CN100410246C - Hydrolysis process of synthesizing potassium acetylsulfamilate and special device for the same - Google Patents
Hydrolysis process of synthesizing potassium acetylsulfamilate and special device for the same Download PDFInfo
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- CN100410246C CN100410246C CNB2006100961786A CN200610096178A CN100410246C CN 100410246 C CN100410246 C CN 100410246C CN B2006100961786 A CNB2006100961786 A CN B2006100961786A CN 200610096178 A CN200610096178 A CN 200610096178A CN 100410246 C CN100410246 C CN 100410246C
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- pump
- reaction pot
- condenser
- hydrolytic reaction
- outlet
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- 238000006460 hydrolysis reaction Methods 0.000 title claims abstract description 23
- 238000000034 method Methods 0.000 title claims abstract description 22
- 230000007062 hydrolysis Effects 0.000 title claims abstract description 19
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 title 1
- 229910052700 potassium Inorganic materials 0.000 title 1
- 239000011591 potassium Substances 0.000 title 1
- 230000002194 synthesizing effect Effects 0.000 title 1
- 238000006243 chemical reaction Methods 0.000 claims abstract description 49
- 239000000463 material Substances 0.000 claims abstract description 33
- 230000003301 hydrolyzing effect Effects 0.000 claims abstract description 30
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 9
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 9
- 230000008676 import Effects 0.000 claims description 10
- 238000006798 ring closing metathesis reaction Methods 0.000 claims description 9
- GLVUDVXMQACDGG-UHFFFAOYSA-N [K].C(C)(=O)C1=C(S(=O)(=O)O)C=CC(=C1)N Chemical compound [K].C(C)(=O)C1=C(S(=O)(=O)O)C=CC(=C1)N GLVUDVXMQACDGG-UHFFFAOYSA-N 0.000 claims description 7
- 238000002347 injection Methods 0.000 claims description 6
- 239000007924 injection Substances 0.000 claims description 6
- 238000006277 sulfonation reaction Methods 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 9
- 238000003756 stirring Methods 0.000 abstract description 3
- 238000001816 cooling Methods 0.000 abstract description 2
- FNXIDRUUVHQLHR-UHFFFAOYSA-N C(C)(=O)OS(=O)(C1=CC=C(C=C1)N)=O.[K] Chemical compound C(C)(=O)OS(=O)(C1=CC=C(C=C1)N)=O.[K] FNXIDRUUVHQLHR-UHFFFAOYSA-N 0.000 abstract 1
- 238000005516 engineering process Methods 0.000 description 7
- AKEJUJNQAAGONA-UHFFFAOYSA-N sulfur trioxide Chemical compound O=S(=O)=O AKEJUJNQAAGONA-UHFFFAOYSA-N 0.000 description 4
- WBZFUFAFFUEMEI-UHFFFAOYSA-M Acesulfame k Chemical compound [K+].CC1=CC(=O)[N-]S(=O)(=O)O1 WBZFUFAFFUEMEI-UHFFFAOYSA-M 0.000 description 3
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 description 3
- 229960004998 acesulfame potassium Drugs 0.000 description 3
- 235000010358 acesulfame potassium Nutrition 0.000 description 3
- 239000000619 acesulfame-K Substances 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000000376 reactant Substances 0.000 description 2
- 238000007363 ring formation reaction Methods 0.000 description 2
- XCVWCSLKKQOBGY-UHFFFAOYSA-N 2-acetyl-4-aminobenzenesulfonic acid Chemical compound CC(=O)C1=CC(N)=CC=C1S(O)(=O)=O XCVWCSLKKQOBGY-UHFFFAOYSA-N 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 1
- 229960005164 acesulfame Drugs 0.000 description 1
- YGCFIWIQZPHFLU-UHFFFAOYSA-N acesulfame Chemical compound CC1=CC(=O)NS(=O)(=O)O1 YGCFIWIQZPHFLU-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 235000013361 beverage Nutrition 0.000 description 1
- 239000012267 brine Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- WASQWSOJHCZDFK-UHFFFAOYSA-N diketene Chemical compound C=C1CC(=O)O1 WASQWSOJHCZDFK-UHFFFAOYSA-N 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 230000002503 metabolic effect Effects 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000001117 sulphuric acid Substances 0.000 description 1
- 235000011149 sulphuric acid Nutrition 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention discloses hydrolysis process and apparatus capable of continuously operating without need of stirring for the potassium acetyl sulfanilate synthesis. The technological scheme includes jetting the sulfonated and cyclized material with a jet pump to the hydrolyzing reaction kettle for hydrolysis, feeding partial material and water from the reaction kettle to the condensator outside the reaction kettle for cooling with a circulating pump, and feeding the cooled material to the other inlet of the jet pump for being jetted together with the sulfonated and cyclized material to the hydrolyzing reaction kettle. The apparatus consists of a hydrolyzing reaction kettle, a jet pump, a circulating pump and a condensator connected together. The present invention has greatly raised production efficiency.
Description
Technical field
The present invention relates to technology and this kind technology specialized apparatus of hydrolysis in the synthesis of acetyl sulfanilic acid potassium process.
Background technology
Acesulfame potassium is a kind of sweeting agent that is widely used in food, beverage industry.This compound has good water solubility, sugariness height, advantages such as physico-chemical property is stable, synergism is strong, non-metabolic.
The method of synthesis of acetyl sulfanilic acid potassium is a lot.Involved in the present invention to the synthetic method of acesulfame potassium to be based on the patent No. be US4; 695; 629 United States Patent (USP); its main method step is as follows: with thionamic acid is that a kind of raw material reacts with ketene dimer under the catalysis of triethylamine; use SO 3 sulfonated cyclization then; make acesulfame through hydrolysis again, make acesulfame potassium with the potassium hydroxide reaction again.Making a general survey of with the sulphur trioxide is other relevant patent of sulphonating agent synthesis of acetyl sulfanilic acid potassium---as: the patent No. is US4,695,629 and US5,011,982 and US5,103,046, also do not find the special reaction equipment that SO 3 sulfonated cyclization is relevant with hydrolysis, the reaction that is hydrolyzed the time all is that material dropping that sulphonation ring closure has been reacted is in reactor usually, simultaneously water also is added drop-wise to the reaction that is hydrolyzed in the reactor, on reactor, generally also be provided with whipping appts to promote reaction process, in addition, in reaction, also must in the chuck of reactor, feed refrigerated brine, sulphur trioxide and water react rapid liberated heat, control reaction temperature during with the cooling hydrolysis; But the dilute sulphuric acid that forms when reaction has very strong corrodibility and oxidisability, can produce corrosion to whipping appts and sealing member, and leakage accident takes place.In addition, this reactive mode can not realize serialization production, and can only be discontinuity production, and efficient is lower.
Summary of the invention
Technical problem to be solved by this invention is: hydrolysis process and this kind technology specialized apparatus in a kind of synthesis of acetyl sulfanilic acid potassium process of can serialization production and not needing to stir are provided.
For solving the problems of the technologies described above, main technical principle of the present invention is: the material that sulphonation ring closure has been reacted with squirt pump continuous high speed ground sprays in the hydrolytic reaction pot, and in reactor, form eddy current with the thorough mixing reactant, pump is played circulation again, reaction mass and water are cooled off, discharging continuously again after reaction is finished by condenser.Do not need whipping appts, solved and leaked and interruption production problem.
The concrete technical scheme that the present invention adopts is: the hydrolysis process in a kind of synthesis of acetyl sulfanilic acid potassium process, be characterized in: the material that sulphonation ring closure has been reacted is incorporated into an input terminus of squirt pump, by squirt pump the material direct injection is entered into the hydrolytic reaction pot reaction that is hydrolyzed; Simultaneously, with recycle pump the partial reaction material in the hydrolytic reaction pot is sent in the condenser with water and cools off, to be incorporated into another input terminus of squirt pump through the cooled material of condenser again, and enter into hydrolytic reaction pot by the squirt pump injection with the material that sulphonation ring closure has reacted; And the material after the hydrolysis reaction end is drawn from the bottom of hydrolytic reaction pot.
Above-mentionedly can preferably be controlled at-10 ℃～15 ℃ through the cooled material temperature of condenser.
In addition, a kind of specific equipment of hydrolysis process recited above, comprise: hydrolytic reaction pot, the sidewall of hydrolytic reaction pot is provided with opening for feed, feedback outlet, the bottom of hydrolytic reaction pot is provided with discharge port, opening for feed is connected with the injection pump outlet, feedback outlet by pipeline be connected with inlet of circulating pump again after the water source is connected, outlet of circulating pump is connected with the import of condenser, the outlet of condenser is connected with an import of squirt pump, and another import of squirt pump is connected with the material that sulfonation reaction is finished.
Above-mentioned opening for feed is separately positioned on the sidewall relative on the hydrolytic reaction pot with feedback outlet.
Advantage of the present invention is: use hydrolysis process of the present invention and specific equipment thereof in synthesis of acetyl sulfanilic acid potassium process, not only technology and equipment are simple, need not whipping appts, and can realize serialization production, have improved production efficiency greatly.
Description of drawings
Fig. 1 is the structure principle chart of the specific equipment of hydrolysis process of the present invention.
Embodiment
The invention will be further described below in conjunction with the drawings and specific embodiments.
As shown in Figure 1, the specific equipment of described hydrolysis process comprises: hydrolytic reaction pot 10, on the relative sidewall of hydrolytic reaction pot 10, be respectively arranged with opening for feed 11, feedback outlet 8, the bottom of hydrolytic reaction pot 10 is provided with discharge port 9, opening for feed 11 is connected with the outlet 5 of squirt pump 4, feedback outlet 8 by pipeline be connected with the import of recycle pump 6 again after water source 7 is connected, the outlet of recycle pump 6 is connected with the import of condenser 12, the outlet of condenser 12 is connected with an import 1 of squirt pump 4, and another import 2 of squirt pump 4 is connected with the material 3 that sulfonation reaction is finished.
Utilize above-mentioned specific equipment, the detailed step of hydrolysis process of the present invention is as follows: the material 3 that sulphonation ring closure has been reacted is incorporated into an input aperture 2 of squirt pump 4, by squirt pump 4 the direct high-velocity jet of material is entered into hydrolytic reaction pot 10 reaction that is hydrolyzed; Simultaneously, with recycle pump 6 the partial reaction material in the hydrolytic reaction pot 10 is sent in the condenser 12 with water and cools off, can preferably be controlled at-10 ℃～15 ℃ through condenser 12 cooled material temperature, to be incorporated into another input terminus 1 of squirt pump 4 through condenser 12 cooled materials again, and enter into hydrolytic reaction pot 10 by squirt pump 4 high-velocity jet with the material that sulphonation ring closure has reacted; And the material after the hydrolysis reaction end is drawn from the bottom discharge mouth 9 of hydrolytic reaction pot 10.
From the above mentioned as can be known, squirt pump 4 can form negative pressure when high-velocity jet, help material 3 that sulphonation ring closure has been reacted more and suck and be ejected in the hydrolytic reaction pot 10, make them form eddy current thereby just need not stir and to carry out sufficient hydrolysis reaction at the inwall of hydrolytic reaction pot 10 through condenser 12 cooled materials; In addition, in reaction process, partial material is incorporated in the condenser 12 of hydrolytic reaction pot 10 outsides and cools off, help controlling the temperature of reactant more; Therefore, use hydrolysis process of the present invention and specific equipment thereof, just can realize serialization production, improved production efficiency greatly.
Claims (4)
1. the hydrolysis process in the synthesis of acetyl sulfanilic acid potassium process is characterized in that: the material that sulphonation ring closure has been reacted is incorporated into an input terminus of squirt pump, by squirt pump the material direct injection is entered into the hydrolytic reaction pot reaction that is hydrolyzed; Simultaneously, with recycle pump the partial reaction material in the hydrolytic reaction pot is sent in the condenser with water and cools off, to be incorporated into another input terminus of squirt pump through the cooled material of condenser again, and enter into hydrolytic reaction pot by the squirt pump injection with the material that sulphonation ring closure has reacted; And the material after the hydrolysis reaction end is drawn from the bottom of hydrolytic reaction pot.
2. hydrolysis process as claimed in claim 1 is characterized in that: be controlled at-10 ℃～15 ℃ through the cooled material temperature of condenser.
3. the specific equipment of a hydrolysis process as claimed in claim 1 or 2, it is characterized in that: comprising: hydrolytic reaction pot, the sidewall of hydrolytic reaction pot is provided with opening for feed, feedback outlet, the bottom of hydrolytic reaction pot is provided with discharge port, opening for feed is connected with the injection pump outlet, feedback outlet by pipeline be connected with inlet of circulating pump again after the water source is connected, outlet of circulating pump is connected with the import of condenser, the outlet of condenser is connected with an import of squirt pump, and another import of squirt pump is connected with the material that sulfonation reaction is finished.
4. specific equipment as claimed in claim 3 is characterized in that: described opening for feed is separately positioned on the sidewall relative on the hydrolytic reaction pot with feedback outlet.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100961786A CN100410246C (en) | 2006-09-24 | 2006-09-24 | Hydrolysis process of synthesizing potassium acetylsulfamilate and special device for the same |
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|---|---|---|---|
| CNB2006100961786A CN100410246C (en) | 2006-09-24 | 2006-09-24 | Hydrolysis process of synthesizing potassium acetylsulfamilate and special device for the same |
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| Publication Number | Publication Date |
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| CN1927849A CN1927849A (en) | 2007-03-14 |
| CN100410246C true CN100410246C (en) | 2008-08-13 |
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| CNB2006100961786A Active CN100410246C (en) | 2006-09-24 | 2006-09-24 | Hydrolysis process of synthesizing potassium acetylsulfamilate and special device for the same |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US11718594B2 (en) | 2016-09-21 | 2023-08-08 | 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 |
| US11724994B2 (en) | 2016-09-21 | 2023-08-15 | 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 |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104292181B (en) * | 2014-09-27 | 2016-10-26 | 安徽金禾实业股份有限公司 | A kind of MVR system concentrates the method for acesulfame potassium mother solution |
| 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 |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4695629A (en) * | 1984-03-22 | 1987-09-22 | Hoechst Aktiengesellschaft | Process for the preparation of 6-methyl-3,4-dihydro-1,2,3-oxathiazin-4-one 2,2-dioxide and its non-toxic salts |
| CN1323792A (en) * | 2001-05-15 | 2001-11-28 | 张家港浩波化学品有限公司 | Synthesis of acetyl sulfanilic acid and its potassium salt |
| CN1336363A (en) * | 2001-07-25 | 2002-02-20 | 张元宾 | Synthesis of potassium acetylsulfanilate |
| CN200949088Y (en) * | 2006-09-24 | 2007-09-19 | 张家港浩波化学品有限公司 | Special device for hydrolyzing process of synthesizing potassium acetylsulfamilate |
-
2006
- 2006-09-24 CN CNB2006100961786A patent/CN100410246C/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4695629A (en) * | 1984-03-22 | 1987-09-22 | Hoechst Aktiengesellschaft | Process for the preparation of 6-methyl-3,4-dihydro-1,2,3-oxathiazin-4-one 2,2-dioxide and its non-toxic salts |
| CN1323792A (en) * | 2001-05-15 | 2001-11-28 | 张家港浩波化学品有限公司 | Synthesis of acetyl sulfanilic acid and its potassium salt |
| CN1336363A (en) * | 2001-07-25 | 2002-02-20 | 张元宾 | Synthesis of potassium acetylsulfanilate |
| CN200949088Y (en) * | 2006-09-24 | 2007-09-19 | 张家港浩波化学品有限公司 | Special device for hydrolyzing process of synthesizing potassium acetylsulfamilate |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US11718594B2 (en) | 2016-09-21 | 2023-08-08 | 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 |
| US11724994B2 (en) | 2016-09-21 | 2023-08-15 | 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 |
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| CN1927849A (en) | 2007-03-14 |
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