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CN111518057A - Acesulfame potassium crystal liquid purification treatment method - Google Patents

Acesulfame potassium crystal liquid purification treatment method Download PDF

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Publication number
CN111518057A
CN111518057A CN202010444786.1A CN202010444786A CN111518057A CN 111518057 A CN111518057 A CN 111518057A CN 202010444786 A CN202010444786 A CN 202010444786A CN 111518057 A CN111518057 A CN 111518057A
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China
Prior art keywords
acesulfame potassium
sugar
purification treatment
addition amount
liquid
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Pending
Application number
CN202010444786.1A
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Chinese (zh)
Inventor
姜维强
陈朝晖
程帮琴
沙里峰
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Anhui Jinhe Industrial Co Ltd
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Anhui Jinhe Industrial Co Ltd
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Priority to CN202010444786.1A priority Critical patent/CN111518057A/en
Publication of CN111518057A publication Critical patent/CN111518057A/en
Pending legal-status Critical Current

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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07DHETEROCYCLIC COMPOUNDS
    • C07D291/00Heterocyclic compounds containing rings having nitrogen, oxygen and sulfur atoms as the only ring hetero atoms
    • C07D291/02Heterocyclic compounds containing rings having nitrogen, oxygen and sulfur atoms as the only ring hetero atoms not condensed with other rings
    • C07D291/06Six-membered rings

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Saccharide Compounds (AREA)

Abstract

The invention relates to an acesulfame potassium crystal liquid purification treatment method, which is characterized in that the acesulfame potassium crystal liquid is pretreated by adopting a solvent repeated extraction method for many times to remove most impurities contained in the acesulfame potassium crystal liquid, and then mother liquor after acesulfame potassium purification is evaporated, concentrated, decolored by heat preservation, frozen and crystallized and filtered to obtain high-purity acesulfame potassium crystals. The method can effectively remove various impurities in the crystallization liquid, improve the crystallization purity of the acesulfame potassium, further reduce the crystallization times, improve the product quality, simplify the production operation, reduce the labor intensity of workers, improve the product purity, save the steam and reduce the energy consumption.

Description

Acesulfame potassium crystal liquid purification treatment method
The technical field is as follows:
the invention relates to a production method of a sweetening agent, in particular to a method for pre-extracting, treating and purifying a crystal liquid in an acesulfame refining process.
Background art:
the refining process in the traditional acesulfame potassium production process comprises the steps of extracting sulfonated cyclization reaction liquid by hydrolysis, extracting by liquid-liquid separation organic phases such as dichloromethane and the like and continuous organic solvents such as dichloromethane and the like, washing the combined organic phases by water, neutralizing the organic phases by KOH, and separating the organic phases to obtain a water phase which is sugar water; the sugar water is usually decolorized, heated and concentrated, frozen and crystallized, centrifuged and separated and other steps to obtain crude sugar (Jiangyu, synthesis research of sweetener acesulfame, 2008, 35,9 of technical innovation guide); the qualified acesulfame potassium product can be obtained after the crude sugar is recrystallized for at least two times, mainly because the organic impurities in the sugar water can be attached to sugar crystals to cause the content of the organic impurities in the primary sugar and the secondary sugar to exceed the standard. The current purification technology from sugar water to qualified products is intermittent production, the repeated crystallization energy consumption is high, the resource waste is serious, the manual operation is complicated, the production cost is high, the reaction equipment is complex and various, the temperature change is large, and the service life of the equipment is short. The production is intermittent, the utilization rate of the device is low, the impurity content in the finished product is easy to exceed the standard, the product quality can not meet the market requirement, and the market value of the product is seriously influenced.
The invention content is as follows:
the invention aims to overcome the defects in the prior art, and provides an improved method for refining acesulfame, namely a method for pre-extracting and purifying a neutralized crystallization liquid, which is to remove organic impurities in sugar water by using an extraction method, so that the content of the organic impurities in primary sugar is reduced, the purity of the primary sugar is improved, and the purity of the heavy sugar in the prior art is basically achieved.
In order to achieve the purpose, the invention adopts the following technical scheme:
a purification treatment method of neutralized crystal liquid after sulfonation cyclization in an acesulfame potassium production process, the production process comprises the steps of condensation, cyclization, sulfonation, hydrolysis and neutralization and decoloration, and the obtained neutralized crystal mixed liquid is separated to obtain sugar water of an alkaline water phase, and the purification treatment method is characterized by comprising the following steps:
(1) and carrying out liquid-liquid extraction on the alkaline aqueous sugar solution for 4-20 times by using an organic solvent, wherein the mass ratio of the sugar solution to the extraction liquid is controlled to be 1: 0.1-10, standing after extraction, and performing phase separation liquid-liquid separation to obtain purified sugar water;
(2) carrying out reduced pressure distillation and concentration on the purified sugar water for 1-24 h, and controlling the pressure to be 0.05-0.099 MPa;
(3) adding activated carbon and hydrogen peroxide into the concentrated sugar water for decolorization, stirring and preserving heat for 1-8 h, and filtering to remove the activated carbon to obtain decolorized concentrated sugar water;
(4) and cooling the obtained decolorized concentrated sugar water to-10-30 ℃, crystallizing for 4-72 hours, and then filtering to obtain initial sugar with the purity of 98-99%, wherein the content of organic impurities is lower than 500 ppm.
The further technical scheme is as follows: the sugar content of the alkaline aqueous sugar water is 10-30%.
The further technical scheme is as follows: and (3) concentrating the purified sugar water in the step (2) to a sugar content of 30-80%.
The further technical scheme is as follows: the organic solvent is any one of ethyl acetate, isopropyl acetate, butyl acetate and dichloromethane, and ethyl acetate is preferred.
The further technical scheme is as follows: the addition amount of the decolorizing agent active carbon is 0.1-10%; the addition amount of the decolorizing agent hydrogen peroxide is 0.1-10%.
The further technical scheme is as follows: the addition amount of the decolorizing agent active carbon is 0.1-10%; the addition amount of the decolorizing agent hydrogen peroxide is 0.1-10%.
The further technical scheme is as follows: the purified sugar water in the step (2) is concentrated to the content of 40-60% preferably.
The further technical scheme is as follows: the addition amount of the decolorizing agent active carbon is preferably 0.5-2%; the addition amount of the decolorizing agent hydrogen peroxide is preferably 0.5-2%.
The further technical scheme is as follows: the addition amount of the decolorizing agent active carbon is preferably 0.5-2%; the addition amount of the decolorizing agent hydrogen peroxide is preferably 0.5-2%.
The invention has the beneficial effects that: organic impurities in the sugar water are removed by a continuous multiple extraction method, so that the content of the organic impurities in the primary sugar is reduced, the purity of the primary sugar is improved, and the purity of the heavy crusted sugar in the prior art is basically achieved. The method can reduce the tertiary crystallization in the prior art into secondary crystallization, reduces the operation of primary crystallization, reduces equipment and process, improves the production stability, reduces energy consumption and reduces the labor intensity of workers. The impurity content in the subsequent finished product is easy to control, the product quality can meet the market requirement, and the market value of the product is improved.
Detailed Description
Example 1
200mL (100 mL of each of an aqueous phase and an organic phase, and 20% of AK sugar content in the aqueous phase) of a neutralized crystalline mixed solution obtained in the neutralization and decoloration process in the production of acesulfame are subjected to standing and layering, and a dichloromethane phase is separated to obtain about 100 mL of sugar water in an alkaline aqueous phase. The sugar solution is extracted with 100 mL of dichloromethane for 4 times (after extraction, the organic phase and the water phase sugar solution are separated, and the water phase sugar solution is extracted with dichloromethane, namely, the water phase obtained each time is extracted for 4 times in total). Distilling and concentrating the extracted and purified sugar water under reduced pressure (0.095MPa,70 ℃) for 1 h to reach the concentration of 40%, cooling to 10 ℃ after distillation, crystallizing for 12h, and then performing suction filtration to obtain 15g of initial sugar with the purity of 99% and the content of organic impurities of 180 ppm. The separated dichloromethane is distilled and recovered under normal pressure, and the recovery rate is 95 percent.
Example 2
200mL (100 mL each of the aqueous phase and the organic phase, and 20% AK sugar content in the aqueous phase) of the neutralized crystal mixture obtained in the previous step was heated and distilled to remove methylene chloride, thereby obtaining about 100 mL of sugar water in the alkaline aqueous phase. The sugar solution was extracted 4 times with 200mL of ethyl acetate. And (3) carrying out reduced pressure (0.095MPa,70 ℃) distillation concentration on the purified sugar water for 1 h to reach the concentration of 40%, cooling to 0 ℃ after the distillation is finished, crystallizing for 12h, and then carrying out suction filtration to obtain 15g of initial sugar with the purity of 99% and the content of organic impurities of 150 ppm. The separated ethyl acetate was recovered by distillation under reduced pressure, and the recovery rate was 95%.
Example 3
200mL (100 mL each of the aqueous phase and the organic phase, and 20% AK sugar content in the aqueous phase) of the neutralized crystal mixture obtained in the previous step was heated and distilled to remove methylene chloride, thereby obtaining about 100 mL of sugar water in the alkaline aqueous phase. The sugar solution was extracted 4 times with 200mL of ethyl acetate. And (3) carrying out reduced pressure (0.095MPa,70 ℃) distillation concentration on the purified sugar water for 1 h until the concentration reaches 40%, adding 0.5g of activated carbon and 0.5g of hydrogen peroxide after the distillation is finished, stirring and preserving heat for 2h, filtering the activated carbon while the solution is hot, cooling the mother solution to 0 ℃, crystallizing for 12h, and then carrying out suction filtration to obtain 14g of primary sugar with the purity of 99% and the content of organic impurities of 120 ppm. The separated ethyl acetate was recovered by distillation under reduced pressure, and the recovery rate was 95%.
Example 4
200mL (100 mL each of the aqueous phase and the organic phase, and 20% AK sugar content in the aqueous phase) of the neutralized crystal mixture obtained in the previous step was heated and distilled to remove methylene chloride, thereby obtaining about 100 mL of sugar water in the alkaline aqueous phase. The sugar solution was extracted 10 times with 200mL of ethyl acetate. And (3) carrying out reduced pressure (0.095MPa,70 ℃) distillation concentration on the purified sugar water for 1 h until the concentration reaches 40%, adding 0.5g of activated carbon and 0.5g of hydrogen peroxide after the distillation is finished, stirring and preserving heat for 2h, filtering the activated carbon while the sugar water is hot, cooling the mother liquor to 0 ℃, crystallizing for 12h, and then carrying out centrifugal filtration to obtain 15g of primary sugar with the purity of 99% and the organic impurity content of 70 ppm. The separated ethyl acetate was recovered by distillation under reduced pressure, and the recovery rate was 95%.
Example 5
200mL (100 mL each of the aqueous phase and the organic phase, and 20% AK sugar content in the aqueous phase) of the neutralized crystal mixture obtained in the previous step was heated and distilled to remove methylene chloride, thereby obtaining about 100 mL of sugar water in the alkaline aqueous phase. The sugar solution was extracted 10 times with 200mL of butyl acetate. And (3) carrying out reduced pressure (0.095MPa,70 ℃) distillation concentration on the purified sugar water for 1 h until the concentration reaches 30%, adding 0.5g of activated carbon and 0.5g of hydrogen peroxide after the distillation is finished, stirring and preserving heat for 2h, filtering the activated carbon while the solution is hot, cooling the mother solution to 10 ℃, crystallizing for 12h, and then carrying out suction filtration to obtain 12g of primary sugar with the purity of 99% and the organic impurity content of 250 ppm. The separated butyl acetate was recovered by distillation under reduced pressure, and the recovery rate was 96%.
Example 6
200mL (100 mL each of the aqueous phase and the organic phase, and 20% AK sugar content in the aqueous phase) of the neutralized crystal mixture obtained in the previous step was heated and distilled to remove methylene chloride, thereby obtaining about 100 mL of sugar water in the alkaline aqueous phase. The sugar solution was extracted 10 times with 200mL of isopropyl acetate. And (3) carrying out reduced pressure (0.08 MPa,90 ℃) distillation and concentration on the purified sugar water for 1 h until the concentration reaches 60%, adding 0.5g of active carbon and 0.5g of hydrogen peroxide after the distillation is finished, stirring, keeping the temperature for 2h, cooling to-5 ℃ for crystallization for 12h, and then carrying out centrifugal filtration to obtain 16g of primary sugar with the purity of 99% and the content of organic impurities of 200 ppm. The separated isopropyl acetate is recovered by reduced pressure distillation, and the recovery rate is 96 percent.

Claims (9)

1. A purification treatment method of acesulfame potassium crystal liquid comprises the step of separating the neutralized crystal mixed liquid obtained in the neutralized crystallization process to obtain sugar water of an alkaline water phase, and is characterized by comprising the following steps:
(1) and carrying out liquid-liquid extraction on the alkaline aqueous sugar solution for 4-20 times by using an organic solvent, wherein the mass ratio of the sugar solution to the extraction liquid is controlled to be 1: 0.1-10, standing after extraction, and performing phase separation liquid-liquid separation to obtain purified sugar water;
(2) carrying out reduced pressure distillation and concentration on the purified sugar water for 1-24 h, and controlling the pressure to be 0.05-0.099 MPa;
(3) adding activated carbon and hydrogen peroxide into the concentrated sugar water for decolorization, stirring and preserving heat for 1-8 h, and filtering to remove the activated carbon to obtain decolorized concentrated sugar water;
(4) and cooling the obtained decolorized concentrated sugar water to-10-30 ℃, crystallizing for 4-72 hours, and then filtering to obtain initial sugar with the purity of 98-99%, wherein the content of organic impurities is lower than 500 ppm.
2. The acesulfame potassium crystal liquid purification treatment method according to claim 1, wherein the method comprises the following steps: the sugar content of the alkaline aqueous sugar water is 10-30%.
3. The acesulfame potassium crystal liquid purification treatment method according to claim 2, wherein the method comprises the following steps: and (3) concentrating the purified sugar water in the step (2) to a sugar content of 30-80%.
4. The method for purifying acesulfame potassium crystal solution according to claim 1, 2 or 3, which comprises: the organic solvent is any one of ethyl acetate, isopropyl acetate, butyl acetate and dichloromethane, and ethyl acetate is preferred.
5. The method for purifying acesulfame potassium crystal solution according to claim 1, 2 or 3, which comprises: the addition amount of the decolorizing agent active carbon is 0.1-10%; the addition amount of the decolorizing agent hydrogen peroxide is 0.1-10%.
6. The acesulfame potassium crystal liquid purification treatment method according to claim 4, wherein the method comprises the following steps: the addition amount of the decolorizing agent active carbon is 0.1-10%; the addition amount of the decolorizing agent hydrogen peroxide is 0.1-10%.
7. The acesulfame potassium crystal liquid purification treatment method according to claim 3, wherein the method comprises the following steps: the purified sugar water in the step (2) is concentrated to the content of 40-60% preferably.
8. The acesulfame potassium crystal liquid purification treatment method according to claim 5, wherein the method comprises the following steps: the addition amount of the decolorizing agent active carbon is preferably 0.5-2%; the addition amount of the decolorizing agent hydrogen peroxide is preferably 0.5-2%.
9. The acesulfame potassium crystal liquid purification treatment method according to claim 6, wherein the method comprises the following steps: the addition amount of the decolorizing agent active carbon is preferably 0.5-2%; the addition amount of the decolorizing agent hydrogen peroxide is preferably 0.5-2%.
CN202010444786.1A 2020-05-23 2020-05-23 Acesulfame potassium crystal liquid purification treatment method Pending CN111518057A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112424176A (en) * 2020-09-21 2021-02-26 安徽金禾实业股份有限公司 Refining method of acesulfame potassium
CN113244854A (en) * 2021-06-10 2021-08-13 黄山友谊南海新材料有限公司 High-purity TGIC system of processing
CN118834251A (en) * 2024-07-03 2024-10-25 丽珠集团福州福兴医药有限公司 Tobramycin method for crystallizing element

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US20090318686A1 (en) * 2006-08-03 2009-12-24 Akira Saito Method for producing potassium salt of 3,4-dihydro-1,2,3-oxathiazin-4-one-2,2-dioxide compound
US20180079736A1 (en) * 2016-09-21 2018-03-22 Celanese International Corporation Acesulfame potassium compositions and processes for producing same
CN110818654A (en) * 2019-12-20 2020-02-21 安徽金禾实业股份有限公司 Optimized acesulfame crystallization method
CN110846443A (en) * 2019-11-16 2020-02-28 安徽金禾实业股份有限公司 Method for optimizing crystallization by back extraction of acesulfame-K syrup

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US20180079736A1 (en) * 2016-09-21 2018-03-22 Celanese International Corporation Acesulfame potassium compositions and processes for producing same
CN110846443A (en) * 2019-11-16 2020-02-28 安徽金禾实业股份有限公司 Method for optimizing crystallization by back extraction of acesulfame-K syrup
CN110818654A (en) * 2019-12-20 2020-02-21 安徽金禾实业股份有限公司 Optimized acesulfame crystallization method

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112424176A (en) * 2020-09-21 2021-02-26 安徽金禾实业股份有限公司 Refining method of acesulfame potassium
WO2022056914A1 (en) * 2020-09-21 2022-03-24 安徽金禾实业股份有限公司 Refining method for acesulfame
CN113244854A (en) * 2021-06-10 2021-08-13 黄山友谊南海新材料有限公司 High-purity TGIC system of processing
CN118834251A (en) * 2024-07-03 2024-10-25 丽珠集团福州福兴医药有限公司 Tobramycin method for crystallizing element

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Application publication date: 20200811