CN112574156A - Back extraction purification method for crude product after ethyl maltol sublimation - Google Patents
Back extraction purification method for crude product after ethyl maltol sublimation Download PDFInfo
- Publication number
- CN112574156A CN112574156A CN202011442712.0A CN202011442712A CN112574156A CN 112574156 A CN112574156 A CN 112574156A CN 202011442712 A CN202011442712 A CN 202011442712A CN 112574156 A CN112574156 A CN 112574156A
- Authority
- CN
- China
- Prior art keywords
- ethyl maltol
- material dissolving
- mother liquor
- kettle
- 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
- YIKYNHJUKRTCJL-UHFFFAOYSA-N Ethyl maltol Chemical compound CCC=1OC=CC(=O)C=1O YIKYNHJUKRTCJL-UHFFFAOYSA-N 0.000 title claims abstract description 38
- 229940093503 ethyl maltol Drugs 0.000 title claims abstract description 38
- 238000000034 method Methods 0.000 title claims abstract description 15
- 239000012043 crude product Substances 0.000 title claims abstract description 13
- 238000000605 extraction Methods 0.000 title claims abstract description 12
- 238000000746 purification Methods 0.000 title claims abstract description 11
- 238000000859 sublimation Methods 0.000 title description 3
- 230000008022 sublimation Effects 0.000 title description 3
- 239000000463 material Substances 0.000 claims abstract description 35
- 239000012535 impurity Substances 0.000 claims abstract description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000012452 mother liquor Substances 0.000 claims abstract description 19
- 238000007710 freezing Methods 0.000 claims abstract description 8
- 230000008014 freezing Effects 0.000 claims abstract description 8
- 238000001816 cooling Methods 0.000 claims abstract description 6
- 239000013078 crystal Substances 0.000 claims abstract description 6
- 238000007599 discharging Methods 0.000 claims abstract description 6
- 239000002085 irritant Substances 0.000 abstract description 3
- 231100000021 irritant Toxicity 0.000 abstract description 3
- 210000003298 dental enamel Anatomy 0.000 description 3
- 238000004090 dissolution Methods 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 2
- 238000009835 boiling Methods 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000004065 wastewater treatment 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 invention relates to a back extraction purification method of a sublimed crude product of ethyl maltol, which comprises the following steps: (1) adding ethyl maltol into the material dissolving kettle, and then adding pure water, wherein the mass ratio of the ethyl maltol to the water is 1:6, after the feeding is finished, starting steam to heat to 80 +/-5 ℃ for material dissolving; (2) and (3) after the material dissolving is finished, transferring the material in the material dissolving kettle to a layering tank, standing for 10min, layering, separating out impurities on the lower layer, putting the water solution layer on the upper layer into a freezing kettle, cooling to 10-15 ℃, centrifuging by using a centrifuge to obtain ethyl maltol crystals after impurity removal, returning the centrifuged mother liquor to the step (1) for material dissolving and applying, and discharging the mother liquor out of the system when the impurity content in the mother liquor exceeds the index. The method can efficiently remove the irritant impurities in the crude product after the ethyl maltol is sublimated.
Description
Technical Field
The invention relates to a back extraction purification method of a sublimed crude product of ethyl maltol.
Background
In the production reaction process of ethyl maltol, a large amount of byproducts are generated, wherein part of impurities with pungent odor and close to the boiling point of ethyl maltol are evaporated out along with the ethyl maltol in a sublimation purification section, and are very easy to dissolve mutually and difficult to separate, so that the quality of the ethyl maltol product is difficult to improve.
Disclosure of Invention
The invention aims to solve the technical problem of providing a back extraction purification method for the sublimed crude product of ethyl maltol, which can efficiently remove irritant impurities in the sublimed crude product of ethyl maltol.
In order to solve the technical problem, the invention provides a back extraction purification method of a sublimed crude product of ethyl maltol, which comprises the following steps:
(1) adding ethyl maltol into the material dissolving kettle, and then adding pure water, wherein the mass ratio of the ethyl maltol to the water is 1:6, after the feeding is finished, starting steam to heat to 80 +/-5 ℃ for material dissolving;
(2) and (3) after the material dissolving is finished, transferring the material in the material dissolving kettle to a layering tank, standing for 10min, layering, separating out impurities on the lower layer, putting the water solution layer on the upper layer into a freezing kettle, cooling to 10-15 ℃, centrifuging by using a centrifuge to obtain ethyl maltol crystals after impurity removal, returning the centrifuged mother liquor to the step (1) for material dissolving and applying, and discharging the mother liquor out of the system when the impurity content in the mother liquor exceeds the index.
For the sake of simplicity of explanation, the method for purifying the sublimed ethyl maltol by back-extraction of the crude product is simply referred to as the present method.
The method has the advantages that: 1. the characteristic that water and irritant impurities are immiscible is utilized, and water is utilized for back extraction, so that a large amount of impurities can be efficiently removed; 2. in order to increase the solubility of ethyl maltol in water, a heating mode is adopted, so that the using amount of water is greatly reduced, and the method can realize that the ethyl maltol: water = minimum usage of 1: 6. 3. The ethyl maltol aqueous solution obtained after layering contains less water-soluble impurities, so that repeated application can be realized, and the difficulty in mother liquor wastewater treatment is reduced.
Drawings
FIG. 1 is a flow chart of the present invention.
Detailed Description
The first embodiment is as follows:
referring to fig. 1, a method for back extraction and purification of a sublimed crude product of ethyl maltol comprises the following steps:
(1) adding ethyl maltol into the dissolving kettle 1, and then adding pure water, wherein the mass ratio of the ethyl maltol to the water is 1:6, after the feeding is finished, starting steam to heat to 75 ℃ for material dissolution;
(2) after the material dissolving is finished, transferring the material in the material dissolving kettle 1 to a layering tank 2, standing for 10min, layering, separating impurities on the lower layer, putting the water solution layer on the upper layer into a freezing kettle 3, cooling to 10 ℃, centrifuging by using a centrifuge 4 to obtain ethyl maltol crystals after impurity removal, returning the centrifuged mother liquor to the step (1) for material dissolving and applying, and discharging the mother liquor after the impurity content in the mother liquor exceeds the index.
The first embodiment is as follows:
referring to fig. 1, a method for back extraction and purification of a sublimed crude product of ethyl maltol comprises the following steps:
(1) adding ethyl maltol into the dissolving kettle 1, and then adding pure water, wherein the mass ratio of the ethyl maltol to the water is 1:6, after the feeding is finished, starting steam to heat to 80 ℃ for material dissolution;
(2) after the material dissolving is finished, transferring the material in the material dissolving kettle 1 to a layering tank 2, standing for 10min, layering, separating impurities on the lower layer, putting the upper layer aqueous solution layer into a freezing kettle 3, cooling to 12.5 ℃, then centrifuging by using a centrifuge 4 to obtain ethyl maltol crystals after impurity removal, returning the centrifuged mother liquor to the step (1) for material dissolving and applying, and discharging the mother liquor after the impurity content in the mother liquor exceeds the index.
The first embodiment is as follows:
referring to fig. 1, a method for back extraction and purification of a sublimed crude product of ethyl maltol comprises the following steps:
(1) adding ethyl maltol into the dissolving kettle 1, and then adding pure water, wherein the mass ratio of the ethyl maltol to the water is 1:6, after the feeding is finished, starting steam to heat to 85 ℃ for material dissolution;
(2) after the material dissolving is finished, transferring the material in the material dissolving kettle 1 to a layering tank 2, standing for 10min, layering, separating impurities on the lower layer, putting the water solution layer on the upper layer into a freezing kettle 3, cooling to 15 ℃, centrifuging by using a centrifuge 4 to obtain ethyl maltol crystals after impurity removal, returning the centrifuged mother liquor to the step (1) for material dissolving and applying, and discharging the mother liquor after the impurity content in the mother liquor exceeds the index.
In the above embodiment:
the material dissolving kettle is an enamel material dissolving kettle with a jacket and stirring;
the layering tank adopts an enamel layering tank (a circular end socket at the upper part and a conical bottom part);
the freezing kettle adopts an enamel freezing kettle with a jacket and a stirrer.
Claims (1)
1. The method for back extraction and purification of the sublimed crude product of ethyl maltol is characterized by comprising the following steps of:
(1) adding ethyl maltol into the material dissolving kettle, and then adding pure water, wherein the mass ratio of the ethyl maltol to the water is 1:6, after the feeding is finished, starting steam to heat to 80 +/-5 ℃ for material dissolving;
(2) and (3) after the material dissolving is finished, transferring the material in the material dissolving kettle to a layering tank, standing for 10min, layering, separating out impurities on the lower layer, putting the water solution layer on the upper layer into a freezing kettle, cooling to 10-15 ℃, centrifuging by using a centrifuge to obtain ethyl maltol crystals after impurity removal, returning the centrifuged mother liquor to the step (1) for material dissolving and applying, and discharging the mother liquor out of the system when the impurity content in the mother liquor exceeds the index.
Priority Applications (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011442712.0A CN112574156A (en) | 2020-12-11 | 2020-12-11 | Back extraction purification method for crude product after ethyl maltol sublimation |
| CN202180065864.XA 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 |
| 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 |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011442712.0A CN112574156A (en) | 2020-12-11 | 2020-12-11 | Back extraction purification method for crude product after ethyl maltol sublimation |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN112574156A true CN112574156A (en) | 2021-03-30 |
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 After (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| 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 |
Country Status (2)
| Country | Link |
|---|---|
| CN (2) | CN112574156A (en) |
| WO (1) | WO2022122028A1 (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| WO2022122028A1 (en) * | 2020-12-11 | 2022-06-16 | 安徽金禾实业股份有限公司 | Method and device for back-extraction purification of crude product obtained by sublimation of maltol or ethyl maltol |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117288003B (en) * | 2023-10-26 | 2024-10-01 | 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 (6)
| 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 |
| CN101585822A (en) * | 2009-06-26 | 2009-11-25 | 滁州学院 | Ethyl maltol synthetic method |
| 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 |
| 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 |
| 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 |
Family Cites Families (4)
| 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 |
| CN108299362B (en) * | 2018-01-13 | 2021-07-09 | 安徽金禾实业股份有限公司 | Method for separating impurities in 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 |
-
2020
- 2020-12-11 CN CN202011442712.0A patent/CN112574156A/en active Pending
-
2021
- 2021-12-10 CN CN202180065864.XA patent/CN116348185A/en active Pending
- 2021-12-10 WO PCT/CN2021/137215 patent/WO2022122028A1/en active Application Filing
Patent Citations (6)
| 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 |
| CN101585822A (en) * | 2009-06-26 | 2009-11-25 | 滁州学院 | Ethyl maltol synthetic method |
| 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 |
| 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 |
| 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 |
Non-Patent Citations (2)
| Title |
|---|
| 刘新宇: ""一滴香"中乙基麦芽酚和1，2-丙二醇的含量测定及其安全性评价研究", 《中国优秀博硕士学位论文全文数据库(硕士)工程科技Ⅰ辑》 * |
| 孙君社 编: "《食品风味化学》", 30 November 1990, 华中理工大学出版 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2022122028A1 (en) * | 2020-12-11 | 2022-06-16 | 安徽金禾实业股份有限公司 | Method and device for back-extraction purification of crude product obtained by sublimation of maltol or ethyl maltol |
| CN116348185A (en) * | 2020-12-11 | 2023-06-27 | 安徽金禾实业股份有限公司 | Method and device for back-extraction purification of crude product after sublimation of maltol or ethyl maltol |
| 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 |
Also Published As
| Publication number | Publication date |
|---|---|
| CN116348185A (en) | 2023-06-27 |
| WO2022122028A1 (en) | 2022-06-16 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN112574156A (en) | Back extraction purification method for crude product after ethyl maltol sublimation | |
| AU2012356848B2 (en) | Lactic acid extraction | |
| JP6207522B2 (en) | Purification of vanillin by liquid-liquid extraction | |
| RU2004117063A (en) | EXTRACTION METHOD FOR EXTRACTION OF IMPURITIES FROM THE UTERINE SOLUTION IN THE SYNTHESIS OF CARBONIC ACID | |
| JP2018012720A (en) | Recovery and refining of dianhydrosugar | |
| CN110402250B (en) | Method for extracting phytosterol from tall oil pitch | |
| CN113548651A (en) | Method for purifying wet-process phosphoric acid by solvent extraction | |
| CN111592453B (en) | Method for removing/recovering organic solvent in long-chain dibasic acid | |
| CN104876847B (en) | Method for extracting indole from methyl naphthalene fraction | |
| CN102633293B (en) | Method for refining multistage circulation evaporation-free copper sulfate | |
| CN110066249B (en) | Novel caprolactam refining and purifying method | |
| CN111315830A (en) | Method for preparing high-purity low-harm lycopene crystal | |
| CN107382694B (en) | Method for recovering phenylacetic acid from penicillin potassium lysate | |
| CN108976128B (en) | Preparation method of 2-nitro-2-methyl-1-propanol crystal | |
| CN103571633A (en) | Esterification-ultrahigh pressure crystallization separation method for distillate of vegetable oil | |
| CN211752616U (en) | Caprolactam device is refined in crystallization | |
| CN105061521A (en) | Extraction method of high-purity L-arabinose | |
| CN115057818B (en) | Process for refining aminopyrine crude product | |
| CN109456172B (en) | Method for purifying dodecanedioic acid in water phase | |
| US11623905B2 (en) | Isolation and crystallization of cannabinoids without distillation or evaporation of solvents | |
| CN110386877B (en) | Separation method of hydrolysis mixture | |
| CN110872540B (en) | Method for extracting unsaturated fatty acid | |
| CN111517918B (en) | Preparation method of D-mannitol alpha crystal form | |
| CN120004761A (en) | A kind of preparation method and system of L-carnenitrile | |
| CN120289402A (en) | A method for continuous purification of ethyl maltol |
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 | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20210330 |
|
| RJ01 | Rejection of invention patent application after publication |