CN111423473A - Production and purification method of glucosamine sodium sulfate particles - Google Patents
Production and purification method of glucosamine sodium sulfate particles Download PDFInfo
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- CN111423473A CN111423473A CN202010383497.5A CN202010383497A CN111423473A CN 111423473 A CN111423473 A CN 111423473A CN 202010383497 A CN202010383497 A CN 202010383497A CN 111423473 A CN111423473 A CN 111423473A
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- 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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- 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- C07H5/00—Compounds containing saccharide radicals in which the hetero bonds to oxygen have been replaced by the same number of hetero bonds to halogen, nitrogen, sulfur, selenium, or tellurium
- C07H5/04—Compounds containing saccharide radicals in which the hetero bonds to oxygen have been replaced by the same number of hetero bonds to halogen, nitrogen, sulfur, selenium, or tellurium to nitrogen
- C07H5/06—Aminosugars
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Abstract
The invention discloses a production and purification method of glucosamine sodium sulfate particles, and a purification device is used in the production and purification process, the purification device comprises a working bin, a partition plate is fixed in the working bin, two opposite support plates are arranged in the working bin, vertical plates are vertically fixed on the side walls of the support plates, a blanking plate is fixed between the two vertical plates, a through hole is formed in the center of the blanking plate, a washing bin is formed by the upper surface of the partition plate and the inside of the working bin, a separation tube is arranged below the blanking plate, a vacuum drying bin is fixed at the bottom end of the separation tube, a liquid collection bin is fixed in the working bin, and the liquid collection bin is positioned below the vacuum drying bin; the device integrates a plurality of devices, reduces the times of raw material transfer during the process of extracting the glucosamine sodium sulfate crude product, prevents the secondary pollution of the glucosamine sodium sulfate crude product, and further influences the purification effect.
Description
Technical Field
The invention belongs to the technical field of biochemistry, and particularly relates to a production and purification method of glucosamine sodium sulfate particles.
Background
Glucosamine sulfate is an important derivative of glucosamine, is an important raw material for synthesizing macromolecules such as amino viscous polysaccharide, glycoprotein, glycolipid and the like in a human body, participates in the formation of organs such as tendons, ligaments, skin, bones, heart valves and the like, and glucosamine sodium sulfate can obviously relieve pain caused by arthritis and rheumatism and improve walking conditions, can prevent, treat and repair damage of connective tissues, has a certain curative effect on the bone and the joint inflammation, and is also beneficial to the healing of acute and chronic wounds.
Contain impurity in the product and need purify after glucosamine sodium sulfate preparation, traditional glucosamine sodium sulfate granule purification method, use multiple chemical reagent to wash glucosamine sodium sulfate crude, and washing work is gone on under non-sealing state, some chemical reagent volatilize, and then cause the influence and easily cause the pollution to the environment to operator's health, in purification process, need carry out many times the transfer with glucosamine sodium sulfate crude, secondary pollution easily appears in the transfer process, and then make the purification effect relatively poor.
Disclosure of Invention
The invention aims to provide a production and purification method of glucosamine sodium sulfate particles.
The technical problems to be solved by the invention are as follows:
traditional glucosamine sodium sulfate particle purification method uses multiple chemical reagent to wash glucosamine sodium sulfate crude product, and the work of washing is gone on under the unsealed state, and partial chemical reagent appears volatilizing, and then causes the influence and easily cause the pollution to the environment to operator's healthy, in the purification process, need carry out multiple transfer with glucosamine sodium sulfate crude product, secondary pollution easily appears in the transfer process, and then makes the purification effect relatively poor.
The purpose of the invention can be realized by the following technical scheme:
a production and purification method of glucosamine sodium sulfate particles comprises the following specific steps:
step S1: adding absolute ethyl alcohol and sodium into a stirring kettle, reacting for 20-30min, adding glucosamine hydrochloride, reacting for 5-10min under the condition that the rotating speed is 600-3500 r/min to obtain reaction liquid, adding the reaction liquid into a centrifugal machine, centrifuging for 10-15min under the condition that the rotating speed is 3000-3500r/min, and removing precipitates to obtain supernatant;
step S2: adding the supernatant obtained in the step S1 into a stirring kettle, adding fuming sulfuric acid, stirring for 1-1.5h at the temperature of-5-0 ℃, adding acetone, stirring for 30-40min, performing suction filtration, and removing filtrate to obtain a glucosamine sodium sulfate crude product;
step S3: and (4) adding the crude product of the glucosamine sodium sulfate prepared in the step (S2) into a purifying device to prepare glucosamine sodium sulfate particles.
Further, the using amount ratio of the absolute ethyl alcohol and the sodium in the step S1 is 50m L: 1g, the using amount molar ratio of the glucosamine hydrochloride to the sodium is 1: 1, the using amount volume ratio of the supernatant and the oleum in the step S2 is 40: 1, and the oleum is oleum with the sulfur trioxide content of 20-25%.
Further, the S3 purifying device comprises a working chamber, a feed inlet is arranged at the bottom end of the working chamber, a discharge outlet is arranged at the center of the bottom end of the working chamber, a partition board is fixed inside the working chamber, a square hole is formed at the center of the partition board, two sealing plates which are oppositely arranged are arranged inside the square hole, two support plates which are oppositely arranged are arranged inside the working chamber, the support plates are positioned below the partition board, vertical plates are vertically fixed on the side walls of the support plates, a blanking plate is fixed between the two vertical plates, a through hole is formed at the center of the blanking plate, a washing chamber is formed between the upper surface of the partition board and the inside of the working chamber, the feed inlet is communicated with the inside of the washing chamber, a motor is fixed at the top end of the outside of the washing chamber, a rotating shaft is fixed at the output end of the motor and positioned inside the washing chamber, the rotating shaft is rotatably connected with the top wall of the washing, the below of flitch is equipped with the separator tube down, the top and the through-hole fixed connection of separator tube, the both sides of separator tube are equipped with the downcomer, the bottom mounting of separator tube has the vacuum drying storehouse, separator tube and the inside intercommunication in vacuum drying storehouse, the bottom in vacuum drying storehouse is equipped with the feed opening, the top fixed connection of feed opening and discharge gate, the outside lateral wall in vacuum drying storehouse is equipped with the heater, the inside in working bin is fixed with a collection liquid storehouse, it is located the below in vacuum drying storehouse to collect the liquid storehouse, the bottom of downcomer and the last fixed surface in collection liquid storehouse are connected, the downcomer communicates with the collection liquid storehouse is inside, the vacuum drying storehouse passes a collection liquid storehouse.
Further, the below of working bin be equipped with the base, be fixed with four evenly distributed's fixed column between base and the working bin, the inside of feed inlet, discharge gate, feed opening, liquid outlet all is equipped with the valve, the inside of liquid outlet and washing bin junction is fixed with first filter screen.
Further, one side both ends of closing plate be fixed with the connecting axle, the connecting axle rotates with the lateral wall in square hole to be connected, the closing plate cooperatees with the square hole, the lower fixed surface of closing plate has the connecting block, is fixed with electric telescopic handle in the backup pad, electric telescopic handle's top is connected with the connecting block hinge.
Further, the inside second filter screen that is equipped with of junction of downcomer and separator tube, the inside of separator tube is fixed with the separation valve, the bottom of the junction of downcomer and separator tube is located same height with the upper surface of separation valve.
The invention has the beneficial effects that: adding a glucosamine sodium sulfate crude product into a washing bin from a feeding hole, adding acetone into the washing bin from the feeding hole, starting a motor, driving a rotating shaft to rotate by the motor, driving blades to stir by the rotating shaft, so that the glucosamine sodium sulfate crude product is washed, after washing is finished, opening a valve inside a liquid outlet to collect the acetone, closing a valve inside the liquid outlet, adding an ether feeding hole into the washing bin, continuing washing, after washing is finished, contracting an electric telescopic rod, rotating a sealing plate downwards by taking a connecting shaft as an axis, feeding the glucosamine sodium sulfate crude product and ether into a separation tube, feeding the ether into a liquid collection bin from a liquid discharge tube to be collected, accumulating the glucosamine sodium sulfate crude product on a separation valve, opening the separation valve, feeding the glucosamine sodium sulfate crude product into a vacuum drying bin, starting a heater, and carrying out vacuum drying on the glucosamine sodium sulfate crude product, accomplish vacuum drying after, open the inside valve of feed opening, collect by the discharge gate, obtain glucosamine sodium sulfate granule, setting through the separator tube, fine with ether and the crude separation of glucosamine sodium sulfate, and then reduced vacuum drying's the degree of difficulty, collect ether by collecting the liquid storehouse, ether to environmental pollution has been reduced, ether has been prevented to cause the injury to the human body, with a plurality of equipment integrations, the number of times that the crude extraction of glucosamine sodium sulfate shifts the in-process raw materials has been reduced, secondary pollution has been prevented to the crude glucosamine sodium sulfate, and then the purification effect has been influenced.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art that other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a schematic structural diagram of a purification apparatus in a method for producing and purifying glucosamine sodium sulfate particles according to the present invention.
FIG. 2 is a schematic view of a portion of the structure of FIG. 1;
FIG. 3 is a top view of a partition plate in the purification apparatus of the present invention;
FIG. 4 is a schematic view showing the structure of a sealing plate in the purification apparatus of the present invention;
FIG. 5 is a top view of a blanking plate in the purification apparatus of the present invention;
FIG. 6 is a schematic view showing the structure of a separation tube in the purification apparatus of the present invention.
In the figure: 1. a working bin; 11. a feed inlet; 12. a discharge port; 13. a base; 14. fixing a column; 2. a partition plate; 21. a square hole; 22. a sealing plate; 221. a connecting shaft; 222. connecting blocks; 23. a support plate; 231. an electric telescopic rod; 232. a vertical plate; 24. a blanking plate; 241. a through hole; 3. a washing bin; 31. a motor; 32. a rotating shaft; 33. a blade; 34. a liquid outlet; 341. a first filter screen; 4. a separation tube; 41. a liquid discharging pipe; 411. a second filter screen; 42. a separation valve; 5. a vacuum drying bin; 51. a feeding port; 52. a heater; 6. and a liquid collecting bin.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings 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 of the 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.
Example 1
A production and purification method of glucosamine sodium sulfate particles comprises the following specific steps:
step S1: adding absolute ethyl alcohol and sodium into a stirring kettle, reacting for 20min, adding glucosamine hydrochloride, reacting for 5min at the rotation speed of 700r/min to obtain a reaction solution, adding the reaction solution into a centrifugal machine, centrifuging for 10min at the rotation speed of 3500r/min, and removing precipitates to obtain a supernatant;
step S2: adding the supernatant prepared in the step S1 into a stirring kettle, adding fuming sulfuric acid, stirring for 1h at the rotation speed of 1000r/min and the temperature of-5 ℃, adding acetone, stirring for 30min, performing suction filtration, and removing filtrate to obtain a glucosamine sodium sulfate crude product;
step S3: and (4) adding the crude product of the glucosamine sodium sulfate prepared in the step (S2) into a purifying device to prepare glucosamine sodium sulfate particles.
Example 2
A production and purification method of glucosamine sodium sulfate particles comprises the following specific steps:
step S1: adding absolute ethyl alcohol and sodium into a stirring kettle, reacting for 30min, adding glucosamine hydrochloride, reacting for 10min at the rotation speed of 600r/min to obtain a reaction solution, adding the reaction solution into a centrifugal machine, centrifuging for 15min at the rotation speed of 3000r/min, and removing precipitates to obtain a supernatant;
step S2: adding the supernatant prepared in the step S1 into a stirring kettle, adding fuming sulfuric acid, stirring for 1.5h at the rotation speed of 800r/min and the temperature of 0 ℃, adding acetone, stirring for 40min, performing suction filtration, and removing filtrate to obtain a glucosamine sodium sulfate crude product;
step S3: and (4) adding the crude product of the glucosamine sodium sulfate prepared in the step (S2) into a purifying device to prepare glucosamine sodium sulfate particles.
Referring to fig. 1-6, the purifying device according to the above embodiment includes a working chamber 1, a feeding hole 11 is disposed at the bottom end of the working chamber 1, a discharging hole 12 is disposed at the center of the bottom end of the working chamber 1, a partition plate 2 is fixed inside the working chamber 1, a square hole 21 is formed at the center of the partition plate 2, two sealing plates 22 are disposed inside the square hole 21, two support plates 23 are disposed inside the working chamber 1, the support plates 23 are disposed below the partition plate 2, vertical plates 232 are vertically fixed on the side walls of the support plates 23, a blanking plate 24 is fixed between the two vertical plates 232, a through hole 241 is formed at the center of the blanking plate 24, a washing chamber 3 is formed between the upper surface of the partition plate 2 and the inside of the working chamber 1, the feeding hole 11 is communicated with the inside of the washing chamber 3, a motor 31 is fixed at the top end of the outside of the washing chamber 3, a rotating shaft 32 is fixed at the output end of the motor, pivot 32 rotates with the roof of washing storehouse 3 to be connected, be fixed with a plurality of evenly distributed's blade 33 in the pivot 32, one side bottom of washing storehouse 3 is equipped with liquid outlet 34, the below of flitch 24 is equipped with separator tube 4 down, the top and the through-hole 241 fixed connection of separator tube 4, the both sides of separator tube 4 are equipped with down liquid pipe 41, the bottom mounting of separator tube 4 has vacuum drying storehouse 5, separator tube 4 and the inside intercommunication in vacuum drying storehouse 5, the bottom in vacuum drying storehouse 5 is equipped with feed opening 51, the top fixed connection of feed opening 51 and discharge gate 12, the outside lateral wall in vacuum drying storehouse 5 is equipped with heater 52, the inside of working bin 1 is fixed with album liquid storehouse 6, album liquid storehouse 6 is located the below in vacuum drying storehouse 5, the bottom of down liquid pipe 41 and the upper surface fixed connection in album liquid storehouse 6, lower liquid pipe 41 and the inside intercommunication in album liquid storehouse 6, vacuum drying storehouse 5 passes album liquid storehouse 6.
The lower side of working bin 1 be equipped with base 13, be fixed with four evenly distributed's fixed column 14 between base 13 and the working bin 1, the inside of feed inlet 11, discharge gate 12, feed opening 51, liquid outlet 34 all is equipped with the valve, the inside first filter screen 341 that is fixed with of liquid outlet 34 and washing bin 3 junction.
The connecting shaft 221 is fixed at two ends of one side of the sealing plate 22, the connecting shaft 221 is rotatably connected with the side wall of the square hole 21, the sealing plate 22 is matched with the square hole 21, the connecting block 222 is fixed on the lower surface of the sealing plate 22, the electric telescopic rod 231 is fixed on the supporting plate 23, and the top end of the electric telescopic rod 231 is hinged with the connecting block 222.
The inside second filter screen 411 that is equipped with of junction of downcomer 41 and separator tube 4, the inside of separator tube 4 is fixed with separation valve 42, and the bottom of the junction of downcomer 41 and separator tube 4 is located the same height with the upper surface of separation valve 42.
The purification device comprises the following working steps and working principle:
adding the glucosamine sodium sulfate crude product prepared in the step S2 into a washing bin 3 through a feeding hole 11, adding acetone into the washing bin 3 through the feeding hole 11, starting a motor 31, driving a rotating shaft 32 to rotate by the motor 31, driving blades 33 to stir by the rotating shaft 32, so that the glucosamine sodium sulfate crude product is washed, after washing is completed, starting an internal valve of a liquid outlet 34 to collect the acetone, closing an internal valve of the liquid outlet 34, adding an ether feeding hole 11 into the washing bin 3, continuing washing, after washing is completed, contracting an electric telescopic rod 231, rotating a sealing plate 22 downwards by taking a connecting shaft 221 as an axis, feeding the glucosamine sodium sulfate crude product and ether into a separation tube 4, feeding the ether into a liquid collection bin 6 through a liquid discharge tube 41 to be collected, accumulating the glucosamine sodium sulfate crude product on a separation valve 42, starting the separation valve 42, feeding the glucosamine sodium sulfate crude product into a vacuum drying bin 5, open heater 52, carry out vacuum drying to glucosamine sodium sulfate crude, accomplish vacuum drying's back, open the inside valve of feed opening 51, collect by discharge gate 12, obtain glucosamine sodium sulfate granule, through the setting of separator tube 4, fine with ether and the crude separation of glucosamine sodium sulfate, and then reduced vacuum drying's the degree of difficulty, collect ether by collecting liquid storehouse 6, reduced ether to environmental pollution, prevented that ether from causing the injury to the human body.
The foregoing is merely exemplary and illustrative of the principles of the present invention and various modifications, additions and substitutions of the specific embodiments described herein may be made by those skilled in the art without departing from the principles of the present invention or exceeding the scope of the claims set forth herein.
Claims (6)
1. A production and purification method of glucosamine sodium sulfate particles is characterized in that: the method comprises the following specific steps:
step S1: adding absolute ethyl alcohol and sodium into a stirring kettle, reacting for 20-30min, adding glucosamine hydrochloride, reacting for 5-10min under the condition that the rotating speed is 600-3500 r/min to obtain reaction liquid, adding the reaction liquid into a centrifugal machine, centrifuging for 10-15min under the condition that the rotating speed is 3000-3500r/min, and removing precipitates to obtain supernatant;
step S2: adding the supernatant obtained in the step S1 into a stirring kettle, adding fuming sulfuric acid, stirring for 1-1.5h at the temperature of-5-0 ℃, adding acetone, stirring for 30-40min, performing suction filtration, and removing filtrate to obtain a glucosamine sodium sulfate crude product;
step S3: and (4) adding the crude product of the glucosamine sodium sulfate prepared in the step (S2) into a purifying device to prepare glucosamine sodium sulfate particles.
2. The method for producing and purifying glucosamine sulfate sodium salt particles as claimed in claim 1, wherein the ratio of the absolute ethanol to the sodium in step S1 is 50m L: 1g, the molar ratio of the glucosamine hydrochloride to the sodium in step S is 1: 1, the volume ratio of the supernatant to the oleum in step S2 is 40: 1, and the oleum is oleum with sulfur trioxide content of 20-25%.
3. The process for the production and purification of glucosamine sulfate sodium salt particles as set forth in claim 1, wherein: the S3 purification device comprises a working bin (1), wherein a feed inlet (11) is formed in the bottom end of the working bin (1), a discharge outlet (12) is formed in the center of the bottom end of the working bin (1), a partition plate (2) is fixed inside the working bin (1), a square hole (21) is formed in the center of the partition plate (2), two sealing plates (22) which are oppositely arranged are arranged inside the square hole (21), two support plates (23) which are oppositely arranged are arranged inside the working bin (1), the support plates (23) are positioned below the partition plate (2), vertical plates (232) are vertically fixed on the side walls of the support plates (23), a blanking plate (24) is fixed between the two vertical plates (232), a through hole (241) is formed in the center of the blanking plate (24), a washing bin (3) is formed by the upper surface of the partition plate (2) and the inside of the working bin (1), and the feed inlet (11) is communicated with the inside of the washing bin, a motor (31) is fixed at the top end of the outside of the washing bin (3), a rotating shaft (32) is fixed at the output end of the motor (31), the rotating shaft (32) is positioned inside the washing bin (3), the rotating shaft (32) is rotatably connected with the top wall of the washing bin (3), a plurality of uniformly distributed blades (33) are fixed on the rotating shaft (32), a liquid outlet (34) is arranged at the bottom end of one side of the washing bin (3), a separating tube (4) is arranged below the blanking plate (24), the top end of the separating tube (4) is fixedly connected with the through hole (241), liquid drainage tubes (41) are arranged at two sides of the separating tube (4), a vacuum drying bin (5) is fixed at the bottom end of the separating tube (4), the separating tube (4) is communicated with the inside of the vacuum drying bin (5), a blanking port (51) is arranged at the bottom end of the vacuum drying bin (5), the blanking port (51) is fixedly connected with the top end of the discharge port (12), the inside of working bin (1) is fixed with album liquid storehouse (6), and album liquid storehouse (6) are located the below of vacuum drying storehouse (5), and the bottom of fluid dropping pipe (41) is connected with the upper surface fixed of album liquid storehouse (6), and fluid dropping pipe (41) and album inside intercommunication in liquid storehouse (6), and collection liquid storehouse (6) are passed in vacuum drying storehouse (5).
4. The method for producing and purifying glucosamine sulfate sodium salt particles according to claim 3, wherein the steps of: the washing machine is characterized in that a base (13) is arranged below the working bin (1), four fixing columns (14) which are uniformly distributed are fixed between the base (13) and the working bin (1), valves are arranged inside the feed inlet (11), the discharge outlet (12), the feed outlet (51) and the liquid outlet (34), and a first filter screen (341) is fixed inside the joint of the liquid outlet (34) and the washing bin (3).
5. The method for producing and purifying glucosamine sulfate sodium salt particles according to claim 3, wherein the steps of: the sealing plate is characterized in that connecting shafts (221) are fixed at two ends of one side of each sealing plate (22), the connecting shafts (221) are rotatably connected with the side walls of the square holes (21), the sealing plates (22) are matched with the square holes (21), connecting blocks (222) are fixed to the lower surfaces of the sealing plates (22), electric telescopic rods (231) are fixed to the supporting plates (23), and the top ends of the electric telescopic rods (231) are hinged to the connecting blocks (222).
6. The method for producing and purifying glucosamine sulfate sodium salt particles according to claim 3, wherein the steps of: the inside second filter screen (411) that is equipped with of junction of downcomer (41) and separator tube (4), the inside of separator tube (4) is fixed with separating valve (42), the bottom of the junction of downcomer (41) and separator tube (4) is located the same height with the upper surface of separating valve (42).
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| Application Number | Priority Date | Filing Date | Title |
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| CN202010383497.5A CN111423473A (en) | 2020-05-08 | 2020-05-08 | Production and purification method of glucosamine sodium sulfate particles |
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| CN202010383497.5A CN111423473A (en) | 2020-05-08 | 2020-05-08 | Production and purification method of glucosamine sodium sulfate particles |
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Application publication date: 20200717 |
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