CN115872847B - Purification device and purification method for rinsing methyl cyclopentenolone crude product - Google Patents
Purification device and purification method for rinsing methyl cyclopentenolone crude product Download PDFInfo
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- CN115872847B CN115872847B CN202211441818.8A CN202211441818A CN115872847B CN 115872847 B CN115872847 B CN 115872847B CN 202211441818 A CN202211441818 A CN 202211441818A CN 115872847 B CN115872847 B CN 115872847B
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- Prior art keywords
- kettle
- ethanol
- decoloring
- methyl cyclopentenolone
- freezing
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- CFAKWWQIUFSQFU-UHFFFAOYSA-N 2-hydroxy-3-methylcyclopent-2-en-1-one Chemical compound CC1=C(O)C(=O)CC1 CFAKWWQIUFSQFU-UHFFFAOYSA-N 0.000 title claims abstract description 43
- 239000012043 crude product Substances 0.000 title claims abstract description 23
- 238000000746 purification Methods 0.000 title claims abstract description 21
- 238000000034 method Methods 0.000 title claims abstract description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 80
- 238000001816 cooling Methods 0.000 claims abstract description 32
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 28
- 238000007710 freezing Methods 0.000 claims abstract description 26
- 230000008014 freezing Effects 0.000 claims abstract description 26
- 238000001035 drying Methods 0.000 claims abstract description 20
- 239000000047 product Substances 0.000 claims abstract description 12
- 239000000203 mixture Substances 0.000 claims description 30
- 238000010438 heat treatment Methods 0.000 claims description 10
- 239000007787 solid Substances 0.000 claims description 10
- 239000007788 liquid Substances 0.000 claims description 4
- 230000005484 gravity Effects 0.000 claims description 3
- 238000005086 pumping Methods 0.000 claims description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 17
- 229910052799 carbon Inorganic materials 0.000 abstract description 9
- 239000012452 mother liquor Substances 0.000 abstract description 3
- 239000010865 sewage Substances 0.000 abstract description 3
- 238000004321 preservation Methods 0.000 abstract 1
- 238000005265 energy consumption Methods 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- 239000002699 waste material Substances 0.000 description 3
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 239000002920 hazardous waste Substances 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
Classifications
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The purifying device for rinsing the crude methyl cyclopentenolone comprises an ethanol tank, a decoloring kettle, a water cooling kettle and a freezing kettle which are sequentially connected, wherein a centrifugal machine and a dryer are further arranged beside the freezing kettle. The purification method comprises the following steps: the bottom of the ethanol tank is conveyed to a decoloring kettle through a metering pump, ethanol is added after the methyl cyclopentenolone crude product is added into the decoloring kettle according to the proportion of the methyl cyclopentenolone crude product, the temperature is raised to 85 ℃, and the decoloring kettle is placed into a water cooling kettle after heat preservation for 2 hours. And then cooling by opening circulating water, putting the cooled circulating water into a freezing kettle for freezing, centrifuging and then drying to obtain a finished product of methyl cyclopentenolone. The invention uses ethanol to replace active carbon to carry out high-temperature rinsing purification on the methyl cyclopentenolone crude product, the yield reaches 75-80%, the whiteness of the finished product reaches 90%, the cost of active carbon treatment is reduced, meanwhile, the mother liquor reduces the cod therein, and the sewage treatment difficulty is reduced.
Description
Technical Field
The invention relates to a purifying device and a purifying method for rinsing a crude product of methyl cyclopentenolone.
Background
The purification method of the crude methyl cyclopentenolone product generally comprises the steps of dissolving the crude methyl cyclopentenolone product, adding active carbon into the solution to adsorb impurities, filtering out the active carbon, concentrating, crystallizing and drying to obtain the finished methyl cyclopentenolone product. The defect of this mode is that the waste activated carbon not only contains the adsorbed impurities, but also has partial methyl cyclopentenolone adsorbed by the activated carbon, and the waste activated carbon contains about 11% of methyl cyclopentenolone, and the waste activated carbon is generally directly burnt, so that the material loss is caused, and the raw material cost is increased.
Disclosure of Invention
The first technical problem to be solved by the invention is to provide a purifying device for rinsing the crude methylcyclopentenolone, which is used for rinsing the crude methylcyclopentenolone at high temperature by replacing active carbon with ethanol, then freezing, crystallizing and centrifugally drying the crude methylcyclopentenolone, so that the yield of the methylcyclopentenolone is increased.
The second technical problem to be solved by the invention is to provide the purification method of the purification device for rinsing the crude methyl cyclopentenolone, which has the advantages of simple steps, convenient operation, low energy consumption, saving and environmental protection.
In order to solve the first technical problem, the invention provides a purifying device for rinsing crude methyl cyclopentenolone, which comprises an ethanol tank, a decoloring kettle, a water cooling kettle and a freezing kettle, wherein a magnetic flap liquid level meter is arranged in the ethanol tank, the specific gravity of a floater of the magnetic flap liquid level meter is 1.07, a discharge hole of the ethanol tank is connected with the decoloring kettle through a metering pump, the discharge hole of the decoloring kettle is connected with a feed hole of the water cooling kettle, the discharge hole of the water cooling kettle is connected with the feed hole of the freezing kettle, and a centrifugal machine and a dryer are further arranged beside the freezing kettle.
In order to solve the second technical problem, the invention provides a purification method of a purification device for rinsing a crude methyl cyclopentenolone, which comprises the following steps:
(1) Placing ethanol in an ethanol tank, adding a methyl cyclopentenolone crude product into a decoloring kettle, and pumping the ethanol into the decoloring kettle through a metering pump to obtain a mixture, wherein the ratio of the methyl cyclopentenolone crude product to the ethanol is 220L of ethanol per 640kg of methyl cyclopentenolone crude product, and the concentration of the ethanol is 65-85%;
(2) Heating the decoloring kettle to 85 ℃ by using steam, stopping heating and preserving heat for 2 hours;
(3) Introducing the mixture in the decoloring kettle into a water cooling kettle, and cooling the mixture to 45 ℃ by circulating water;
(4) Transferring the mixture from the water cooling kettle to a freezing kettle for cooling;
(5) And when the temperature of the mixture is reduced to 10 ℃ in the freezing kettle, transferring the mixture into a centrifugal machine for centrifugal drying, and finally transferring the solid obtained by the centrifugal drying into a dryer for drying until the solid is absolute dry, thus obtaining the finished product of methyl cyclopentenolone.
The invention has the advantages that: according to the invention, ethanol is used for replacing active carbon to rinse the methyl cyclopentenolone crude product at high temperature, then freezing crystallization and centrifugal drying are carried out, the yield of the methyl cyclopentenolone crude product reaches 75-80%, the whiteness of the finished product reaches 90%, the cost of treating hazardous waste active carbon is correspondingly reduced, meanwhile, the cod in the mother liquor is reduced, and the sewage treatment difficulty is reduced. In addition, the whole purification process method has simple steps, convenient operation, low energy consumption, saving and environmental protection.
Drawings
Fig. 1 is a schematic flow chart of the present invention.
Detailed Description
Referring to fig. 1, a purifying device for rinsing crude methylcyclopentenolone comprises an ethanol tank 1, a decoloring kettle 2, a water cooling kettle 3 and a freezing kettle 4, wherein a magnetic flap level gauge is arranged in the ethanol tank 1, the specific gravity of a floater of the magnetic flap level gauge is 1.07, a discharge port of the ethanol tank 1 is connected with the decoloring kettle 2 through a metering pump, a discharge port of the decoloring kettle 2 is connected with a feed port of the water cooling kettle 3, a discharge port of the water cooling kettle 3 is connected with a feed port of the freezing kettle 4, and a centrifugal machine 5 and a dryer 6 are further arranged beside the freezing kettle 4.
Embodiment one:
the purification method of the purification device for rinsing the crude methyl cyclopentenolone comprises the following steps:
(1) Ethanol is stored in an ethanol tank 1, 640kg of methyl cyclopentenolone crude product is put into a decoloring kettle 2, and then 220L of ethanol is pumped into the decoloring kettle 2 through a metering pump to obtain a mixture, wherein the concentration of the ethanol is 65%;
(2) Heating the decoloring kettle 2 to 85 ℃ by using steam, stopping heating and preserving heat for 2 hours;
(3) Introducing the mixture in the decoloring kettle 2 into a water cooling kettle 3, and cooling the mixture to 45 ℃ by circulating water;
(4) Transferring the mixture from the water cooling kettle 3 to the freezing kettle 4 for cooling;
(5) When the temperature of the mixture is reduced to 10 ℃ in the freezing kettle 4, transferring the mixture into a centrifugal machine 5 for centrifugal drying, transferring the solid obtained by centrifugal drying into a dryer 6 for drying until the solid is absolute, thus obtaining 465kg of methyl cyclopentenolone finished product, and the yield of the crude product is 72%.
Embodiment two:
the purification method of the purification device for rinsing the crude methyl cyclopentenolone comprises the following steps:
(1) Ethanol is stored in an ethanol tank 1, 640kg of methyl cyclopentenolone crude product is put into a decoloring kettle 2, and then 220L of ethanol is pumped into the decoloring kettle 2 through a metering pump to obtain a mixture, wherein the concentration of the ethanol is 75%;
(2) Heating the decoloring kettle 2 to 85 ℃ by using steam, stopping heating and preserving heat for 2 hours;
(3) Introducing the mixture in the decoloring kettle 2 into a water cooling kettle 3, and cooling the mixture to 45 ℃ by circulating water;
(4) Transferring the mixture from the water cooling kettle 3 to the freezing kettle 4 for cooling;
(5) When the temperature of the mixture is reduced to 10 ℃ in the freezing kettle 4, transferring the mixture into a centrifugal machine 5 for centrifugal drying, transferring the solid obtained by centrifugal drying into a dryer 6 for drying until the solid is absolute, and obtaining 490kg of finished methyl cyclopentenolone product, wherein the yield of the crude product is 76%.
Embodiment III:
the purification method of the purification device for rinsing the crude methyl cyclopentenolone comprises the following steps:
(1) Ethanol is stored in an ethanol tank 1, 640kg of methyl cyclopentenolone crude product is put into a decoloring kettle 2, and then 220L of ethanol is pumped into the decoloring kettle 2 through a metering pump to obtain a mixture, wherein the concentration of the ethanol is 85%;
(2) Heating the decoloring kettle 2 to 85 ℃ by using steam, stopping heating and preserving heat for 2 hours;
(3) Introducing the mixture in the decoloring kettle 2 into a water cooling kettle 3, and cooling the mixture to 45 ℃ by circulating water;
(4) Transferring the mixture from the water cooling kettle 3 to the freezing kettle 4 for cooling;
(5) When the temperature of the mixture is reduced to 10 ℃ in the freezing kettle 4, transferring the mixture into a centrifugal machine 5 for centrifugal drying, transferring the solid obtained by centrifugal drying into a dryer 6 for drying until the solid is absolute, and obtaining 520kg of methyl cyclopentenolone finished product, wherein the yield of the crude product is 81%.
The invention has the advantages that: according to the invention, ethanol is used for replacing active carbon to rinse the methyl cyclopentenolone crude product at high temperature, then freezing crystallization and centrifugal drying are carried out, the yield of the methyl cyclopentenolone crude product reaches 75-80%, the whiteness of a finished product reaches 90%, the cost of treating hazardous waste active carbon is correspondingly reduced, meanwhile, the cod in the mother liquor is reduced, and the sewage treatment difficulty is reduced. In addition, the whole purification process method has simple steps, convenient operation, low energy consumption, saving and environmental protection.
Claims (1)
1. The purification method for rinsing the methyl cyclopentenolone crude product comprises an ethanol tank, a decoloring kettle, a water cooling kettle and a freezing kettle, wherein a magnetic flap liquid level meter is arranged in the ethanol tank, the specific gravity of a floater of the magnetic flap liquid level meter is 1.07, a discharge port of the ethanol tank is connected with the decoloring kettle through a metering pump, the discharge port of the decoloring kettle is connected with a feed port of the water cooling kettle, the discharge port of the water cooling kettle is connected with the feed port of the freezing kettle, and a centrifugal machine and a dryer are further arranged beside the freezing kettle, and the purification method is characterized by comprising the following steps:
(1) Placing ethanol in an ethanol tank, adding a methyl cyclopentenolone crude product into a decoloring kettle, and pumping the ethanol into the decoloring kettle through a metering pump to obtain a mixture, wherein the ratio of the methyl cyclopentenolone crude product to the ethanol is 220L of ethanol per 640kg of methyl cyclopentenolone crude product, and the concentration of the ethanol is 65-85%;
(2) Heating the decoloring kettle to 85 ℃ by using steam, stopping heating and preserving heat for 2 hours;
(3) Introducing the mixture in the decoloring kettle into a water cooling kettle, and cooling the mixture to 45 ℃ by circulating water;
(4) Transferring the mixture from the water cooling kettle to a freezing kettle for cooling;
(5) And when the temperature of the mixture is reduced to 10 ℃ in the freezing kettle, transferring the mixture into a centrifugal machine for centrifugal drying, and finally transferring the solid obtained by the centrifugal drying into a dryer for drying until the solid is absolute dry, thus obtaining the finished product of methyl cyclopentenolone.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211441818.8A CN115872847B (en) | 2022-11-17 | 2022-11-17 | Purification device and purification method for rinsing methyl cyclopentenolone crude product |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211441818.8A CN115872847B (en) | 2022-11-17 | 2022-11-17 | Purification device and purification method for rinsing methyl cyclopentenolone crude product |
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| Publication Number | Publication Date |
|---|---|
| CN115872847A CN115872847A (en) | 2023-03-31 |
| CN115872847B true CN115872847B (en) | 2024-03-29 |
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|---|---|---|---|
| CN202211441818.8A Active CN115872847B (en) | 2022-11-17 | 2022-11-17 | Purification device and purification method for rinsing methyl cyclopentenolone crude product |
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| CN (1) | CN115872847B (en) |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101348453A (en) * | 2008-08-29 | 2009-01-21 | 广东肇庆星湖生物科技股份有限公司 | Method for purifying proline |
| 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 |
| CN104193071A (en) * | 2014-09-27 | 2014-12-10 | 安徽金禾实业股份有限公司 | Treating method of high-ammonia-nitrogen mother liquor wastewater in MCP (methyl cyclopentenolone) production |
| CN104370725A (en) * | 2014-09-27 | 2015-02-25 | 安徽金禾实业股份有限公司 | Methyl cyclopentenolone (MCP) rearrangement optimizing production method |
| CN206069735U (en) * | 2016-08-28 | 2017-04-05 | 山东昆达生物科技有限公司 | A kind of sorbic acid production system |
| CN206240280U (en) * | 2016-12-02 | 2017-06-13 | 连云港瑞威化工有限公司 | A kind of methyl cyclopentenyl ketone produces exhaust gas processing device |
| CN108586223A (en) * | 2018-05-28 | 2018-09-28 | 盐城市春竹香料有限公司 | The production technology of purified by crystallisation methyl cyclopentenyl ketone |
| CN112480186A (en) * | 2020-11-30 | 2021-03-12 | 安徽金禾实业股份有限公司 | Method for treating primary mother liquor of sucralose |
-
2022
- 2022-11-17 CN CN202211441818.8A patent/CN115872847B/en active Active
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101348453A (en) * | 2008-08-29 | 2009-01-21 | 广东肇庆星湖生物科技股份有限公司 | Method for purifying proline |
| 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 |
| CN104193071A (en) * | 2014-09-27 | 2014-12-10 | 安徽金禾实业股份有限公司 | Treating method of high-ammonia-nitrogen mother liquor wastewater in MCP (methyl cyclopentenolone) production |
| CN104370725A (en) * | 2014-09-27 | 2015-02-25 | 安徽金禾实业股份有限公司 | Methyl cyclopentenolone (MCP) rearrangement optimizing production method |
| CN206069735U (en) * | 2016-08-28 | 2017-04-05 | 山东昆达生物科技有限公司 | A kind of sorbic acid production system |
| CN206240280U (en) * | 2016-12-02 | 2017-06-13 | 连云港瑞威化工有限公司 | A kind of methyl cyclopentenyl ketone produces exhaust gas processing device |
| CN108586223A (en) * | 2018-05-28 | 2018-09-28 | 盐城市春竹香料有限公司 | The production technology of purified by crystallisation methyl cyclopentenyl ketone |
| CN112480186A (en) * | 2020-11-30 | 2021-03-12 | 安徽金禾实业股份有限公司 | Method for treating primary mother liquor of sucralose |
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| CN115872847A (en) | 2023-03-31 |
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