CN112574265A - Method and device for continuous high-temperature reaction of sucralose - Google Patents
Method and device for continuous high-temperature reaction of sucralose Download PDFInfo
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- CN112574265A CN112574265A CN202011365527.6A CN202011365527A CN112574265A CN 112574265 A CN112574265 A CN 112574265A CN 202011365527 A CN202011365527 A CN 202011365527A CN 112574265 A CN112574265 A CN 112574265A
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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- C07H5/00—Compounds containing saccharide radicals in which the hetero bonds to oxygen have been replaced by the same number of hetero bonds to halogen, nitrogen, sulfur, selenium, or tellurium
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- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
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Abstract
The invention relates to a method and a device for continuous high-temperature reaction of sucralose, which are characterized in that: (1) heating the low-temperature chlorination solution by a No. 1 reboiler, sending the heated low-temperature chlorination solution into a No. 1 high-temperature chlorination reaction tower, controlling the temperature at 68-71 ℃ and the pressure at-4 to-2 Mpa in the tower, condensing the gas from the top of the tower, returning the condensed gas into the tower, and circularly heating the condensed gas for 30min to obtain a solution A; (2) heating the solution A by a 2# reboiler, then feeding the solution A into a 2# high-temperature chlorination reaction tower, controlling the temperature in the tower to be 98-101 ℃ and the pressure to be-4 to-2 Mpa, condensing the gas from the top of the tower, then returning the gas into the tower, and circularly heating the gas for 60min to obtain a solution B; (3) and heating the solution B by a 3# reboiler, then feeding the solution B into a 3# high-temperature chlorination reaction tower, controlling the temperature in the tower to be 109-DEG C and the pressure to be-4 to-2 Mpa, condensing the gas from the top of the tower, returning the condensed gas into the tower, and circularly heating the condensed gas for 120min to obtain a solution C. The invention has the advantages that: 3 high-temperature chlorination reaction towers are connected in series, so that continuous reaction can be realized, the heating rate is increased, the pressure and the heating environment of a high-temperature chlorination system are optimized, the quality and the yield of products are improved, and the emission amount of tail gas is reduced.
Description
Technical Field
The invention belongs to the technical field of sucralose production, and relates to a method and a device for continuous high-temperature reaction of trichloroethane.
Background
Sucralose is obtained by substituting hydroxyl groups at three positions of 4, 1 and 6 in a sucrose molecule with chlorine atoms. The sucrose molecule has 8 hydroxyl groups in total, and 3 hydroxyl groups at specific positions are replaced by selective chlorination, while the hydroxyl groups at other positions are not changed, which is difficult of course, and the synthesis of sucralose is more difficult because the reactivity of the hydroxyl groups at each position is different. The existing process mostly puts the esterification liquid which is well reacted at low temperature into a high-temperature reaction kettle to carry out high-temperature reaction in three stages, mostly adopts single kettle reaction, has discontinuous reaction, is not easy to control the reaction, has insufficient reaction, wastes time and labor, and causes the increase of production cost.
Disclosure of Invention
The present invention aims at solving the problems and providing a method and a device for continuous high temperature reaction of trichloroethane.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a device for continuous high-temperature reaction of trichloroethane is characterized in that: the original high-temperature chlorination reaction kettle is replaced by three high-temperature chlorination reaction towers which are connected in series, a reboiler, a condenser and a reflux tank are connected to each high-temperature chlorination reaction tower, and the high-temperature chlorination reactor can realize self circulation.
A method for continuous high-temperature reaction of sucralose is characterized by comprising the following steps:
(1) introducing the low-temperature chlorination liquid from the previous working section into a No. 1 reboiler in an amount of 10-12 m/h, heating the low-temperature chlorination liquid from the previous working section to 30-40 ℃ by the No. 1 reboiler, then introducing the high-temperature chlorination liquid into a No. 1 high-temperature chlorination reaction tower, opening circulation, controlling the temperature in the No. 1 high-temperature chlorination reaction tower to be 68-71 ℃ and the pressure to be-4 to-2 MPa, condensing the gas (trichloroethane gas) from the top of the No. 1 high-temperature chlorination reaction tower through a condenser at 1# (20-35 ℃), then introducing the gas into a No. 1 reflux tank, then returning the gas into the No. 1 high-temperature chlorination reaction tower through the No. 1 reflux tank, and circularly;
(2) extracting the solution A from the bottom of a No. 1 high-temperature chlorination reaction tower in an amount of 10-12 m/h, heating the solution A to 90-93 ℃ by a No. 2 reboiler, then entering the No. 2 high-temperature chlorination reaction tower, opening a cycle, controlling the temperature in the No. 2 high-temperature chlorination reaction tower to be 98-101 ℃ and the pressure to be-4 to-2 MPa, condensing the gas (trichloroethane gas) from the top of the No. 2 high-temperature chlorination reaction tower by a condenser No. 2 (20-35 ℃), then entering a No. 2 reflux tank, then returning the gas to the No. 2 high-temperature chlorination reaction tower through the No. 2 reflux tank, and circularly heating for 60min to obtain a solution B;
(3) extracting the solution B from the bottom of a 2# high-temperature chlorination reaction tower in an amount of 10-12L/h, heating the solution B to 106-.
Compared with the prior art, the invention has the following advantages:
1. the device is simple, the original high-temperature chlorination reaction kettle is replaced by connecting 3 high-temperature chlorination reaction towers in series, so that continuous reaction can be realized, the link of manual material receiving is omitted, and manpower is saved;
2. the temperature rise rate is improved by entering different reaction towers at different stages, the pressure and temperature rise environment of a high-temperature chlorination system are optimized, the quality (the content is improved from 40-45% to 55-60%) and the yield (improved by 60%) of the product are improved, and the emission amount of tail gas is reduced;
3. the energy consumption and the abrasion of equipment are reduced, the labor amount of operation is reduced, the cost is reduced, and the operation safety is improved.
Drawings
FIG. 1 is a schematic diagram of a continuous high temperature reaction process for sucralose;
FIG. 2 is a schematic diagram of a conventional process.
Detailed Description
The invention is further illustrated with reference to fig. 1:
a device for continuous high-temperature reaction of trichloroethane comprises the following devices: the bottom outlet of the 1# high-temperature chlorination reaction tower is connected with the top inlet of the 3# high-temperature chlorination reaction tower through a pipeline and the 3# reboiler; the outlet at the top of the 1# high-temperature chlorination reaction tower is sequentially connected with a condenser 1# and a 1# reflux tank through a pipeline, the outlet of the 1# reflux tank is connected to the inlet at the top of the 1# high-temperature chlorination reaction tower, the outlet at the top of the 2# high-temperature chlorination reaction tower is sequentially connected with a condenser 2# and a 2# reflux tank through a pipeline, the outlet of the 2# reflux tank is connected to the inlet at the top of the 2# high-temperature chlorination reaction tower, the outlet at the top of the 3# high-temperature chlorination reaction tower is sequentially connected with a condenser 3# and a 3# reflux tank through a pipeline, and the outlet of the 3# reflux tank is connected to; the bottom of 1# high temperature chlorination reaction tower, 2# high temperature chlorination reaction tower, 3# high temperature chlorination reaction tower all are equipped with the pipeline and realize self circulation, and the vent gas in 1# reflux tank, 2# reflux tank, the 3# reflux tank passes through the pipeline and sends tail gas processing system.
A method for continuous high-temperature reaction of sucralose specifically comprises the following steps:
example 1
(1) Introducing the low-temperature chlorination liquid from the previous working section into a No. 1 reboiler at the rate of 10 m/h, heating the low-temperature chlorination liquid to 35 ℃ by the No. 1 reboiler, then introducing the low-temperature chlorination liquid into a No. 1 high-temperature chlorination reaction tower, opening circulation, controlling the temperature in the No. 1 high-temperature chlorination reaction tower to be 69 ℃ and the pressure to be-3 Mpa, condensing the gas (trichloroethane gas) coming out of the top of the No. 1 high-temperature chlorination reaction tower through a condenser at the temperature of No. 1 (28 ℃), introducing the condensed gas into a No. 1 reflux tank, then returning the condensed gas into the No. 1 high-temperature chlorination reaction tower through the No. 1 reflux;
(2) b, extracting the solution A from the bottom of a No. 1 high-temperature chlorination reaction tower in an amount of 10 m/h, heating the solution A to 92 ℃ by a No. 2 reboiler, then feeding the solution A into a No. 2 high-temperature chlorination reaction tower, opening a cycle, controlling the temperature in the No. 2 high-temperature chlorination reaction tower to be 99 ℃ and the pressure to be-3 Mpa, condensing the gas (trichloroethane gas) coming out of the top of the No. 2 high-temperature chlorination reaction tower through a condenser No. 2 (28 ℃), feeding the condensed gas into a No. 2 reflux tank, then returning the condensed gas into the No. 2 high-temperature chlorination reaction tower through the No. 2 reflux tank, and circularly heating the condensed;
(3) and (2) extracting the solution B from the bottom of a 2# high-temperature chlorination reaction tower in an amount of 10 m/h, heating the solution B to 106 ℃ by a 3# reboiler, then entering the 3# high-temperature chlorination reaction tower, opening a cycle, controlling the temperature in the 3# high-temperature chlorination reaction tower to be 110 ℃ and the pressure to be-43 Mpa, condensing the gas (trichloroethane gas) coming out of the top of the 3# high-temperature chlorination reaction tower through a condenser 3# (28 ℃), then entering a 3# reflux tank, returning the gas into the 3# high-temperature chlorination reaction tower through the 3# reflux tank, circularly heating the gas for 120min to obtain a solution C, and then extracting the solution C from the bottom of the 3# high-temperature chlorination reaction tower.
Example 2
(1) Introducing the low-temperature chlorination liquid from the previous working section into a No. 1 reboiler at the rate of 11 m/h, heating the low-temperature chlorination liquid to 32 ℃ by the No. 1 reboiler, then conveying the heated low-temperature chlorination liquid into a No. 1 high-temperature chlorination reaction tower, opening a cycle, controlling the temperature in the No. 1 high-temperature chlorination reaction tower to be 68 ℃ and the pressure to be-4 Mpa, condensing the gas (trichloroethane gas) coming out of the top of the No. 1 high-temperature chlorination reaction tower through a condenser at the temperature of No. 1 (22 ℃), then introducing the condensed gas into a No. 1 reflux tank, then returning the condensed gas into the No. 1 high-temperature chlorination reaction tower through the;
(2) extracting the solution A from the bottom of a No. 1 high-temperature chlorination reaction tower in an amount of 11 m/h, heating the solution A to 90 ℃ by a No. 2 reboiler, then entering the No. 2 high-temperature chlorination reaction tower, opening a cycle, controlling the temperature in the No. 2 high-temperature chlorination reaction tower to be 98 ℃ and the pressure to be-4 Mpa, condensing the gas (trichloroethane gas) coming out of the top of the No. 2 high-temperature chlorination reaction tower through a condenser No. 2 (22 ℃), then entering a No. 2 reflux tank, then returning the gas to the No. 2 high-temperature chlorination reaction tower through the No. 2 reflux tank, and circularly heating for 60min to obtain a solution B;
(3) and (2) extracting the solution B from the bottom of a 2# high-temperature chlorination reaction tower in an amount of 11 m/h, heating the solution B to 106 ℃ by a 3# reboiler, then entering the 3# high-temperature chlorination reaction tower, opening a cycle, controlling the temperature in the 3# high-temperature chlorination reaction tower to be 109 ℃ and the pressure to be-4 Mpa, condensing the gas (trichloroethane gas) coming out of the top of the 3# high-temperature chlorination reaction tower through a condenser at the temperature of 3# (22 ℃), then entering a 3# reflux tank, then returning the gas into the 3# high-temperature chlorination reaction tower through the 3# reflux tank, circularly heating the gas for 120min to obtain a solution C, and then extracting the solution C from the bottom of the 3# high-temperature chlorination reaction.
Example 3
(1) Introducing the low-temperature chlorination liquid from the previous working section into a No. 1 reboiler in an amount of 12 m/h, heating the low-temperature chlorination liquid to 38 ℃ by the No. 1 reboiler, introducing the heated low-temperature chlorination liquid into a No. 1 high-temperature chlorination reaction tower, opening a cycle, controlling the temperature in the No. 1 high-temperature chlorination reaction tower to be 71 ℃ and the pressure to be-2 MPa, condensing the gas (trichloroethane gas) coming out of the top of the No. 1 high-temperature chlorination reaction tower through a condenser at the temperature of No. 1 (33 ℃), introducing the condensed gas into a No. 1 reflux tank, returning the condensed gas into the No. 1 high-temperature chlorination reaction tower through the No. 1 reflux tank;
(2) extracting the solution A from the bottom of a No. 1 high-temperature chlorination reaction tower in an amount of 12 m/h, heating the solution A to 93 ℃ by a No. 2 reboiler, then entering the No. 2 high-temperature chlorination reaction tower, opening a cycle, controlling the temperature in the No. 2 high-temperature chlorination reaction tower to be 101 ℃ and the pressure to be-2 Mpa, condensing the gas (trichloroethane gas) coming out of the top of the No. 2 high-temperature chlorination reaction tower through a condenser No. 2 (33 ℃), then entering a No. 2 reflux tank, then returning the gas to the No. 2 high-temperature chlorination reaction tower through the No. 2 reflux tank, and circularly heating for 60min to obtain a solution B;
(3) and (2) extracting the solution B from the bottom of a 2# high-temperature chlorination reaction tower in an amount of 12 m/h, heating the solution B to 107 ℃ by a 3# reboiler, then entering the 3# high-temperature chlorination reaction tower, opening a cycle, controlling the temperature in the 3# high-temperature chlorination reaction tower to be 111 ℃ and the pressure to be-2 Mpa, condensing the gas (trichloroethane gas) coming out of the top of the 3# high-temperature chlorination reaction tower through a condenser 3# (33 ℃) and then entering a 3# reflux tank, then returning the gas into the 3# high-temperature chlorination reaction tower through the 3# reflux tank, circularly heating the gas for 120min to obtain a solution C, and then extracting the solution C from the bottom of the 3# high-temperature chlorination reaction tower.
TABLE 1
TABLE 2
Claims (3)
1. A method for continuous high-temperature reaction of sucralose is characterized by comprising the following steps:
(1) introducing the low-temperature chlorination liquid from the previous working section into a No. 1 reboiler in an amount of 10-12 m/h, heating the low-temperature chlorination liquid from the previous working section to 30-40 ℃ by the No. 1 reboiler, then introducing the high-temperature chlorination liquid into a No. 1 high-temperature chlorination reaction tower, opening circulation, controlling the temperature in the No. 1 high-temperature chlorination reaction tower to be 68-71 ℃ and the pressure to be-4 to-2 MPa, condensing the gas from the top of the No. 1 high-temperature chlorination reaction tower by a condenser No. 1, introducing the gas into a No. 1 reflux tank, then returning the gas into the No. 1 high-temperature chlorination reaction tower through the No. 1 reflux tank, and circularly heating;
(2) extracting the solution A from the bottom of a No. 1 high-temperature chlorination reaction tower in an amount of 10-12 m/h, heating the solution A to 90-93 ℃ by a No. 2 reboiler, then entering the No. 2 high-temperature chlorination reaction tower, opening a cycle, controlling the temperature in the No. 2 high-temperature chlorination reaction tower to be 98-101 ℃ and the pressure to be-4 to-2 MPa, condensing the gas from the top of the No. 2 high-temperature chlorination reaction tower by a condenser No. 2, then entering a No. 2 reflux tank, then returning the gas to the No. 2 high-temperature chlorination reaction tower through the No. 2 reflux tank, and circularly heating for 60min to obtain a solution B;
(3) extracting the solution B from the bottom of a 2# high-temperature chlorination reaction tower in an amount of 10-12 m/h, heating the solution B to 106-.
2. The method of claim 1, wherein the continuous high temperature reaction of sucralose is as follows: the temperatures of the condenser 1#, the condenser 2# and the condenser 3# are 20-35 ℃.
3. A device for continuous high-temperature reaction of trichloroethane is characterized in that: the original high-temperature chlorination reaction kettle is replaced by three high-temperature chlorination reaction towers which are connected in series, a reboiler, a condenser and a reflux tank are connected to each high-temperature chlorination reaction tower, and the high-temperature chlorination reactor can realize self circulation.
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| CN202011365527.6A CN112574265A (en) | 2020-11-28 | 2020-11-28 | Method and device for continuous high-temperature reaction of sucralose |
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| CN202011365527.6A CN112574265A (en) | 2020-11-28 | 2020-11-28 | Method and device for continuous high-temperature reaction of sucralose |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113694862A (en) * | 2021-08-26 | 2021-11-26 | 山东康宝生化科技有限公司 | Built-in continuous temperature rising device and method for sucralose chlorination |
| CN114146673A (en) * | 2021-12-20 | 2022-03-08 | 安徽金禾实业股份有限公司 | Device and method for continuous neutralization in sucralose production |
-
2020
- 2020-11-28 CN CN202011365527.6A patent/CN112574265A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113694862A (en) * | 2021-08-26 | 2021-11-26 | 山东康宝生化科技有限公司 | Built-in continuous temperature rising device and method for sucralose chlorination |
| CN114146673A (en) * | 2021-12-20 | 2022-03-08 | 安徽金禾实业股份有限公司 | Device and method for continuous neutralization in sucralose production |
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