CN110981922A - Preparation method of sucrose octasulfonate potassium - Google Patents
Preparation method of sucrose octasulfonate potassium Download PDFInfo
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- CN110981922A CN110981922A CN201911302882.6A CN201911302882A CN110981922A CN 110981922 A CN110981922 A CN 110981922A CN 201911302882 A CN201911302882 A CN 201911302882A CN 110981922 A CN110981922 A CN 110981922A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H11/00—Compounds containing saccharide radicals esterified by inorganic acids; Metal salts thereof
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D9/00—Crystallisation
- B01D9/0063—Control or regulation
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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
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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
- C07H1/06—Separation; Purification
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D9/00—Crystallisation
- B01D2009/0086—Processes or apparatus therefor
Abstract
The invention discloses a preparation method of sucrose octasulfonate potassium, which takes sucrose and chlorosulfonic acid as raw materials and pyridine as a solvent to react under certain conditions to generate the sucrose octasulfonate potassium and discloses a recrystallization device.
Description
Technical Field
The invention relates to the technical field of organic compound synthesis, in particular to a preparation method of sucrose octasulfonate potassium.
Background
The sucrose octasulfonate potassium belongs to a potassium salt compound of sucrose ester, and the sucrose ester is a non-ionic surfactant with excellent performance, is harmless to human bodies, does not irritate skins and mucous membranes, is nontoxic and is easy to biodegrade into substances absorbable by human bodies; meanwhile, the emulsion has good functions of emulsification, dispersion, decontamination, foaming, viscosity adjustment, antibiosis, aging resistance, crystallization prevention and the like, so the emulsion is widely applied to the fields of food, pharmacy, sugar manufacturing, daily chemicals and the like.
The prior preparation method of sucrose octasulfonate potassium is less, and Chinese invention CN201810290956.8 discloses a method for preparing sucrose octasulfonate potassium by using sucrose as a raw material, reacting the sucrose octasulfonate potassium with triethylamine-sulfur trioxide compound and adjusting pH with potassium hydroxide.
The sucrose octasulfonate potassium is an organic salt compound, a method of repeated recrystallization is usually adopted for purification, the conventional recrystallization device needs to discharge a recrystallized solid-liquid mixture from a discharge hole, filter the solid and add the solid into the recrystallization device, the process is complicated, and the labor amount of an operator is greatly increased.
Disclosure of Invention
The invention aims to provide a preparation method of sucrose octasulfonate potassium, which overcomes the defect that sulfur trioxide is used as a raw material by changing an esterification raw material from a triethylamine-sulfur trioxide system into a pyridine-chlorosulfonic acid system, avoids the pollution of sulfur trioxide gas generated in the reaction process to the environment, reduces the requirements of reaction equipment on corrosion resistance and air tightness and the requirements of raw material transportation, and reduces the production cost.
In order to achieve the purpose, the invention provides the following technical scheme:
a preparation method of sucrose octasulfonate potassium comprises the following steps:
s1, dissolving sucrose in pyridine, cooling the reaction liquid to 0-10 ℃, dropwise adding excessive chlorosulfonic acid while stirring, and reacting for 2-6h at 5-30 ℃ to obtain a sucrose octasulfonate solution;
s2, adding 1-5mol/L potassium hydroxide aqueous solution into the sucrose octasulfonate solution obtained in S1, adjusting the pH to 8-9, cooling the reaction solution to room temperature, and filtering to obtain a sucrose octasulfonate potassium filter cake;
s3, dissolving the sucrose octasulfonate potassium filter cake in deionized water, adding the solution into a recrystallization device for recrystallization for 2-3 times, removing impurities, and drying the obtained sucrose octasulfonate potassium by using a vacuum drying oven to obtain a sucrose octasulfonate potassium pure product, wherein the reaction process is as follows:
compare sulfur trioxide, chlorosulfonic acid has higher reactivity, can reduce the required temperature of reaction, it is more mild to make reaction conditions, and sulfur trioxide is as esterification reaction's raw materials, need the heating to go on, solvent and sulfur trioxide that the reaction heating easily arouses volatilize, cause the pollution to the environment, and sulfur trioxide's heating reaction needs reaction unit to possess good corrosion resisting property and sealing performance, has increased manufacturing cost in the intangible.
As a further embodiment of the present invention, the molar ratio of sucrose to chlorosulfonic acid is 1: 8-9, and the amount of pyridine used is 5-10L per mole of sucrose.
As a further scheme of the invention, the recrystallization device comprises a kettle body and a kettle cover, wherein the kettle cover is detachably connected above the kettle body;
the bottom end of the kettle body is provided with a discharge valve, the outer side wall of the kettle body is fixedly connected with a jacket, the upper end and the lower end of the outer side wall of the jacket are respectively provided with a water outlet and a water inlet, and the kettle body is conveniently heated or cooled by arranging the jacket, so that the recrystallization device can meet the temperature change required in the recrystallization process;
the kettle cover top fixedly connected with rotates the motor, rotates the drive shaft fixedly connected with dwang of motor, and dwang one end extends to the internal portion lower extreme of cauldron to fixedly connected with stirring rake, fixedly connected with bracing piece on the dwang, the tip fixedly connected with scraper blade of bracing piece, scraper blade are apart from cauldron internal side wall-mm, through setting up the scraper blade, make the crystallization on cauldron internal wall can in time be scraped down, feed inlet and steam pipe have been seted up to kettle cover top face, steam pipe and condenser intercommunication, and condenser lower extreme intercommunication has the liquid storage pot, through setting up condenser and liquid storage pot, can retrieve the solvent to the liquid storage pot in when concentrating solution, realizes the cyclic utilization of solvent.
As a further scheme of the invention, the outer side wall of the upper end of the kettle body and the outer side wall of the lower end of the kettle cover are both fixedly connected with pins, the pins are fixedly connected through bolts, the kettle body and the kettle cover can be detachably connected through the pins, and the device is convenient to disassemble, clean or maintain.
As a further scheme of the invention, the discharge valve comprises a discharge pipe, a first sealing cover and a second sealing cover, through holes are correspondingly arranged on the first sealing cover and the second sealing cover, the first sealing cover is positioned above the discharge pipe, the second sealing cover is rotatably connected in a groove arranged at the bottom of the first sealing cover, the second sealing cover is rotatably connected in the first sealing cover, the through holes are corresponding through the second sealing cover, only liquid is discharged from the discharge valve, a telescopic pipe and a threaded sleeve are fixedly connected to the bottom end surface of the second sealing cover, the threaded sleeve is positioned in the telescopic pipe, a first rotating valve is fixedly connected to the surface of the telescopic pipe, the first rotating valve is rotatably connected to the lower end of the discharge pipe, a second rotating valve is rotatably connected to the lower end of the first rotating valve, a threaded rod is fixedly connected to the top end surface of the second rotating valve, the threaded rod is threadedly connected in the threaded, make first sealed lid can shift up, make the bleeder valve can open completely, through setting up the bleeder valve, can filter the recrystallization mother liquor in the recrystallization device, will appear the crystal and take out the reentering from the recrystallization device repeatedly when having avoided repeated crystallization operation, simplified the operation process of recrystallization, alleviateed operator's the amount of labour.
As a further scheme of the invention, the recrystallization operation steps are as follows:
firstly, adding deionized water into a recrystallization device, introducing hot steam into a jacket, heating the deionized water to 50-70 ℃, adding a sucrose octasulfonate potassium solid from a feed inlet under stirring at a rotating speed of 300r/min at 200-;
evaporating the deionized water to saturate the potassium sucrose octasulfonate in the boiling deionized water, stopping heating, and introducing cold water into the jacket to cool the solution in the recrystallization device to 5-15 ℃ so as to separate the potassium sucrose octasulfonate from the deionized water;
rotating the first rotating valve to drive the second sealing cover to rotate, enabling the recrystallization mother liquor to flow out of the discharge valve, separating the recrystallization mother liquor from the sucrose octasulfonate potassium crystals, closing the first rotating valve, and adding new deionized water from the feed inlet;
and fourthly, repeating the processes of the second step and the third step for 1-2 times, then rotating the second rotating valve to enable the mixture of the crystal and the crystal mother liquor to flow out from the discharge valve, filtering the flowing-out mixture to obtain a filter cake, namely recrystallized potassium sucrose octasulfonate crystals, collecting the recrystallized mother liquor separately after flowing out, combining the mother liquors of repeated recrystallization operation, and then recycling the potassium sucrose octasulfonate.
Compared with the prior art, the invention has the beneficial effects that:
the invention provides a preparation method of sucrose octasulfonate potassium, which has mild condition, simple and convenient operation, high yield and high purity and is suitable for industrial production, chlorosulfonic acid is used as a raw material of esterification reaction, compared with sulfur trioxide, chlorosulfonic acid has higher reaction activity, the temperature required by the reaction can be reduced, the reaction condition is milder, the esterification reaction of sulfur trioxide as the raw material needs to be heated, the solvent and sulfur trioxide which are easily caused by reaction heating are volatilized, the environment is polluted, the reaction device is required to have good corrosion resistance and sealing performance by the heating reaction of sulfur trioxide, and the production cost is increased invisibly;
the recrystallization device provided by the invention can be used for conveniently carrying out recrystallization operation, the discharge valve is arranged, the first sealing cover can move upwards through the matching of the threaded sleeve and the threaded rod of the discharge valve, so that the discharge valve can be completely opened, the second sealing cover is rotatably connected in the first sealing cover, the first sealing cover and the second sealing cover are correspondingly provided with through holes, the second sealing cover is rotated to ensure that the through holes correspond, so that the discharge valve only discharges liquid, the recrystallization mother liquor can be filtered in the recrystallization device, the phenomenon that precipitated crystals are repeatedly taken out of the recrystallization device and then put in the recrystallization device during repeated crystallization operation is avoided, the operation process of recrystallization is simplified, and the labor amount of an operator is reduced.
Drawings
FIG. 1 is a schematic view of the overall structure of a recrystallization apparatus;
FIG. 2 is a schematic view of a discharge valve of a recrystallization apparatus;
FIG. 3 is a schematic view of a first sealing cap of the recrystallization apparatus;
FIG. 4 is a schematic view of a second sealing cap of the recrystallization apparatus;
in the figure: 1. a kettle body; 2. a kettle cover; 3. a discharge valve; 4. a jacket; 5. a water outlet; 6. a water inlet; 7. rotating the motor; 8. rotating the rod; 9. a stirring paddle; 10. a support bar; 11. a squeegee; 12. a feed inlet; 13. a steam pipe; 14. a condenser; 15. a liquid storage tank; 16. a pin; 17. a bolt; 18. a discharge pipe; 19. a first sealing cover; 20. a second sealing cover; 21. a telescopic pipe; 22. a threaded bushing; 23. a first rotary valve; 24. a second rotary valve; 25. a threaded rod; 26. and a through hole.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to fig. 1 to 4 in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
A preparation method of sucrose octasulfonate potassium comprises the following steps:
s1, dissolving 1kg (2.92mol) of sucrose in 15L of pyridine, cooling the reaction liquid to 5 ℃, dropwise adding 2.78kg (24mol) of chlorosulfonic acid while stirring, and reacting for 2h at 15-25 ℃ to obtain a sucrose octasulfonate solution;
s2, adding 2mol/L potassium hydroxide aqueous solution into the sucrose octasulfonate solution obtained in S1, adjusting the pH to 8-9, cooling the reaction solution to 25 ℃, and filtering to obtain a sucrose octasulfonate potassium filter cake;
s3, adding the sucrose octasulfonate potassium filter cake into a recrystallization device for recrystallization for 2-3 times, removing impurities, and drying the obtained sucrose octasulfonate potassium by using a vacuum drying oven to obtain 3.27kg of white solid powder with the yield of 89%, wherein the reaction process is as follows:
compare sulfur trioxide, chlorosulfonic acid has higher reactivity, can reduce the required temperature of reaction, it is more mild to make reaction conditions, and sulfur trioxide is as esterification reaction's raw materials, need the heating to go on, solvent and sulfur trioxide that the reaction heating easily arouses volatilize, cause the pollution to the environment, and sulfur trioxide's heating reaction needs reaction unit to possess good corrosion resisting property and sealing performance, has increased manufacturing cost in the intangible.
The recrystallization device comprises a kettle body 1 and a kettle cover 2, wherein the kettle cover 2 is detachably connected above the kettle body 1;
the bottom end of the kettle body 1 is provided with a discharge valve 3, the outer side wall of the kettle body 1 is fixedly connected with a jacket 4, the upper end and the lower end of the outer side wall of the jacket 4 are respectively provided with a water outlet 5 and a water inlet 6, and the kettle body 1 is conveniently heated or cooled by arranging the jacket 4, so that the recrystallization device can meet the temperature change required in the recrystallization process;
2 top fixedly connected with of kettle cover rotate motor 7, the drive shaft fixedly connected with dwang 8 of rotating motor 7, dwang 8 one end extends to the inside lower extreme of the cauldron body 1, and fixedly connected with stirring rake 9, fixedly connected with bracing piece 10 on the dwang 8, the tip fixedly connected with scraper blade 11 of bracing piece 10, scraper blade 11 is apart from 1 inside wall 1-3mm of the cauldron body, through setting up scraper blade 11, make the crystallization on the internal wall of cauldron 1 in time scraped, feed inlet 12 and steam pipe 13 have been seted up to 2 top faces of kettle cover, steam pipe 13 and condenser 14 intercommunication, condenser 14 lower extreme intercommunication has liquid storage pot 15, through setting up condenser 14 and liquid storage pot 15, can retrieve the solvent to liquid storage pot 15 when concentrating solution, realize the cyclic utilization of solvent.
The equal fixedly connected with pin 16 of lateral wall and the 2 lower extremes of kettle cover of the lateral wall of the 1 upper end of the cauldron body, through 17 fixed connection of bolt, can dismantle the cauldron body 1 and kettle cover 2 through pin 16 and be connected, conveniently dismantle, clear up or maintain the device.
The discharge valve 3 comprises a discharge pipe 18, a first sealing cover 19 and a second sealing cover 20, through holes 26 are correspondingly arranged on the first sealing cover 19 and the second sealing cover 20 in a penetrating manner, the first sealing cover 19 is positioned above the discharge pipe 18, the second sealing cover 20 is rotatably connected in a groove arranged at the bottom of the first sealing cover 19, the second sealing cover 20 is rotatably connected in the first sealing cover 19, the through holes 26 are corresponding to each other through the rotation of the second sealing cover 20, the discharge valve 3 only discharges liquid, a telescopic pipe 21 and a threaded sleeve 22 are fixedly connected to the bottom end face of the second sealing cover 20, the threaded sleeve 22 is positioned in the telescopic pipe 21, a first rotating valve 23 is fixedly connected to the bottom end face of the telescopic pipe 21, the first rotating valve 23 is rotatably connected to the lower end of the discharge pipe 18, a second rotating valve 24 is rotatably connected to the lower end face of the first rotating valve 23, a threaded rod 25 is fixedly connected to, through the cooperation of threaded sleeve 22 and threaded rod 25, make first sealed lid 19 can shift up, make bleeder valve 3 can open completely, through setting up bleeder valve 3, can filter the recrystallization mother liquor in the recrystallization device, will appear the crystal and take out the reentering from the recrystallization device repeatedly when having avoided the repeated crystallization operation, simplify the operation process of recrystallization, alleviateed operator's the amount of labour.
The recrystallization operation steps are as follows:
firstly, adding deionized water into a recrystallization device through a feed inlet 12, introducing hot steam into a jacket 4 through a water outlet 5 and a water inlet 6, heating the deionized water to 50 ℃, starting a rotating motor 7 to enable a rotating rod 8 to rotate at a rotating speed of 200r/min, adding a sucrose octasulfonate potassium solid from the feed inlet 12 under rotating and stirring until the added solid is not dissolved any more, and preserving the heat for 10 minutes;
secondly, raising the temperature of hot steam in the jacket 4 to heat and evaporate the deionized water, so that the potassium sucrose octasulfonate is saturated in the boiling deionized water, stopping heating, and introducing cold water into the jacket 4 to cool the solution in the recrystallization device to 5 ℃ so that the potassium sucrose octasulfonate is separated out from the deionized water;
thirdly, rotating the first rotating valve 23, driving the second sealing cover 20 to rotate by the first rotating valve 23 through the extension pipe 21, enabling the second sealing cover 20 to be overlapped with the through hole 26 on the first sealing cover 19, enabling the recrystallization mother liquor to enter the discharging pipe 18 from the through hole 26 and flow out of the discharging valve 3, closing the first rotating valve 23 after separating the recrystallization mother liquor and the sucrose octasulfonate potassium crystals, and adding new deionized water from the feeding hole 12;
and fourthly, after repeating the processes of the second step and the third step for 2 times, rotating a second rotating valve 24, driving a threaded rod 25 to rotate by the second rotating valve 24, enabling a threaded sleeve 22 to move upwards, extending an extension pipe 21, and exposing a gap between a first sealing cover 19 and a discharge pipe 18, so that a crystal and crystal mother liquor mixture flows out from a discharge valve 3, filtering the flowing-out mixture, obtaining a filter cake which is the recrystallized sucrose octasulfonate potassium crystal, collecting the recrystallized mother liquor after flowing out separately, and recovering the sucrose octasulfonate potassium after merging the mother liquors of repeated recrystallization operations.
The preferred embodiments of the invention disclosed above are intended to be illustrative only. The preferred embodiments are not intended to be exhaustive or to limit the invention to the precise forms disclosed. Obviously, many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, to thereby enable others skilled in the art to best utilize the invention. The invention is limited only by the claims and their full scope and equivalents.
Claims (6)
1. A preparation method of sucrose octasulfonate potassium is characterized by comprising the following steps: the preparation method comprises the following steps:
s1, dissolving sucrose in pyridine, cooling the sucrose pyridine solution to 0-10 ℃, dropwise adding excessive chlorosulfonic acid while stirring, and reacting for 2-6h at 5-30 ℃ to obtain a sucrose octasulfonate solution;
s2, adding 1-5mol/L potassium hydroxide aqueous solution into the sucrose octasulfonate solution obtained in S1, adjusting the pH to 8-9, cooling the reaction solution to room temperature, and filtering to obtain a sucrose octasulfonate potassium filter cake;
and S3, adding the sucrose octasulfonate potassium filter cake and deionized water into a recrystallization device, carrying out recrystallization operation for 2-3 times, removing impurities, and drying the obtained sucrose octasulfonate potassium by using a vacuum drying oven to obtain the sucrose octasulfonate potassium pure product.
2. The method for preparing the potassium sucrose octasulfonate according to claim 1, wherein the molar ratio of the sucrose to the chlorosulfonic acid is 1: 8-9, and the amount of pyridine used is 5-10L per mole of sucrose.
3. The preparation method of the potassium sucrose octasulfonate according to claim 1, wherein the recrystallization device comprises a kettle body (1) and a kettle cover (2), and the kettle cover (2) is detachably connected above the kettle body (1);
a discharge valve (3) is installed at the bottom end of the kettle body (1), a jacket (4) is fixedly connected to the outer side wall of the kettle body (1), and a water outlet (5) and a water inlet (6) are respectively arranged at the upper end and the lower end of the outer side wall of the jacket (4);
kettle cover (2) top fixedly connected with rotates motor (7), drive shaft fixedly connected with dwang (8) of rotating motor (7), dwang (8) one end extends to the inside lower extreme of the cauldron body (1), and fixedly connected with stirring rake (9), fixedly connected with bracing piece (10) are gone up in dwang (8), bracing piece (10) are located dwang (8) middle part, tip fixedly connected with scraper blade (11) of bracing piece (10), scraper blade (11) are apart from cauldron body (1) inside wall 1-3mm, feed inlet (12) and steam pipe (13) have been seted up to kettle cover (2) top face, steam pipe (13) intercommunication has condenser (14), condenser (14) lower extreme intercommunication has liquid storage pot (15).
4. The preparation method of the potassium sucrose octasulfonate according to claim 3, wherein pins (16) are fixedly connected to the outer side wall of the upper end of the kettle body (1) and the outer side wall of the lower end of the kettle cover (2), and the pins (16) are fixedly connected through bolts (17).
5. The preparation method of the potassium sucrose octasulfonate according to claim 3, wherein the discharge valve (3) comprises a discharge pipe (18), a first sealing cover (19) and a second sealing cover (20), through holes (26) are correspondingly formed in the first sealing cover (19) and the second sealing cover (20), the first sealing cover (19) is positioned above the discharge pipe (18), the second sealing cover (20) is rotatably connected in a groove formed at the bottom of the first sealing cover (19), a telescopic pipe (21) and a threaded sleeve (22) are fixedly connected to the bottom end surface of the second sealing cover (20), the threaded sleeve (22) is positioned inside the telescopic pipe (21), a first rotating valve (23) is fixedly connected to the bottom end surface of the telescopic pipe (21), the first rotating valve (23) is rotatably connected to the lower end of the discharge pipe (18), the lower end of the first rotating valve (23) is rotatably connected to a second rotating valve (24), the top end face of the second rotary valve (24) is fixedly connected with a threaded rod (25), and the threaded rod (25) is in threaded connection with the inside of the threaded sleeve (22).
6. The method for preparing potassium sucrose octasulfonate according to claim 1, wherein the recrystallization procedure comprises:
firstly, adding deionized water into a recrystallization device, introducing hot steam into a jacket (4), heating the deionized water to 50-70 ℃, adding a sucrose octasulfonate potassium solid from a feed inlet (12) under stirring at a rotating speed of 200-300r/min until the added solid is not dissolved any more, and preserving heat for 5-20 minutes;
secondly, evaporating the deionized water to saturate the sucrose potassium octasulfonate in the boiling deionized water, stopping heating, and introducing cold water into the jacket (4) to cool the saturated solution in the recrystallization device to 5-15 ℃ so as to separate out the sucrose potassium octasulfonate from the deionized water;
thirdly, rotating the first rotating valve (23) to drive the second sealing cover (20) to rotate, enabling the recrystallization mother liquor to flow out of the discharge valve (3), separating the recrystallization mother liquor from the crystallization of the sucrose octasulfonate potassium, closing the first rotating valve (23), and adding new deionized water from the feed inlet (12);
and fourthly, repeating the processes of the second step and the third step for 1-2 times, then rotating a second rotating valve (24) to enable the mixture of the crystal and the crystal mother liquor to flow out from the discharging valve (3), and filtering the flowing-out mixture to obtain a filter cake, namely the recrystallized potassium sucrose octasulfonate crystal.
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| CN201911302882.6A CN110981922A (en) | 2019-12-17 | 2019-12-17 | Preparation method of sucrose octasulfonate potassium |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114436858A (en) * | 2020-11-03 | 2022-05-06 | 江苏开元药业有限公司 | Preparation method of triethylamine salt of pharmaceutic adjuvant |
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