2020-12-11 | 2021-03-30 | 安徽金禾实业股份有限公司 | Back extraction purification method for crude product after ethyl maltol sublimation |
| CN114437009A (en) * | 2022-02-10 | 2022-05-06 | 河北省天利海香精香料有限公司 | Method for separating and purifying ethyl maltol |
| CN117288003A (en) * | 2023-10-26 | 2023-12-26 | 滁州金沃生物科技有限公司 | Device and method for improving heat exchange efficiency of chlorination reaction heat exchanger in maltol production |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CA2259481A1 (en) * | 1998-02-09 | 1999-08-09 | Kemestrie Inc. | Direct extraction and/or purification of high purity maltol and essential oils by sublimation process |
| US5939565A (en) * | 1997-11-03 | 1999-08-17 | Cultor Food Science, Inc. | Recovery of γ-pyrones |
| CN101993428A (en) * | 2010-11-10 | 2011-03-30 | 广东省肇庆香料厂有限公司 | Method for purifying ethyl maltol |
| CN104387355A (en) * | 2014-09-27 | 2015-03-04 | 安徽金禾实业股份有限公司 | Ethyl maltol crystallization mother liquor recovery method |
| CN105906597A (en) * | 2016-05-11 | 2016-08-31 | 广东省肇庆香料厂有限公司 | Synthetic process of ethyl maltol |
| CN108299362A (en) * | 2018-01-13 | 2018-07-20 | 安徽金禾实业股份有限公司 | A method of impurity in separation maltol crude product |
| CN112574156A (en) * | 2020-12-11 | 2021-03-30 | 安徽金禾实业股份有限公司 | Back extraction purification method for crude product after ethyl maltol sublimation |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3832357A (en) * | 1971-05-26 | 1974-08-27 | Daicel Ltd | Process for preparation of 3-hydroxy-2-alkyl-4-pyrone |
| CN101585822B (en) * | 2009-06-26 | 2011-05-18 | 滁州学院 | Ethyl maltol synthetic method |
| CN103570658A (en) * | 2013-11-01 | 2014-02-12 | 安徽金禾实业股份有限公司 | Decolorizing and recrystallizing method of methyl maltol |
-
2020
- 2020-12-11 CN CN202011442712.0A patent/CN112574156A/en active Pending
-
2021
- 2021-12-10 WO PCT/CN2021/137215 patent/WO2022122028A1/en active Application Filing
- 2021-12-10 CN CN202180065864.XA patent/CN116348185A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5939565A (en) * | 1997-11-03 | 1999-08-17 | Cultor Food Science, Inc. | Recovery of γ-pyrones |
| CA2259481A1 (en) * | 1998-02-09 | 1999-08-09 | Kemestrie Inc. | Direct extraction and/or purification of high purity maltol and essential oils by sublimation process |
| CN101993428A (en) * | 2010-11-10 | 2011-03-30 | 广东省肇庆香料厂有限公司 | Method for purifying ethyl maltol |
| CN104387355A (en) * | 2014-09-27 | 2015-03-04 | 安徽金禾实业股份有限公司 | Ethyl maltol crystallization mother liquor recovery method |
| CN105906597A (en) * | 2016-05-11 | 2016-08-31 | 广东省肇庆香料厂有限公司 | Synthetic process of ethyl maltol |
| CN108299362A (en) * | 2018-01-13 | 2018-07-20 | 安徽金禾实业股份有限公司 | A method of impurity in separation maltol crude product |
| CN112574156A (en) * | 2020-12-11 | 2021-03-30 | 安徽金禾实业股份有限公司 | Back extraction purification method for crude product after ethyl maltol sublimation |
Non-Patent Citations (1)
| Title |
|---|
| 李士雨: "乙基麦芽酚精制技术的改进", 化学工业与工程, no. 01, 15 February 1995 (1995-02-15), pages 50 - 53 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN112574156A (en) | 2021-03-30 |
| WO2022122028A1 (en) | 2022-06-16 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN116348185A (en) | Method and device for back-extraction purification of crude product after sublimation of maltol or ethyl maltol | |
| CN109956983B (en) | Method for extracting sucralose-6-ethyl ester | |
| JP2004358466A5 (en) | ||
| CN106674292B (en) | A kind of purification processing method of Sucralose water crystallization mother liquor | |
| CN102781913A (en) | Method of manufacturing epsilon-caprolactam | |
| RU2004117062A (en) | EXTRACTION METHOD FOR REMOVING IMPURITIES FROM AQUEOUS MIXTURE | |
| US10265641B2 (en) | Simultaneous recovery of organic compounds and extractants | |
| CN101049980A (en) | Method for comprehensive utilization for benzene extracting concentrated solution of residue wastewater | |
| CN110724045A (en) | Preparation method of curcumin with low solvent residue | |
| JPH04228084A (en) | Recovery of citric acid | |
| CN106146374B (en) | A method of recycling cyclohexanone oxime vapour phase rearrangement product fractionation weight raffinate | |
| CN103724288A (en) | Post-processing method for preparing 1H-tetrazole-1-acetic acid through triethyl orthoformate method | |
| FR2470762A1 (en) | PROCESS FOR TREATING AN ADIPIC ACID PRODUCTION RESIDUE | |
| JPH0433440B2 (en) | ||
| CN102464898A (en) | Method for recovering yellow ginger pigment from yellow ginger hydrolysate saponin extraction waste liquid | |
| WO2022233040A1 (en) | Method for purifying sucralose-6-ethyl ester | |
| US2234269A (en) | Method of extracting sulphur | |
| WO2009064037A1 (en) | Recovery of catalysts, benzoic acid and aromatic acid | |
| CN110270582B (en) | Treatment device and process for solid waste residues in nitromethane production | |
| JPH10500941A (en) | Purification of amidocarboxylic acid | |
| CN108409536B (en) | Method for recovering pentaerythritol from alcohol hydrolysis liquid filter residue of antioxidant 1010 mother liquor | |
| US2608560A (en) | Method for isolation and purification of active plant principles | |
| CN105017153A (en) | Method for refining caprolactam | |
| US1762979A (en) | Process of recovering resorcinol | |
| CN110386877B (en) | Separation method of hydrolysis mixture |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |