CN112110963A - Method for continuous high-temperature chlorination of sucralose - Google Patents
Method for continuous high-temperature chlorination of sucralose Download PDFInfo
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- CN112110963A CN112110963A CN202011027939.9A CN202011027939A CN112110963A CN 112110963 A CN112110963 A CN 112110963A CN 202011027939 A CN202011027939 A CN 202011027939A CN 112110963 A CN112110963 A CN 112110963A
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- chlorination
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H5/00—Compounds containing saccharide radicals in which the hetero bonds to oxygen have been replaced by the same number of hetero bonds to halogen, nitrogen, sulfur, selenium, or tellurium
- C07H5/02—Compounds containing saccharide radicals in which the hetero bonds to oxygen have been replaced by the same number of hetero bonds to halogen, nitrogen, sulfur, selenium, or tellurium to halogen
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H1/00—Processes for the preparation of sugar derivatives
Abstract
The invention relates to a method for continuous high-temperature chlorination of sucralose, which is characterized by comprising the following steps: the primary reactor is sequentially connected with a primary chlorination transfer kettle, a secondary reactor, a secondary chlorination transfer kettle and a high-temperature chlorination liquid transfer tank, and the primary chlorination transfer kettle and the secondary chlorination transfer kettle are respectively connected with a tail gas recovery device; (1) feeding the esterification product into a primary reactor, controlling the temperature to be 55-60 ℃ and the pressure to be-45 to-55 KPa, and feeding the material into a primary chlorination transfer kettle after 3-5 hours, wherein the temperature in the kettle is 55-65 ℃ and the pressure to be-45 to-55 KPa; (2) when the liquid in the kettle reaches 1/2-2/3, sending the liquid into a secondary reactor, controlling the temperature to be 110-115 ℃ and the pressure to be-45 to-55 KPa, and after 3-5 hours, feeding the materials into a secondary chlorination transfer kettle, wherein the temperature in the kettle is 55-65 ℃ and the pressure to be-45 to-55 KPa; (3) when the liquid in the kettle reaches 1/2-2/3, the mixture is sent into a high-temperature chlorination liquid transfer tank. The invention has the advantages that: the single batch operation becomes a process capable of continuous reaction; half of kettle reactors are reduced, and the equipment cost is reduced; reduces human operation errors, improves the production stability and indirectly improves the reaction yield.
Description
Technical Field
The invention belongs to the technical field of chemical production, and relates to a method for continuous high-temperature chlorination of sucralose.
Background
Sucralose (TGS), a novel sweetener developed by the british tare company (Tate & ly) and filed in 1976 with the university of london. The sugar-free functional sweetener is a functional sweetener only taking sucrose as a raw material, the original trade name is Splenda, and the sweetness can reach 600 times that of the sucrose. The sweetener has the characteristics of no energy, high sweetness, pure sweetness, high safety and the like, and is one of the most excellent functional sweeteners at present.
The industrial production of sucralose adopts a monoester method, DMF is used as a solvent, acetic anhydride is used as an acylating agent to obtain sucrose-6-ethyl ester, thionyl chloride is usually used as a chlorinating agent to carry out chlorination reaction, the chlorination operation is mostly carried out in a tank reactor, and the problems of low product yield (65-75%), long reaction time (12-16 h), high reaction temperature and high requirement on equipment exist.
Disclosure of Invention
The invention aims to solve the problems and provide a method for continuously chlorinating sucralose at high temperature.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a method for continuous high-temperature chlorination of sucralose is characterized by adopting the following devices: the primary reactor is sequentially connected with a primary chlorination transfer kettle, a secondary reactor, a secondary chlorination transfer kettle and a high-temperature chlorination liquid transfer tank, and the primary chlorination transfer kettle and the secondary chlorination transfer kettle are connected with a tail gas recovery device through pipelines;
the method comprises the following steps:
(1) sending an esterification product (with the content of sucrose-6-ethyl ester being 300-;
(2) when the liquid in the first-stage chlorination transfer kettle reaches the kettle volume of 1/2-2/3, sending the materials in the kettle into a second-stage reactor in an amount of 1.5-3 m/h, controlling the temperature of the second-stage reactor to be 110-115 ℃, the pressure to be-45 to-55 KPa, and the reaction time to be 3-5h, sending the materials from the second-stage reactor into a second-stage chlorination transfer kettle in an amount of 1.5-3 m/h, and controlling the temperature of the first-stage chlorination transfer kettle to be 55-65 ℃ and the pressure to be-45 to-55 KPa;
(3) gas generated by the first-stage chlorination transfer kettle and the second-stage chlorination transfer kettle enters the tail gas recovery device, and when liquid in the second-stage chlorination transfer kettle reaches the kettle volume of 1/2-2/3, materials in the second-stage chlorination transfer kettle are sent into the high-temperature chlorination liquid transfer groove in an amount of 1-1.5 m for cultivation per hour.
The invention has the following advantages:
1. the invention changes the original single batch operation into an operation process capable of realizing continuous reaction by adopting a secondary reactor and a secondary transfer kettle; compared with the original kettle type reaction process, the invention adopts the device with the same specification, which can reduce half of the kettle type reactor and greatly reduce the investment cost of the equipment;
2. by adopting the device, continuous and automatic operation can be realized, excessive personnel are prevented from participating in the production of the device, the labor is saved, and the labor cost is reduced;
3. the continuous and automatic operation process can reduce manual operation errors, improve the production stability, indirectly improve the reaction yield and improve the production safety.
Drawings
FIG. 1 is a schematic diagram of a continuous high temperature chlorination process for sucralose.
Detailed Description
The invention is further illustrated with reference to fig. 1:
the utility model provides a device of continuous high temperature chlorination of sucralose, is including the one-level cauldron formula reactor, one-level chlorination transfer kettle, second grade cauldron formula reactor, second grade chlorination transfer kettle, the high temperature chlorination liquid transfer groove that connect gradually, and the top of one-level chlorination transfer kettle, second grade chlorination transfer kettle links to each other through pipeline and tail gas recovery unit respectively.
Example 1
(1) Opening emptying valves of the primary chlorination transfer kettle and the secondary chlorination transfer kettle, starting a water ring vacuum pump, and operating a tail gas recovery device;
(2) respectively opening heat conducting oil of a primary reactor and a secondary reactor, and controlling the outlet temperatures of the primary reactor and the secondary reactor to be 60 ℃ and 112 ℃ respectively;
(3) 1000 ml of low-temperature chlorination liquid (the content of sucrose-6-ethyl ester is 300-;
(4) when the volume of the reaction liquid in the first-stage chlorination transfer kettle reaches 300ml, sending the reaction liquid into a second-stage reactor and a second-stage chlorination transfer kettle at the flow rate of 5ml/min, adjusting the temperature of the second-stage reactor and the temperature of the second-stage chlorination transfer kettle to be 112 ℃, and adjusting the pressure to be-50 KPa;
(5) when the volume of the reaction liquid in the secondary chlorination transfer kettle reaches 300ml, the reaction liquid is extracted at the flow rate of 5ml/min and sent into a high-temperature chlorination transfer tank, and then neutralization reaction is carried out.
Example 2
(1) Opening emptying valves of the primary chlorination transfer kettle and the secondary chlorination transfer kettle, starting a water ring vacuum pump, and operating a tail gas recovery device;
(2) respectively opening heat conducting oil of a primary reactor and a secondary reactor, and controlling the outlet temperatures of the primary reactor and the secondary reactor to be 55 ℃ and 115 ℃ respectively;
(3) 1200 ml of low-temperature chlorination liquid (the content of sucrose-6-ethyl ester is 310-;
(4) when the volume of the reaction liquid in the first-stage chlorination transfer kettle reaches 400ml, feeding the reaction liquid into a second-stage reactor and a second-stage chlorination transfer kettle at the flow rate of 5.5ml/min, adjusting the temperature of the second-stage reactor and the temperature of the second-stage chlorination transfer kettle to be 115 ℃, and adjusting the pressure to be-52 KPa;
(5) when the volume of the reaction liquid in the secondary chlorination transfer kettle reaches 400ml, the reaction liquid is extracted at the flow rate of 5.5ml/min and sent into a high-temperature chlorination transfer tank, and then neutralization reaction is carried out.
Claims (2)
1. A method for continuous high-temperature chlorination of sucralose is characterized by adopting the following devices: the primary reactor is sequentially connected with a primary chlorination transfer kettle, a secondary reactor, a secondary chlorination transfer kettle and a high-temperature chlorination liquid transfer tank, and the primary chlorination transfer kettle and the secondary chlorination transfer kettle are connected with a tail gas recovery device through pipelines;
the method comprises the following steps:
(1) sending an esterification product (with the content of sucrose-6-ethyl ester being 300-;
(2) when the liquid in the first-stage chlorination transfer kettle reaches the kettle volume of 1/2-2/3, sending the materials in the kettle into a second-stage reactor in an amount of 1.5-3 m/h, controlling the temperature of the second-stage reactor to be 110-115 ℃, the pressure to be-45 to-55 KPa, and the reaction time to be 3-5h, sending the materials from the second-stage reactor into a second-stage chlorination transfer kettle in an amount of 1.5-3 m/h, and controlling the temperature of the second-stage chlorination transfer kettle to be 55-65 ℃ and the pressure to be-45 to-55 KPa;
(3) gas generated by the first-stage chlorination transfer kettle and the second-stage chlorination transfer kettle enters the tail gas recovery device, and when liquid in the second-stage chlorination transfer kettle reaches the kettle volume of 1/2-2/3, materials in the second-stage chlorination transfer kettle are sent into the high-temperature chlorination liquid transfer groove in an amount of 1-1.5 m for cultivation per hour.
2. The method of claim 1, wherein the continuous high temperature chlorination of sucralose is performed by: the content of sucrose-6-ethyl ester in the esterification product in the step (1) is 320 g/l.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202011027939.9A CN112110963A (en) | 2020-09-26 | 2020-09-26 | Method for continuous high-temperature chlorination of sucralose |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202011027939.9A CN112110963A (en) | 2020-09-26 | 2020-09-26 | Method for continuous high-temperature chlorination of sucralose |
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| CN202011027939.9A Pending CN112110963A (en) | 2020-09-26 | 2020-09-26 | Method for continuous high-temperature chlorination of sucralose |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5908922A (en) * | 1996-04-02 | 1999-06-01 | Mitsubishi Chemical Corporation | Method for producing a sucrose fatty acid ester |
| WO2008084197A1 (en) * | 2007-01-09 | 2008-07-17 | Tate & Lyle Technology Limited | Method for the synthesis of sucrose-6-esters |
| CN105111250A (en) * | 2015-08-28 | 2015-12-02 | 山东康宝生化科技有限公司 | Method for preparing sucralose-6-ester by utilizing bis(trichloromethyl)carbonate |
| CN109724368A (en) * | 2018-12-10 | 2019-05-07 | 安徽金禾实业股份有限公司 | The recovery method of chlorinated exhaust in a kind of production of Sucralose |
-
2020
- 2020-09-26 CN CN202011027939.9A patent/CN112110963A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5908922A (en) * | 1996-04-02 | 1999-06-01 | Mitsubishi Chemical Corporation | Method for producing a sucrose fatty acid ester |
| WO2008084197A1 (en) * | 2007-01-09 | 2008-07-17 | Tate & Lyle Technology Limited | Method for the synthesis of sucrose-6-esters |
| CN105111250A (en) * | 2015-08-28 | 2015-12-02 | 山东康宝生化科技有限公司 | Method for preparing sucralose-6-ester by utilizing bis(trichloromethyl)carbonate |
| CN109724368A (en) * | 2018-12-10 | 2019-05-07 | 安徽金禾实业股份有限公司 | The recovery method of chlorinated exhaust in a kind of production of Sucralose |
Non-Patent Citations (2)
| Title |
|---|
| 天津大学化工学院主编: "《注册化工工程师执业资格考试专业考试复习教程》", 31 July 2016, 天津大学出版社 * |
| 崔灿 等: "三氯蔗糖制备工艺中氯化反应的优化研究", 《中国食品添加剂》 * |
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Application publication date: 20201222 |