CN105085160A - Method for recycling dichloromethane in acesulfame potassium synthesis process - Google Patents
Method for recycling dichloromethane in acesulfame potassium synthesis process Download PDFInfo
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- CN105085160A CN105085160A CN201510517560.9A CN201510517560A CN105085160A CN 105085160 A CN105085160 A CN 105085160A CN 201510517560 A CN201510517560 A CN 201510517560A CN 105085160 A CN105085160 A CN 105085160A
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- methylene dichloride
- dichloromethane
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Abstract
The invention discloses a method for recycling dichloromethane in an acesulfame potassium synthesis process. The method comprises the steps of a, adding roughly distilled dichloromethane into a dehydrating tower, heating, condensing to enable steam of a mixed solution of dichloromethane and water to enter a dehydration overflow tank and dichloromethane containing qualified water at the bottom to enter a semi-finished product tank so as to be used by a rectifying tower; b, enabling dichloromethane containing unqualified water at the bottom of the overflow tank to enter the dehydrating tower again through backflow and dichloromethane with high water content at the top to enter a crude product tank, and regularly discharging layered water in the crude product tank; c, enabling dichloromethane containing qualified water in the semi-finished product tank to enter the rectifying tower, distilling to 45 DEG C, enabling dichloromethane steam to enter the dehydration overflow tank, and sucking dichloromethane with high impurity content at the bottom into a residual solution tank; and d, after detecting dichloromethane in the dehydration overflow tank to be qualified, placing dichloromethane into a finished product tank so as to be used for synthesizing and sulfonating, and enabling the unqualified dichloromethane to enter the rectifying tower so as to be rectified again.
Description
Technical field
The present invention relates to the recovery method of methylene dichloride in a kind of acesulfame potassium synthesis technique.
Background technology
In traditional acesulfame potassium synthesis technique, methylene dichloride reclaims route as shown in Figure 1, will first by methylene dichloride by through slightly heating up in a steamer, then proceed in removal of impurities still add sulphur trioxide removal of impurities, proceed to again in and still, logical ammonia neutralization, neutralize rear steam heating, obtain finished product methylene dichloride; Recovery stage complex process, the technological reaction time is long, and production capacity is low, and production cost is high, does not meet the industry policy of country.
Acesulfame potassium methylene dichloride double-tower type reclaims the proposition of new production process, completely solves the problems referred to above.Single covering device production time is shortened in operate continuously, and strengthen production capacity, save a small amount of ammonia, sulphur trioxide, a large amount of steam, reduces costs, and improves the quality of products simultaneously, can reach the target level of product quality of chemical industry completely.
Summary of the invention
Object of the present invention is exactly to overcome the shortcoming existed in existing technology, and provide the recovery method of methylene dichloride in a kind of acesulfame potassium synthesis technique, the method can reduce costs, and improves production capacity and quality product.
To achieve these goals, present invention employs following technical scheme: the recovery method of methylene dichloride in acesulfame potassium synthesis technique, is characterized in that, comprises following operation steps:
A, by slightly steam after methylene dichloride add in dehydration tower, add and be steam heated to 42 DEG C, methylene dichloride and water mixed liquid steam enter dehydration overflow groove by condensation, and bottom water divides qualified methylene dichloride to enter work in-process groove, for rectifying tower; B, the underproof methylene dichloride of isopipe root moisture enter dehydration tower again by backflow, and the methylene dichloride that top moisture is high enters crude product groove, are regularly discharged by layering water in crude product groove; The methylene dichloride that in c, work in-process groove, moisture is qualified enters rectifying tower, steams to 45 DEG C, and methylene dichloride steam enters in rectifying overflow groove, by impure for bottom many methylene dichloride suction raffinate grooves; In d, rectifying overflow groove methylene dichloride qualified after testing after, put into pan tank, for synthesis sulfonation, underproofly enter rectifying tower rectifying again.
Beneficial effect of the present invention:
1, double-tower type recovery method of the present invention realizes the continuity of production operation, reduces labor strength.
2, more original traditional methylene dichloride recovery process, double-tower type recovery method stability of the present invention is high, stock product Quality advance.
3, this technique has 1. concise in technology, less investment, and production efficiency increases substantially.2. the every 1000L methylene dichloride of former technique needs to drip sulphur trioxide 25 kilograms, and need current every day to reclaim 180000L methylene dichloride, novel process saves sulphur trioxide 4.5 tons every day, can save sulphur trioxide 1650 tons every year.3. this Process is adopted to remove N-process, annual saving 240 tons of ammonias.4. reduce removal of impurities still and in and still, original rectifying needs to heat up for four times, and three coolings, change three intensification into, twice cooling, save 20 tons of steam every day, every year saving 7000 tons of steam, for enterprise saves a large amount of production cost.
Accompanying drawing explanation
Fig. 1 is methylene dichloride recovery method schema in existing acesulfame potassium building-up process;
Fig. 2 is methylene dichloride double-tower type recovery process figure in acesulfame potassium building-up process of the present invention.
Embodiment
1) as shown in Figure 2, the recovery method of methylene dichloride in acesulfame potassium synthesis technique, comprise following operation steps: a, by slightly steam after methylene dichloride add in dehydration tower, add and be steam heated to 42 DEG C, methylene dichloride and water mixed liquid steam enter dehydration overflow groove by condensation, bottom water divides qualified methylene dichloride to enter work in-process groove, for rectifying tower; B, the underproof methylene dichloride of isopipe root moisture enter dehydration tower again by backflow, and the methylene dichloride that top moisture is high enters crude product groove, are regularly discharged by layering water in crude product groove; The methylene dichloride that in c, work in-process groove, moisture is qualified enters rectifying tower, steams to 45 DEG C, and methylene dichloride steam enters in rectifying overflow groove, by impure for bottom many methylene dichloride suction raffinate grooves; In d, rectifying overflow groove methylene dichloride qualified after testing after, put into pan tank, for synthesis sulfonation, underproofly enter rectifying tower rectifying again.
The above is only preferred embodiment of the present invention, not does any pro forma restriction to the present invention; Any those of ordinary skill in the art, do not departing under technical solution of the present invention ambit, the Method and Technology content of above-mentioned announcement all can be utilized to make many possible variations and modification to technical solution of the present invention, or be revised as the Equivalent embodiments of equivalent variations.Therefore, every content not departing from technical solution of the present invention, according to technical spirit of the present invention to any simple modification made for any of the above embodiments, equivalent replacement, equivalence change and modification, all still belongs in the scope of technical solution of the present invention protection.
Claims (1)
1. the recovery method of methylene dichloride in acesulfame potassium synthesis technique, it is characterized in that, comprise following operation steps: a, by slightly steam after methylene dichloride add in dehydration tower, add and be steam heated to 42 DEG C, methylene dichloride and water mixed liquid steam enter dehydration overflow groove by condensation, bottom water divides qualified methylene dichloride to enter work in-process groove, for rectifying tower; B, the underproof methylene dichloride of isopipe root moisture enter dehydration tower again by backflow, and the methylene dichloride that top moisture is high enters crude product groove, are regularly discharged by layering water in crude product groove; The methylene dichloride that in c, work in-process groove, moisture is qualified enters rectifying tower, steams to 45 DEG C, and methylene dichloride steam enters in rectifying overflow groove, by impure for bottom many methylene dichloride suction raffinate grooves; In d, rectifying overflow groove methylene dichloride qualified after testing after, put into pan tank, for synthesis sulfonation, underproofly enter rectifying tower rectifying again.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510517560.9A CN105085160A (en) | 2015-08-22 | 2015-08-22 | Method for recycling dichloromethane in acesulfame potassium synthesis process |
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| CN201510517560.9A CN105085160A (en) | 2015-08-22 | 2015-08-22 | Method for recycling dichloromethane in acesulfame potassium synthesis process |
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106349009A (en) * | 2016-08-30 | 2017-01-25 | 安徽金禾实业股份有限公司 | Distillation-condensation method of dichloromethane in acesulfame-k compound |
| CN106365952A (en) * | 2016-08-30 | 2017-02-01 | 安徽金禾实业股份有限公司 | Method for solvent self-heating separation in acesulfame potassium synthesis |
| US10023546B2 (en) | 2016-09-21 | 2018-07-17 | Celanese International Corporation | Acesulfame potassium compositions and processes for producing same |
| US10029998B2 (en) | 2016-09-21 | 2018-07-24 | Celanese International Corporation | Acesulfame potassium compositions and processes for producing same |
| US10030000B2 (en) | 2016-09-21 | 2018-07-24 | Celanese International Corporation | Acesulfame potassium compositions and processes for producing same |
| US10029999B2 (en) | 2016-09-21 | 2018-07-24 | Celanese International Corporation | Acesulfame potassium compositions and processes for producing same |
| CN109776257A (en) * | 2019-03-26 | 2019-05-21 | 山东亚邦化工科技有限公司 | The method and apparatus of methylene chloride dehydration rectifying in acesulfame-K production |
| CN109912383A (en) * | 2019-04-15 | 2019-06-21 | 新中天环保股份有限公司 | A kind of purification system recycling methylene chloride from pharmaceuticals industry waste liquid |
| CN109928861A (en) * | 2019-04-15 | 2019-06-25 | 新中天环保股份有限公司 | A kind of method of purification recycling methylene chloride from solvent slop |
| CN111995492A (en) * | 2020-09-26 | 2020-11-27 | 安徽金禾实业股份有限公司 | Method for recovering solvent dichloromethane in acesulfame potassium production |
| CN112142555A (en) * | 2019-06-27 | 2020-12-29 | 南通醋酸化工股份有限公司 | Method for recovering dichloromethane in acesulfame potassium synthesis |
| CN113620456A (en) * | 2021-06-30 | 2021-11-09 | 南通醋酸化工股份有限公司 | Solvent recovery and waste acid treatment system and method suitable for producing acesulfame potassium |
| CN113636911A (en) * | 2021-07-13 | 2021-11-12 | 南通醋酸化工股份有限公司 | Method and device for recovering dichloromethane serving as solvent for producing acesulfame |
| CN114163297A (en) * | 2021-11-26 | 2022-03-11 | 安徽金禾实业股份有限公司 | Method for recovering solvent dichloromethane in acesulfame potassium production |
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2015
- 2015-08-22 CN CN201510517560.9A patent/CN105085160A/en active Pending
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| CN106349009B (en) * | 2016-08-30 | 2018-11-06 | 安徽金禾实业股份有限公司 | Dichloromethane rectifying condensation method in a kind of synthesis of acesulfame potassium |
| CN106365952A (en) * | 2016-08-30 | 2017-02-01 | 安徽金禾实业股份有限公司 | Method for solvent self-heating separation in acesulfame potassium synthesis |
| CN106349009A (en) * | 2016-08-30 | 2017-01-25 | 安徽金禾实业股份有限公司 | Distillation-condensation method of dichloromethane in acesulfame-k compound |
| US10759771B2 (en) | 2016-09-21 | 2020-09-01 | Celanese International Corporation | Acesulfame potassium compositions and processes for producing same |
| US10590098B2 (en) | 2016-09-21 | 2020-03-17 | Celanese International Corporation | Acesulfame potassium compositions and processes for producing same |
| US10029999B2 (en) | 2016-09-21 | 2018-07-24 | Celanese International Corporation | Acesulfame potassium compositions and processes for producing same |
| US10781191B2 (en) | 2016-09-21 | 2020-09-22 | Celanese International Corporation | Acesulfame potassium compositions and processes for producing same |
| US10208004B2 (en) | 2016-09-21 | 2019-02-19 | Celanese International Corporation | Acesulfame potassium compositions and processes for producing same |
| US10781190B2 (en) | 2016-09-21 | 2020-09-22 | Celanese International Corporation | Acesulfame potassium compositions and processes for producing same |
| US10233164B2 (en) | 2016-09-21 | 2019-03-19 | Celanese International Corporation | Acesulfame potassium compositions and processes for producing same |
| US10233163B2 (en) | 2016-09-21 | 2019-03-19 | Celanese International Corporation | Acesulfame potassium compositions and processes for producing same |
| US10975047B2 (en) | 2016-09-21 | 2021-04-13 | Celanese International Corporation | Acesulfame potassium compositions and processes for producing same |
| US10030000B2 (en) | 2016-09-21 | 2018-07-24 | Celanese International Corporation | Acesulfame potassium compositions and processes for producing same |
| US11731948B2 (en) | 2016-09-21 | 2023-08-22 | Celanese International Corporation | Acesulfame potassium compositions and processes for producing same |
| US10590095B2 (en) | 2016-09-21 | 2020-03-17 | Celanese International Corporation | Acesulfame potassium compositions and processes for producing same |
| US10590097B2 (en) | 2016-09-21 | 2020-03-17 | Celanese International Corporation | Acesulfame potassium compositions and processes for producing same |
| US11718594B2 (en) | 2016-09-21 | 2023-08-08 | Celanese International Corporation | Acesulfame potassium compositions and processes for producing same |
| US10590096B2 (en) | 2016-09-21 | 2020-03-17 | Celenese International Corporation | Acesulfame potassium compositions and processes for producing same |
| US10023546B2 (en) | 2016-09-21 | 2018-07-17 | Celanese International Corporation | Acesulfame potassium compositions and processes for producing same |
| US11724994B2 (en) | 2016-09-21 | 2023-08-15 | Celanese International Corporation | Acesulfame potassium compositions and processes for producing same |
| US10029998B2 (en) | 2016-09-21 | 2018-07-24 | Celanese International Corporation | Acesulfame potassium compositions and processes for producing same |
| US10227316B2 (en) | 2016-09-21 | 2019-03-12 | Celanese International Corporation | Acesulfame potassium compositions and processes for producing same |
| US10759770B2 (en) | 2016-09-21 | 2020-09-01 | Celanese International Corporation | Acesulfame potassium compositions and processes for producing same |
| US11724993B2 (en) | 2016-09-21 | 2023-08-15 | Celanese International Corporation | Acesulfame potassium compositions and processes for producing same |
| US10954203B2 (en) | 2016-09-21 | 2021-03-23 | Celanese International Corporation | Acesulfame potassium compositions and processes for producing same |
| US10954204B2 (en) | 2016-09-21 | 2021-03-23 | Celanese International Corporation | Acesulfame potassium compositions and processes for producing same |
| US10961207B2 (en) | 2016-09-21 | 2021-03-30 | Celanese International Corporation | Acesulfame potassium compositions and processes for producing same |
| CN109776257A (en) * | 2019-03-26 | 2019-05-21 | 山东亚邦化工科技有限公司 | The method and apparatus of methylene chloride dehydration rectifying in acesulfame-K production |
| CN109912383A (en) * | 2019-04-15 | 2019-06-21 | 新中天环保股份有限公司 | A kind of purification system recycling methylene chloride from pharmaceuticals industry waste liquid |
| CN109928861B (en) * | 2019-04-15 | 2022-03-08 | 新中天环保股份有限公司 | Purification method for recovering dichloromethane from waste solvent |
| CN109912383B (en) * | 2019-04-15 | 2021-09-14 | 新中天环保股份有限公司 | Purification system for recovering dichloromethane from pharmaceutical industry waste liquid |
| CN109928861A (en) * | 2019-04-15 | 2019-06-25 | 新中天环保股份有限公司 | A kind of method of purification recycling methylene chloride from solvent slop |
| CN112142555B (en) * | 2019-06-27 | 2023-04-18 | 南通醋酸化工股份有限公司 | Method for recovering dichloromethane in acesulfame potassium synthesis |
| CN112142555A (en) * | 2019-06-27 | 2020-12-29 | 南通醋酸化工股份有限公司 | Method for recovering dichloromethane in acesulfame potassium synthesis |
| CN111995492A (en) * | 2020-09-26 | 2020-11-27 | 安徽金禾实业股份有限公司 | Method for recovering solvent dichloromethane in acesulfame potassium production |
| CN113620456A (en) * | 2021-06-30 | 2021-11-09 | 南通醋酸化工股份有限公司 | Solvent recovery and waste acid treatment system and method suitable for producing acesulfame potassium |
| CN113636911A (en) * | 2021-07-13 | 2021-11-12 | 南通醋酸化工股份有限公司 | Method and device for recovering dichloromethane serving as solvent for producing acesulfame |
| CN114163297A (en) * | 2021-11-26 | 2022-03-11 | 安徽金禾实业股份有限公司 | Method for recovering solvent dichloromethane in acesulfame potassium production |
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Application publication date: 20151125 |