CN112480032A - Method for recycling secondary mother liquor in acesulfame potassium production - Google Patents
Method for recycling secondary mother liquor in acesulfame potassium production Download PDFInfo
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- CN112480032A CN112480032A CN202011367866.8A CN202011367866A CN112480032A CN 112480032 A CN112480032 A CN 112480032A CN 202011367866 A CN202011367866 A CN 202011367866A CN 112480032 A CN112480032 A CN 112480032A
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- mother liquor
- secondary mother
- filtrate
- hydrolysis
- hydrolysis acid
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D291/00—Heterocyclic compounds containing rings having nitrogen, oxygen and sulfur atoms as the only ring hetero atoms
- C07D291/02—Heterocyclic compounds containing rings having nitrogen, oxygen and sulfur atoms as the only ring hetero atoms not condensed with other rings
- C07D291/06—Six-membered rings
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Abstract
The invention relates to a method for recycling secondary mother liquor in acesulfame potassium production, which is characterized by comprising the following steps: (1) filtering the secondary mother liquor centrifugally thrown out by recrystallization through a plate filter press, collecting crude sugar, removing a decolorization post, and pumping the filtrate to a secondary mother liquor high-level storage tank; (2) in normal production, a secondary mother liquor head tank dripping valve is opened, and materials in the secondary mother liquor head tank are dripped into a hydrolysis acid phase tank; pumping the produced hydrolysis acid into a hydrolysis acid phase groove, carrying out hydrolysis reaction on the filtrate and the hydrolysis acid in the hydrolysis acid phase groove, and controlling the volume ratio of the filtrate to the hydrolysis acid not to exceed 10%; (3) adding 5-15 m of the material in the hydrolysis acid phase tank3The amount of/h is pumped to the extraction system and then to the normal production process. The invention has the advantages that: the process is simple and easy to operate, and the whole process flow can realize automatic control; about 1% of the finished sugar can be filtered again; approximately 1 ton of finished sugar can be added per day; and the subsequent treatment section of mother liquor is reduced.
Description
Technical Field
The invention belongs to the technical field of acesulfame potassium production, and relates to a method for recycling secondary mother liquor in acesulfame potassium production.
Background
Acesulfame potassium is a food additive, similar to saccharin, and is readily soluble in water, with a solubility of 27 grams at 20 deg.C; the sweetener is added to food, is not nutrient, has good taste and no calorie, has the characteristics of no metabolism and no absorption in human bodies (being an ideal sweetener for middle-aged and elderly people, obese patients and diabetic patients), has good heat and acid stability and the like, and is a fourth-generation synthetic sweetener in the world at present.
At present, most of acesulfame potassium are synthesized by the following steps: under the condition that dichloromethane is used as a solvent and triethylamine is used as a catalyst, diketene and sulfamic acid generate an intermediate (acetoacetyl compound) under a certain condition, sulfur trioxide is diluted to a certain concentration and used as a sulfonating agent to react with the intermediate at a low temperature, the intermediate is dehydrated to generate a hexahydric cyclic compound, and acid acesulfame potassium is generated through hydrolysis; neutralizing acid acesulfame potassium with liquid potassium hydroxide solution to generate crude acesulfame potassium; the specific reaction equation is as follows:
at present, a concentration working section in an acesulfame potassium production process evaporates part of water in sugar water (sugar water generated after potassium hydroxide neutralization), then carries out centrifugal treatment after cooling crystallization to obtain crude sugar, generates primary mother liquor, and carries out secondary centrifugation after the primary mother liquor is concentrated, cooled and crystallized to generate secondary mother liquor, wherein the secondary mother liquor originally serves as raffinate to be sent to a triethylamine workshop for waste treatment because the secondary mother liquor contains more impurities and the viscosity of the mother liquor is high, but the secondary mother liquor also contains part of finished sugar (containing 5-10%) and is treated as raffinate, which is a pity.
Disclosure of Invention
The invention aims to solve the problems that a small amount of sugar (5-10%) in secondary mother liquor in the conventional acesulfame potassium production is difficult to recover and cannot be utilized, and provides a method for recovering and utilizing the secondary mother liquor in the acesulfame potassium production.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a method for recycling secondary mother liquor in acesulfame potassium production is characterized by adopting the following devices: the filtering device is connected with the secondary mother liquor head tank and the hydrolysis acid phase tank in sequence;
the method comprises the following steps:
(1) filtering the secondary mother liquor (the content of finished sugar is 5-10%) centrifugally thrown out by recrystallization by a plate filter press, collecting crude sugar, removing a decolorization post, boiling the material, decolorizing, collecting filtrate, and pumping the filtrate to a secondary mother liquor high-level storage tank;
(2) in normal production, a secondary mother liquor head tank dripping valve is opened, and materials in the secondary mother liquor head tank are dripped into a hydrolysis acid phase tank; the hydrolytic acid generated in the production is pumped into a hydrolytic acid phase groove, the filtrate and the hydrolytic acid carry out hydrolysis reaction in the hydrolytic acid phase groove, the dripping process is uniform, the ratio (volume ratio) of the filtrate to the hydrolytic acid is controlled not to exceed 10 percent, and excessive dripping is strictly forbidden (the secondary mother liquor is excessively dripped, so that a large amount of bubbles are generated in the reaction, and the quality of subsequent products is influenced after floccules enter an extraction system);
(3) adding 5-15 m of the material in the hydrolysis acid phase tank3The amount of/h is pumped to the extraction system and then to the normal production process.
Further, the volume ratio of the filtrate to the hydrolytic acid in the step (2) is 3-8%.
Further, the volume ratio of the filtrate to the hydrolytic acid in the step (2) is 5-6%.
Further, the dropping flow rate of the filtrate in the step (2) is 0.5-1.0m3/h。
Further, the flow rate of the hydrolysis acid in the step (2) is 8-10 m3/h。
Further, the dropping flow rate of the filtrate in the step (2) is 0.5-0.8m3/h。
Further, the flow rate of the hydrolysis acid in the step (2) is 8-9 m3/h。
The invention utilizes the neutralization reaction of the acesulfame and the potassium hydroxide which are generated by the hydrolysis reaction to generate the acesulfame potassium, and the acesulfame potassium and the hydrolysis acid phase react to generate the acesulfame potassium again by utilizing the principle of preparing weak acid by strong acid because the acesulfame potassium belongs to strong base and weak acid salt; the method is based on the principle that secondary mother liquor generated by centrifugation in production is filtered and then fully reacts with a hydrolysis acid phase generated by hydrolysis reaction, and then the secondary mother liquor is subjected to extraction, water washing and neutralization, so that the recycling is realized, and the discharge of residual mother liquor is avoided.
The invention has the advantages that:
1. the invention has simple process and easy operation, and the whole process flow can realize automatic control;
2. the secondary mother liquor obtained after recrystallization and centrifugation is further filtered, so that a part of crude sugar can be obtained, the yield of the crude sugar is increased, and about 1% of finished sugar can be filtered again;
3. the secondary mother liquor obtained after recrystallization and centrifugation is filtered to remove sugar and then is fed into a hydrolysis system again, the sugar in the mother liquor is generated by maximally reacting by using a chemical reaction method, the mother liquor is maximally utilized, nearly 1 ton of finished sugar can be added every day, and the yield is improved; and a subsequent treatment working section of the mother liquor is omitted, so that a large amount of labor and equipment investment is saved, and the cost is greatly saved.
Drawings
FIG. 1 is a process flow diagram for recovering secondary mother liquor in acesulfame potassium production.
Detailed Description
The invention is further illustrated with reference to fig. 1:
a method for recycling secondary mother liquor in acesulfame potassium production comprises the following specific implementation steps:
example 1
(1) The secondary mother liquor (the sugar content of the finished product is 8%) obtained after recrystallization and centrifugation is 15m3Filtering with plate filter press, decolorizing crude sugar at decolorizing station of 14.5m3Filtrate in 2m3The volume of the solution/h is sent to a secondary mother solution head tank;
(2) opening the dripping valve of the secondary mother liquid elevated tank, dripping filtrate into the hydrolytic acid phase tank, and controlling the dripping amount to be 0.5m by a flowmeter3H, paying attention to uniform speed in the dripping process, and strictly prohibiting excessive dripping;
(3) hydrolysis productRaw hydrolyzed acid phase of 8m3The volume of the filtrate and the hydrolysis acid continuously enter a hydrolysis acid phase groove, the hydrolysis reaction is carried out on the filtrate and the hydrolysis acid in the hydrolysis acid phase groove, and the hydrolysis product is 8.5m3The amount/h is fed to the extraction section (taking care not to entrain large amounts of bubbles and flocs into the extraction system) for extraction, followed by water washing and neutralization.
Example 2
(1) The secondary mother liquor 13m obtained after recrystallization and centrifugation3Filtering with plate filter press, filtering, collecting crude sugar, removing heavy residue, decolorizing at 12.5m3Filtrate at 1.6m3The volume of the solution/h is sent to a secondary mother solution head tank;
(2) opening the dripping valve of the secondary mother liquid head tank, dripping filtrate into the hydrolytic acid phase tank, and controlling the dripping amount to be 0.75m by a flowmeter3H, paying attention to uniform speed in the dripping process, and strictly prohibiting excessive dripping;
(3) the hydrolysis produced a hydrolysis acid phase of 10 m3The volume of the filtrate and the hydrolysis acid continuously enter a hydrolysis acid phase groove, the hydrolysis reaction is carried out on the filtrate and the hydrolysis acid in the hydrolysis acid phase groove, and the hydrolysis product is 10.75m3The/h enters an extraction section (taking care not to entrain a large amount of bubbles and floccules into the extraction system) for extraction, and then washing and neutralization are carried out.
Example 3
(1) The secondary mother liquor obtained after recrystallization and centrifugation is 14m3Filtering with plate filter press, filtering, collecting crude sugar, removing heavy residue, decolorizing at 13.5 m3The filtrate was taken at 1.8m3The volume of the solution/h is sent to a secondary mother solution head tank;
(2) opening the dripping valve of the secondary mother liquid elevated tank, dripping filtrate into the hydrolytic acid phase tank, and controlling the dripping amount to be 0.8m by a flowmeter3H, paying attention to uniform speed in the dripping process, and strictly prohibiting excessive dripping;
(3) the hydrolysis produced a hydrolysis acid phase of 9 m3The volume of the filtrate and the hydrolysis acid continuously enter a hydrolysis acid phase groove, the hydrolysis reaction is carried out on the filtrate and the hydrolysis acid in the hydrolysis acid phase groove, and the hydrolysis product is 9.8m3The/h enters the extraction section (care is taken not to entrain a large amount of bubbles and flocs into the extraction system)Extraction was performed followed by water washing and neutralization.
Claims (8)
1. A method for recycling secondary mother liquor in acesulfame potassium production is characterized by adopting the following devices: the filtering device is connected with the secondary mother liquor head tank and the hydrolysis acid phase tank in sequence;
the method comprises the following steps:
(1) filtering the secondary mother liquor centrifugally thrown out by recrystallization through a plate filter press, collecting crude sugar, removing a decolouring post for boiling and decolouring, and pumping the filtrate to a secondary mother liquor high-level storage tank after collecting;
(2) in normal production, a secondary mother liquor head tank dripping valve is opened, and materials in the secondary mother liquor head tank are dripped into a hydrolysis acid phase tank; pumping the produced hydrolysis acid into a hydrolysis acid phase groove, carrying out hydrolysis reaction on the filtrate and the hydrolysis acid in the hydrolysis acid phase groove, and controlling the volume ratio of the filtrate to the hydrolysis acid not to exceed 10%;
(3) adding 5-15 m of the material in the hydrolysis acid phase tank3The amount of/h is pumped to the extraction system and then to the normal production process.
2. The method for recycling the secondary mother liquor in the production of acesulfame potassium according to claim 1, which is characterized in that: the content of finished sugar in the secondary mother liquor in the step (1) is 5-10%.
3. The method for recycling the secondary mother liquor in the production of acesulfame potassium according to claim 1, which is characterized in that: the volume ratio of the filtrate to the hydrolytic acid in the step (2) is 3-8%.
4. The method for recycling the secondary mother liquor in the production of acesulfame potassium according to claim 1, which is characterized in that: the volume ratio of the filtrate to the hydrolytic acid in the step (2) is 5-6%.
5. The method for recycling the secondary mother liquor in the production of acesulfame potassium according to claim 1, which is characterized in that: the dropping flow rate of the filtrate in the step (2) is 0.5-1.0m3/h。
6. The method for recycling the secondary mother liquor in the production of acesulfame potassium according to any one of claims 1, 2 or 5, which is characterized in that: the flow rate of the hydrolysis acid in the step (2) is 8-10 m3/h。
7. The method for recycling the secondary mother liquor in the production of acesulfame potassium according to claim 1 or 2, which is characterized in that: the dropping flow rate of the filtrate in the step (2) is 0.5-0.8m3/h。
8. The method for recycling the secondary mother liquor in the production of acesulfame potassium according to claim 1 or 2, which is characterized in that: the flow rate of the hydrolysis acid in the step (2) is 8-9 m3/h。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011367866.8A CN112480032A (en) | 2020-11-30 | 2020-11-30 | Method for recycling secondary mother liquor in acesulfame potassium production |
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| CN202011367866.8A CN112480032A (en) | 2020-11-30 | 2020-11-30 | Method for recycling secondary mother liquor in acesulfame potassium production |
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| CN112480032A true CN112480032A (en) | 2021-03-12 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114133363A (en) * | 2021-11-23 | 2022-03-04 | 安徽金禾实业股份有限公司 | Method for recycling AK sugar from AK sugar crystallization waste liquid |
| CN115677620A (en) * | 2022-11-17 | 2023-02-03 | 安徽金禾实业股份有限公司 | Method for treating coarse mother liquor in acesulfame potassium production |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20090318685A1 (en) * | 2006-08-03 | 2009-12-24 | Akira Saito | Method for producing 3,4-dihydro-1,2,3-oxathiazin-4-one-2,2-dioxide compound or salt thereof |
| US20180297968A1 (en) * | 2016-09-21 | 2018-10-18 | Celanese International Corporation | Acesulfame Potassium Compositions and Processes for Producing Same |
| CN109705058A (en) * | 2018-12-10 | 2019-05-03 | 安徽金禾实业股份有限公司 | A kind of acesulfame potassium high concentrated acid continuous hydrolysis method and device |
| CN111228854A (en) * | 2020-03-20 | 2020-06-05 | 安徽维多食品配料有限公司 | Method for extracting acesulfame potassium mother liquor |
-
2020
- 2020-11-30 CN CN202011367866.8A patent/CN112480032A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20090318685A1 (en) * | 2006-08-03 | 2009-12-24 | Akira Saito | Method for producing 3,4-dihydro-1,2,3-oxathiazin-4-one-2,2-dioxide compound or salt thereof |
| US20180297968A1 (en) * | 2016-09-21 | 2018-10-18 | Celanese International Corporation | Acesulfame Potassium Compositions and Processes for Producing Same |
| CN109705058A (en) * | 2018-12-10 | 2019-05-03 | 安徽金禾实业股份有限公司 | A kind of acesulfame potassium high concentrated acid continuous hydrolysis method and device |
| CN111228854A (en) * | 2020-03-20 | 2020-06-05 | 安徽维多食品配料有限公司 | Method for extracting acesulfame potassium mother liquor |
Non-Patent Citations (1)
| Title |
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| 李家林等: "AK糖的合成工艺及研究现状", 《广东化工》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114133363A (en) * | 2021-11-23 | 2022-03-04 | 安徽金禾实业股份有限公司 | Method for recycling AK sugar from AK sugar crystallization waste liquid |
| CN115677620A (en) * | 2022-11-17 | 2023-02-03 | 安徽金禾实业股份有限公司 | Method for treating coarse mother liquor in acesulfame potassium production |
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Application publication date: 20210312 |