CN113694862A - Built-in continuous temperature rising device and method for sucralose chlorination - Google Patents
Built-in continuous temperature rising device and method for sucralose chlorination Download PDFInfo
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Abstract
The invention discloses a built-in continuous heating device and a built-in continuous heating method for sucralose chlorination, and the built-in continuous heating device comprises a continuous heating tower and a condenser, wherein the lower end of the continuous heating tower is provided with a tower kettle, the upper end of the continuous heating tower is provided with a built-in condensing tube array, the upper end of the tower kettle is provided with a built-in heater, a cavity section is arranged between the heater and the condensing tube array, the upper end of the condensing tube array is provided with a shell pass inlet, the lower end of the condensing tube array is provided with a shell pass outlet, and the cavity section is provided with a feed inlet and a liquid phase inlet; the gas outlet at the top of the continuous heating tower is connected with the inlet of a condenser, the liquid phase outlet of the condenser is connected with the liquid phase inlet of the cavity section, and the shell side outlet is connected with the feed inlet; and a steam jacket is arranged outside the tower kettle, and a steam water outlet of the heater is connected with a steam water inlet of the steam jacket. The device and the method not only fully utilize the heat and the refrigerating capacity of the materials, save a large amount of steam and refrigeration input, but also realize the continuous operation of a high-temperature chlorination working section in the production of the sucralose, and the temperature rise process does not need to wait intermittently.
Description
Technical Field
The invention relates to a sucralose production technology, in particular to a built-in continuous heating device and a built-in continuous heating method for sucralose chlorination.
Background
In the production process of sucralose, the high-temperature chlorination process mostly adopts an intermittent production process of a glass lining reaction kettle, as shown in figure 1, trichloroethane and thionyl chloride in a certain proportion are firstly added into a low-temperature chlorination kettle, saline water with the temperature of minus 20 ℃ is introduced into a jacket of the low-temperature chlorination kettle, and the temperature of materials in the kettle is controlled below 5 ℃. Then, dropping esterification liquid (DMF solution of sucrose-6-ethyl ester), controlling the dropping speed to ensure that the temperature in the low-temperature chlorination kettle is not more than 5 ℃, and carrying out Vickers chemical reaction to generate Vickers salt, wherein the formula is shown as follows:
sucrose ester reacts with Vickers salt to produce sucrose-6-ethyl ester-O-alkyl chloride salt, which is shown as the following formula:
after the low-temperature chlorination reaction is finished, the low-temperature chlorinated solution flows into a high-temperature chlorination kettle, steam is introduced into a jacket of the high-temperature chlorination kettle, the feed liquid is controlled to be heated in a stepped mode and is kept warm, and sucralose-6-ethyl-O-alkyl chloride salt is generated through the reaction, and the formula is shown as follows:
at present, a 12-hour high-temperature chlorination process (heating to 112 ℃ within 10 hours and then preserving heat for 2 hours) or a 7-hour high-temperature chlorination process (heating to 112 ℃ within 5 hours and then preserving heat for 2 hours) is mostly adopted in an industrial production workshop, the intermittent production consumes long time and needs a lot of equipment, the intermittent production is mainly limited by a glass lining reaction kettle, and the heat conduction rate and the heat transfer area are small by virtue of jacket steam heating of the glass lining reaction kettle.
The approximate composition of 1 batch of raw material liquid in the production plant is shown in the table 1, the 20.8 ton raw material liquid needs to be divided into 2 low-temperature chlorination kettles with 12.5m3,
TABLE 1
At present, the daily feeding amount of an industrial production workshop is 24 batches, the quality of a raw material liquid is 499.2 tons, each kettle is filled with 10.4 tons, and the time consumption of each batch of high-temperature chlorination is 10 hours, so that the number of the high-temperature chlorination kettles at least needs to be: 499.2 × 10 ÷ 10.4 ÷ 24 ÷ 20 stands.
Therefore, the existing batch production of the glass lining reaction kettle has the defects of various devices, high energy consumption (mainly steam power) and long production period.
Applicants have found experimentally that higher yields can be obtained by using a 1 hour temperature ramp to 118 ℃ and a 1.5 hour hold. The shorter the reaction time, the more likely it is to achieve a continuous high temperature chlorination process.
In conclusion, a new device is developed to accelerate the mass transfer and heat transfer rate of chlorination reaction, and the defect of intermittent production of the glass lining reaction kettle can be overcome.
The patent with application number 202011365527.6 discloses a method and a device for continuous high-temperature reaction of sucralose, which uses three high-temperature chlorination reaction towers connected in series and three reboilers for 'relay type' temperature rise to realize continuous high-temperature reaction, but the patent still has the following problems:
1. the reaction equipment is more, and three reboilers, three reaction towers and accessory equipment are required to be connected in series;
2. the energy consumption is high, the low-temperature chlorination liquid needs to be heated by a No. 1 reboiler, and after the trichloroethane is gasified, the low-temperature chlorination liquid needs to be condensed and refluxed;
3. the method is characterized in that the method does not realize continuous production, low-temperature chlorination liquid enters a No. 1 high-temperature chlorination reaction tower to be circularly heated for 30 minutes to obtain a solution A, then enters a No. 2 high-temperature chlorination reaction tower to be circularly heated for 60 minutes to obtain a solution B, and then enters a No. 3 high-temperature chlorination reaction tower to be circularly heated for 120 minutes to obtain a solution C, and the time periods of circular heating of the towers are different and are sequentially increased, so that the continuous production cannot be realized;
4. trichloroethane steam, hydrogen chloride and sulfur dioxide all go to the condenser of tower external, and the flow of material is big, and pipeline equipment all can be bigger, and 1 batch of high temperature chlorination liquid of workshop is constituteed as shown in table 2, and the trichloroethane accounts for than the biggest in the gaseous phase.
TABLE 2
The feed rate was 20.8 t/hr, the amount of trichloroethane vaporized per hour was 14.8 t, hydrogen chloride was 0.9 t, sulfur dioxide was 1.7 t, and the trichloroethane mass fraction was 85%. The gas flow rate was calculated as 22.4 liters per mol of the material and is shown in Table 3:
TABLE 3
The gas flow velocity in the pipeline is less than 5m/s, otherwise the gas velocity is too high to easily entrain materials and cause loss, and the minimum diameter of the pipeline and the condenser is calculated as
The condensers 1#, 2#, and 3# and their respective gas phase lines connecting the tops of the columns in the patent are relatively large.
If part of trichloroethane can be condensed and refluxed in the tower in advance, the gas flow to the condenser outside the tower is reduced, and the diameters of the pipeline and the condenser can be greatly reduced, so that the equipment investment is reduced.
In view of the above problems, we have developed a device and method for continuous temperature rise in a built-in sucralose chlorination process. The tower kettle, the heater and the condensing tube are integrated, the condensing tube can realize heat exchange between trichloroethane gas phase and low-temperature chlorination liquid, and secondary steam discharged by the heater continuously heats the tower kettle, so that the low-temperature chlorination liquid is heated for three times in the same equipment, namely, the trichloroethane gas phase heating, the heater heating, the tower kettle heating and the temperature step type lifting are carried out, and the phenomenon that materials are carbonized when the temperature is directly raised to be higher than 112 ℃ is avoided. In addition, the low-temperature chlorinated liquid has lower temperature, and can well lower the temperature of trichloroethane gas phase, thereby saving a large amount of refrigeration investment compared with the prior art.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provides a built-in continuous heating device and method for sucralose chlorination.
In order to achieve the purpose, the technical scheme of the invention is as follows: a built-in continuous heating device for sucralose chlorination is characterized in that: the continuous heating tower comprises a continuous heating tower and a condenser, wherein a tower kettle is arranged at the lower end of the continuous heating tower, a tubular heater is arranged in the upper end of the tower kettle of the continuous heating tower, a condensing tubular is arranged in the upper end of the interior of the continuous heating tower, a cavity section is arranged between the heater and the condensing tubular, a shell side inlet is arranged at the upper end of the condensing tubular, a shell side outlet is arranged at the lower end of the condensing tubular, a feed inlet is arranged in the center of the cavity section, and a liquid phase inlet is arranged at the upper end of the feed inlet of the cavity section; the gas outlet at the top of the continuous heating tower is connected with the inlet of a condenser through a pipeline, the gas outlet of the condenser is connected with a tail gas treatment pipeline, the liquid outlet of the condenser is connected with the liquid inlet of the cavity section through a pipeline, and the shell side outlet of the condenser is connected with the feed inlet through a pipeline; the tower kettle is externally provided with a steam jacket, the kettle bottom is provided with a recovery port, the heater is provided with a steam inlet and a steam water outlet, and the steam water outlet is connected with the steam water inlet of the steam jacket through a pipeline.
Further, the method comprises the following steps of; still be equipped with the circulation export at the bottom of the tower cauldron, the cavity section is equipped with circulation entry at the feed inlet lower extreme, the circulation export passes through pipe connection circulation entry, be equipped with at least one circulating pump, second flowmeter and second thermometer on the connecting line of circulation export.
Further, the method comprises the following steps of; and the continuous heating tower is provided with a first differential pressure liquid level meter at the top of the upper tube plate of the heater and a second differential pressure liquid level meter at the height position of the circulating inlet.
Further, the method comprises the following steps of; the shell pass inlet is connected with a feeding pipeline, at least one feeding pump is arranged on the feeding pipeline, and a first flowmeter and a first thermometer are arranged between the feeding pump and the shell pass inlet.
Further, the method comprises the following steps of; and a connecting pipeline between the shell side outlet and the feed inlet is provided with a fifth thermometer, a connecting pipeline of an air outlet at the top of the continuous heating tower is provided with a fourth thermometer, and a connecting pipeline of a liquid phase outlet of the condenser is provided with a sixth thermometer.
Further, the method comprises the following steps of; the tower kettle extraction outlet is connected with a downstream device through a pipeline, and a third flowmeter, a third thermometer and at least one extraction pump are arranged on the extraction outlet connecting pipeline.
The other technical scheme of the invention is as follows: a sucralose chlorination built-in continuous heating method is characterized by comprising the following steps:
(1) the feeding pump conveys low-temperature chlorination liquid from the low-temperature chlorination working section to a shell pass inlet of a condensing shell and tube, the low-temperature chlorination liquid enters the shell pass of the condensing shell and tube, is heated by ascending trichloroethane gas phase in the descending process of the shell pass of the condensing shell and tube, flows out from a shell pass outlet of the condensing shell and tube after the first heating is finished, and enters a cavity section through a feeding hole;
(2) the chlorination liquid entering the cavity section falls into the tube pass of the heater under the action of gravity, is heated by steam in the tube pass of the heater, and enters the tower kettle after the secondary heating is finished;
(3) steam in the tube pass of the heater flows out through a steam water outlet, then enters a steam jacket of the tower kettle through a steam water inlet of the steam jacket of the tower kettle to heat the tower kettle, and the chlorination liquid entering the tower kettle is heated for the third time in the tower kettle;
(4) the high-temperature chlorination liquid in the tower kettle is conveyed to a circulating inlet through a circulating pump to enter a cavity section, and falls into a tube pass of a heater under the action of gravity to realize circulating heating; the other part is extracted through an extraction outlet and is conveyed to a downstream device through an extraction pump;
(5) after the chlorinated liquid is heated in the continuous heating tower, trichloroethane is gasified and rises to enter the cavity section, then the chlorinated liquid continuously rises to enter a condensing tube shell pass, the chlorinated liquid is condensed and liquefied by low-temperature chlorinated liquid in the condensing tube shell pass, then the chlorinated liquid falls into the tower again under the action of gravity, a small part of uncondensed trichloroethane gas phase enters a condenser for condensation and liquefaction, the liquefied gas phase is discharged from a liquid phase outlet and flows into the continuous heating tower through a liquid phase inlet, and the uncondensed gas phase enters a tail gas treatment pipeline through a gas phase outlet.
Further, the method comprises the following steps of; the temperature of the low-temperature chlorinated fluid conveyed to the shell pass inlet of the condensation tube array in the step (1) is 5 ℃, the temperature of the chlorinated fluid flowing out of the shell pass outlet of the condensation tube array after the first heating is finished is 79-82 ℃, the temperature of the high-temperature chlorinated fluid conveyed to the circulation inlet through the circulation pump in the step (4) is 116-.
Further, the method comprises the following steps of; the flow of the extraction pump plus the flow of the gas phase outlet of the condenser is balanced with the flow of the feeding pump.
Further, the method comprises the following steps of; the liquid level of the materials in the cavity section is near the middle position of the upper tube plate of the heater and the circulating inlet, the liquid level (L) of the materials is measured by a first differential pressure liquid level meter and a second differential pressure liquid level meter, the liquid level range is 1m, and L floats between 0.2m and 0.8 m.
The invention has the beneficial effects that: the built-in continuous temperature raising device for sucralose chlorination integrates a tower kettle, a heater and a condensing tube array, wherein the condensing tube array can realize heat exchange between a trichloroethane gas phase and a low-temperature chlorination liquid, and secondary steam discharged by the heater continuously heats the tower kettle, so that the low-temperature chlorination liquid is heated for three times in a continuous temperature raising tower, and the three times are respectively heated by the trichloroethane gas phase, the heater and the tower kettle, and the temperature is raised in a step manner, so that the phenomenon that materials are carbonized when the temperature is directly raised to be higher than 112 ℃ is avoided. In addition, the low-temperature chlorination liquid has lower temperature, and can well cool the gaseous phase of trichloroethane, so that compared with the prior art, the device and the method not only fully utilize the heat and the refrigerating capacity of the materials, save a large amount of steam and refrigerating investment, but also realize the continuous operation of a high-temperature chlorination working section in the production of sucralose, and do not need intermittent waiting in the temperature rise process.
Because partial trichloroethane gas phase is condensed and refluxed in the condensing tube section, the gas flow to the condenser outside the tower is reduced, so that the pipe diameter of the gas outlet pipeline at the top of the continuous heating tower and the diameter of the condenser can be greatly reduced, and the equipment investment is reduced.
Drawings
FIG. 1 is a schematic diagram of a prior art structure in the background art;
FIG. 2 is a schematic structural view of the present invention;
in fig. 2: 1. continuously heating the tower; 2. a condenser; 3. a tower kettle; 4. a heater; 5. a condensation tube array; 6. a cavity section; 7. a shell side inlet; 8. a shell-side outlet; 9. a feed inlet; 10. a liquid phase inlet; 11. a tail gas treatment line; 12. a steam jacket; 13. a recycle inlet; 14. a recycle outlet; 15. a production port; 16. a first differential pressure liquid level meter; 17. a second differential pressure liquid level meter; 18. a feed pump; 19. a production pump; 20. a circulation pump; f01, first flow meter; TO1, first thermometer; f02, second flow meter; TO2, second thermometer; f03, a third flow meter; TO3, third thermometer; TO4, fourth thermometer; TO5, fifth thermometer; TO6, sixth thermometer.
Detailed Description
Example 1:
as shown in fig. 2, a built-in continuous temperature raising device for sucralose chlorination comprises a continuous temperature raising tower 1 and a condenser 2, wherein the lower end of the continuous temperature raising tower 1 is a tower kettle 3, a tubular heater 4 is built in the upper end of the tower kettle 3 of the continuous temperature raising tower 1, a condensing tubular 5 is built in the upper end of the continuous temperature raising tower 1, a cavity section 6 is arranged between the heater 4 and the condensing tubular 5, the upper end of the condensing tubular 5 is provided with a shell side inlet 7, the lower end of the condensing tubular 5 is provided with a shell side outlet 8, the center of the cavity section 6 is provided with a feed inlet 9, and the upper end of the feed inlet 9 of the cavity section 6 is provided with a liquid phase inlet 10; 2 entrys of tube coupling condenser are passed through TO1 top gas outlet in continuous heating tower, 2 gaseous phase exit linkage tail gas treatment pipeline 11 of condenser, liquid phase export pass through the liquid phase import 10 of tube coupling cavity section 6, shell side export 8 passes through tube coupling feed inlet 9, be equipped with fifth thermometer TO5 on the connecting line between shell side export 8 and the feed inlet 9, shell side import 7 connects the feed line, be equipped with two charge-in pumps 18 on the feed line, be equipped with first flowmeter F01 and first thermometer TO1 between charge-in pump 18 and the shell side import 7, two charge-in pumps 18 parallel connection.
The tower kettle 3 is externally provided with a steam jacket 12, the kettle bottom is provided with a sampling port 15, the heater 4 is provided with a steam inlet and a steam water outlet, and the steam water outlet is connected with the steam jacket 12 through a pipeline.
Still be equipped with circulation outlet 14 at the bottom of 3 cauldron in tower cauldron, cavity section 6 is equipped with circulation inlet 13 at the feed inlet lower extreme, circulation outlet 14 passes through pipe connection circulation inlet 13, be equipped with two circulating pumps 20, second flowmeter F02 and second thermometer TO2 on circulation outlet 14's the connecting line, two circulating pumps 20 parallel connection.
Continuous heating tower 1 is equipped with first differential pressure level gauge 16, is equipped with second differential pressure level gauge 17 at circulation entry 13 high position on the tube sheet top on heater 4, be equipped with fourth thermometer TO4 on the 1 top gas outlet connecting line of continuous heating tower, be equipped with sixth thermometer TO6 on the 2 liquid phase export connecting line of condenser, the 15 of tower cauldron 3 extraction port passes through the pipeline connection low reaches device, be equipped with third flowmeter F03, third thermometer TO3 and two extraction pumps 19 on the 15 connecting line of extraction port, two extraction pumps 19 parallel connection.
Example 2:
a sucralose chlorination built-in continuous heating method comprises the following steps:
(1) the feed pump 18 conveys low-temperature chlorination liquid from a low-temperature chlorination working section TO a shell pass inlet 7 of a condensing tube array 5, a first thermometer T01 is 5 ℃, the flow rate of a first flowmeter F01 is 20.8T/h, the low-temperature chlorination liquid enters the shell pass of the condensing tube array 5, is heated by ascending trichloroethane gas phase in the descending process of the shell pass of the condensing tube array 5, flows out from a shell pass outlet 8 after first heating is completed, and enters a cavity section 6 through a feed inlet 9, and the temperature of a fifth thermometer TO5 is 81 ℃;
(2) the chlorination liquid entering the cavity section 6 falls into the tube pass of the heater 4 under the action of gravity, is heated by steam in the tube pass of the heater 4, and enters the tower kettle 3 after the secondary heating is finished;
(3) steam in the tube pass of the heater 4 flows out through a steam water outlet, then enters the steam jacket 12 through a steam water inlet of the steam jacket 12 of the tower kettle 3 to heat the tower kettle 3, the chlorination liquid entering the tower kettle 3 is heated for the third time in the tower kettle 3, the liquid level of the material in the cavity section 6 is near the middle position of the upper tube plate of the heater 4 and the circulating inlet 13, and L is 0.5 m.
(4) Part of the high-temperature chlorination liquid in the tower kettle 3 is conveyed to a circulating inlet 13 through a circulating pump 20 to enter a cavity section 6, and falls into a tube side of a heater 4 under the action of gravity to realize circulating heating, wherein the temperature of a second thermometer T02 is 118 ℃, and the flow of a second flowmeter F02 is 39.6T/h; the other part is extracted through an extraction outlet 15 and is conveyed to a downstream device through an extraction pump 19, the temperature of a third thermometer T03 is 117 ℃, and the flow of a third flowmeter F03 is 18.3T/h;
(5) after the chlorinated liquid is heated in the continuous heating tower 1, trichloroethane is gasified and rises to enter the cavity section 6, then the chlorinated liquid continuously rises to enter a shell pass of a condensing tube array 5, the chlorinated liquid is condensed and liquefied by low-temperature chlorinated liquid in the shell pass of the condensing tube array 5, then the chlorinated liquid falls into the tower again under the action of gravity, a small part of uncondensed trichloroethane gas phase enters a condenser 2 from a gas outlet at the top of the continuous heating tower 1 for condensation and liquefaction, a fourth thermometer T04 has the temperature of 95 ℃, the liquefied chlorinated liquid phase is discharged from a liquid phase outlet of the condenser 2 and flows into the continuous heating tower 1 through a liquid phase inlet 10, a sixth thermometer T06 has the temperature of 45 ℃, the uncondensed gas phase enters a tail gas treatment pipeline 11 through a gas phase outlet of the condenser 2 and is conveyed to a tail gas separation device, the flow of the extraction pump 19 and the gas phase outlet flow of the condenser 2 are balanced with the flow of a feed pump 18, and the uncondensed gas phase mainly comprises sulfur dioxide and hydrogen chloride gases, and separating and canning the mixture in a tail gas separation device to obtain a liquefied high-purity hydrogen chloride product and a sulfur dioxide product.
Example 3-example 4:
examples 3-4 differ from example 2 in the flow and temperature parameters and the material level, the specific parameter values are shown in table 4.
TABLE 4
Example 5:
765g of feed liquid (49 g of cane sugar equivalent) extracted by the extraction pump 19 in the embodiment 4 is taken, the temperature is reduced to5 ℃, ammonia water is added dropwise, the pH value of the feed liquid is adjusted to 10, stirring is continued for 5 minutes, and hydrochloric acid is added dropwise to adjust the pH value of the feed liquid to 7. The temperature during the pH adjustment does not exceed 10 ℃.
Putting the feed liquid with the adjusted pH value into a rotary evaporator, removing trichloroethane, DMF (dimethyl formamide) and water under a negative pressure state to obtain syrup, supplementing a proper amount of water, diluting the syrup, performing suction filtration to obtain 17 g of solid filter residue and 370mL of filtrate, and analyzing the filtrate, wherein the pH value is shown in Table 5:
TABLE 5
| Content of liquid chromatography | Content of external standard | |
| Monochloro sucrose | 1.31％ | |
| Dichlorosucrose | 4.97％ | |
| Sucralose | 0.61％ | 0.91g/L |
| Tetrachlorosucrose | 6.85％ | |
| Sucralose-6-ethyl ester | 58.66％ | 91.69g/L |
The mass of sucralose-6-ethyl ester in the filtrate was 91.69 × 0.370 ═ 33.92 g.
The yield was 33.92 ÷ 49 ÷ 69.22%.
Comparative example 1:
and (3) putting 856g (49 g of sucrose equivalent) of low-temperature chlorination liquid from a low-temperature chlorination section into a 1000mL four-neck flask, starting stirring at the temperature of 5 ℃, starting an oil bath for heating, uniformly heating the liquid to 112 ℃ within 10 hours, and then preserving the heat at 112 ℃ for 2 hours.
Then cooling to5 ℃, dropwise adding ammonia water, adjusting the pH value of the feed liquid to 10, continuously stirring for 5 minutes, and dropwise adding hydrochloric acid to adjust the pH value of the feed liquid to 7. The temperature during the pH adjustment does not exceed 10 ℃.
Putting the feed liquid with the adjusted pH value into a rotary evaporator, removing trichloroethane, DMF and water under the negative pressure state to obtain syrup, supplementing a proper amount of water, diluting the syrup, performing suction filtration to obtain 19g of solid filter residue and 375mL of filtrate, and analyzing the filtrate, wherein the pH value is shown in Table 6:
TABLE 6
| Content of liquid chromatography | Content of external standard | |
| Monochloro sucrose | 1.66％ | |
| Dichlorosucrose | 5.30％ | |
| Sucralose | 1.68％ | 2.27g/L |
| Tetrachlorosucrose | 6.58％ | |
| Sucralose-6-ethyl ester | 57.87％ | 83.07g/L |
The mass of sucralose-6-ethyl ester in the filtrate was 83.07 × 0.375 ═ 31.15 g.
The yield was 31.15 ÷ 49 ═ 63.57%.
Comparative example 2:
taking 515g of low-temperature chlorination liquid (29.5 g of cane sugar equivalent) from a low-temperature chlorination section, putting the low-temperature chlorination liquid into a 1000mL four-neck flask, starting stirring at the temperature of 5 ℃, starting oil bath for heating, uniformly heating the liquid to 112 ℃ within 5 hours, and then preserving the heat at 112 ℃ for 2 hours.
Then cooling to5 ℃, dropwise adding ammonia water, adjusting the pH value of the feed liquid to 10, continuously stirring for 5 minutes, and dropwise adding hydrochloric acid to adjust the pH value of the feed liquid to 7. The temperature during the pH adjustment does not exceed 10 ℃.
Putting the feed liquid with the adjusted pH value into a rotary evaporator, removing trichloroethane, DMF (dimethyl formamide) and water under a negative pressure state to obtain syrup, supplementing a proper amount of water, diluting the syrup, performing suction filtration to obtain 12g of solid filter residue and 263mL of filtrate, and analyzing the filtrate, wherein the pH value is shown in Table 7:
TABLE 7
| Content of liquid chromatography | Content of external standard | |
| Monochloro sucrose | 1.56％ | |
| Dichlorosucrose | 5.76％ | |
| Sucralose | 2.19％ | 2.53g/L |
| Tetrachlorosucrose | 6.04％ | |
| Sucralose-6-ethyl ester | 58.69％ | 72.12g/L |
The mass of sucralose-6-ethyl ester in the filtrate was 72.12 × 0.263-18.97 g.
The yield was 18.97 ÷ 29.5 ═ 64.31%.
Comparative example 3:
855g of low-temperature chlorination liquid (49 g of sucrose equivalent) from the low-temperature chlorination section is taken and placed into a 1000mL four-neck flask, the temperature is 5 ℃, stirring is started, oil bath heating is started, the liquid is heated to 118 ℃ at a constant speed for 1 hour, and then the temperature of 118 ℃ is kept for 1.5 hours.
Then cooling to5 ℃, dropwise adding ammonia water, adjusting the pH value of the feed liquid to 10, continuously stirring for 5 minutes, and dropwise adding hydrochloric acid to adjust the pH value of the feed liquid to 7. The temperature during the pH adjustment does not exceed 10 ℃.
Putting the feed liquid with the adjusted pH value into a rotary evaporator, removing trichloroethane, DMF (dimethyl formamide) and water under a negative pressure state to obtain syrup, supplementing a proper amount of water, diluting the syrup, performing suction filtration to obtain 13g of solid filter residue and 280mL of filtrate, and analyzing the filtrate, wherein the pH value is shown in Table 8:
TABLE 8
| Content of liquid chromatography | Content of external standard | |
| Monochloro sucrose | 1.99％ | |
| Dichlorosucrose | 7.04％ | |
| Sucralose | 1.26％ | 2.22g/L |
| Tetrachlorosucrose | 4.82％ | |
| Sucralose-6-ethyl ester | 65.06％ | 121.63g/L |
The mass of sucralose-6-ethyl ester in the filtrate was 121.63 × 0.280 ═ 34.06 g.
The yield was 34.06 ÷ 49 ═ 69.51%.
The experimental results of the example 5 and the comparative examples 1 to3 show that the continuous operation of the high-temperature chlorination section in the sucralose production can be realized, and higher yield can be obtained.
The above-described embodiments are merely preferred embodiments of the present invention, which is not intended to be limiting in any way, and other variations and modifications are possible without departing from the scope of the invention as set forth in the appended claims.
In the description of the present invention, it is to be understood that the terms indicating an orientation or positional relationship are based on the orientation or positional relationship shown in the drawings only for the convenience of describing the present invention and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and thus, should not be construed as limiting the present invention.
Claims (10)
1. A built-in continuous heating device for sucralose chlorination is characterized in that: the continuous heating tower comprises a continuous heating tower and a condenser, wherein a tower kettle is arranged at the lower end of the continuous heating tower, a heater is arranged in the continuous heating tower at the upper end of the tower kettle, a condensing tube is arranged in the continuous heating tower at the upper end, a cavity section is arranged between the heater and the condensing tube, a shell side inlet is arranged at the upper end of the condensing tube, a shell side outlet is arranged at the lower end of the condensing tube, a feed port is arranged in the center of the cavity section, and a liquid phase inlet is arranged at the upper end of the feed port of the cavity section; the gas outlet at the top of the continuous heating tower is connected with the inlet of a condenser through a pipeline, the gas outlet of the condenser is connected with a tail gas treatment pipeline, the liquid outlet of the condenser is connected with the liquid inlet of the cavity section through a pipeline, and the shell side outlet of the condenser is connected with the feed inlet through a pipeline; the tower kettle is externally provided with a steam jacket, the kettle bottom is provided with a recovery port, the heater is provided with a steam inlet and a steam water outlet, and the steam water outlet is connected with the steam water inlet of the steam jacket through a pipeline.
2. The sucralose chlorination built-in continuous heating device according to claim 1, wherein: still be equipped with the circulation export at the bottom of the tower cauldron, the cavity section is equipped with circulation entry at the feed inlet lower extreme, the circulation export passes through pipe connection circulation entry, be equipped with at least one circulating pump, second flowmeter and second thermometer on the connecting line of circulation export.
3. The sucralose chlorination built-in continuous heating device according to claim 1, wherein: and the continuous heating tower is provided with a first differential pressure liquid level meter at the top of the upper tube plate of the heater and a second differential pressure liquid level meter at the height position of the circulating inlet.
4. The sucralose chlorination built-in continuous heating device according to claim 1, wherein: the shell pass inlet is connected with a feeding pipeline, at least one feeding pump is arranged on the feeding pipeline, and a first flowmeter and a first thermometer are arranged between the feeding pump and the shell pass inlet.
5. The sucralose chlorination built-in continuous heating device according to claim 1, wherein: and a connecting pipeline between the shell side outlet and the feed inlet is provided with a fifth thermometer, a connecting pipeline of an air outlet at the top of the continuous heating tower is provided with a fourth thermometer, and a connecting pipeline of a liquid phase outlet of the condenser is provided with a sixth thermometer.
6. The sucralose chlorination built-in continuous heating device according to claim 1, wherein: the tower kettle extraction outlet is connected with a downstream device through a pipeline, and a third flowmeter, a third thermometer and at least one extraction pump are arranged on the extraction outlet connecting pipeline.
7. A sucralose chlorination built-in continuous heating method is characterized by comprising the following steps:
(1) the feeding pump conveys low-temperature chlorination liquid from the low-temperature chlorination working section to a shell pass inlet of a condensing shell and tube, the low-temperature chlorination liquid enters the shell pass of the condensing shell and tube, is heated by ascending trichloroethane gas phase in the descending process of the shell pass of the condensing shell and tube, flows out from a shell pass outlet of the condensing shell and tube after the first heating is finished, and enters a cavity section through a feeding hole;
(2) the chlorination liquid entering the cavity section falls into the tube pass of the heater under the action of gravity, is heated by steam in the tube pass of the heater, and enters the tower kettle after the secondary heating is finished;
(3) steam in the tube pass of the heater flows out through a steam water outlet, then enters a steam jacket of the tower kettle through a steam water inlet of the steam jacket of the tower kettle to heat the tower kettle, and the chlorination liquid entering the tower kettle is heated for the third time in the tower kettle;
(4) the high-temperature chlorination liquid in the tower kettle is conveyed to a circulating inlet through a circulating pump to enter a cavity section, and falls into a tube pass of a heater under the action of gravity to realize circulating heating; the other part is extracted through an extraction outlet and is conveyed to a downstream device through an extraction pump;
(5) after the chlorinated liquid is heated in the continuous heating tower, trichloroethane is gasified and rises to enter the cavity section, then the chlorinated liquid continuously rises to enter a condensing tube shell pass, the chlorinated liquid is condensed and liquefied by low-temperature chlorinated liquid in the condensing tube shell pass, then the chlorinated liquid falls into the tower again under the action of gravity, a small part of uncondensed trichloroethane gas phase enters a condenser for condensation and liquefaction, the liquefied gas phase is discharged from a liquid phase outlet and flows into the continuous heating tower through a liquid phase inlet, and the uncondensed gas phase enters a tail gas treatment pipeline through a gas phase outlet.
8. The method of claim 7, wherein the internal continuous temperature raising for sucralose chlorination is as follows: the temperature of the low-temperature chlorinated fluid conveyed to the shell pass inlet of the condensation tube array in the step (1) is 5 ℃, the temperature of the chlorinated fluid flowing out of the shell pass outlet of the condensation tube array after the first heating is finished is 79-82 ℃, the temperature of the high-temperature chlorinated fluid conveyed to the circulation inlet through the circulation pump in the step (4) is 116-.
9. The method of claim 7, wherein the internal continuous temperature raising for sucralose chlorination is as follows: the flow of the extraction pump plus the flow of the gas phase outlet of the condenser is balanced with the flow of the feeding pump.
10. The method of claim 7, wherein the internal continuous temperature raising for sucralose chlorination is as follows: the liquid level of the materials in the cavity section is near the middle position between the upper tube plate of the heater and the circulating inlet.
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| CN202110990058.5A CN113694862A (en) | 2021-08-26 | 2021-08-26 | Built-in continuous temperature rising device and method for sucralose chlorination |
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| CN202110990058.5A CN113694862A (en) | 2021-08-26 | 2021-08-26 | Built-in continuous temperature rising device and method for sucralose chlorination |
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