Method for producing vitamin B12 by using potassium ferrocyanide

Abstract

The invention provides a method for producing vitamin B12 by using potassium ferrocyanide, and belongs to the technical field of vitamin B12 production. The preparation method comprises the following steps: transferring a vitamin B12 fermentation solution into a rotary evaporator for concentration, transferring a vitamin B12 fermentation concentrated solution into a reaction container A for cooling, and adding a potassium ferrocyanide solution into a reaction container B for later use; performing ultrasonic atomization on the liquid in the reaction container A and the reaction container B, and transferring the atomized liquid in the reaction container A and the reaction container B into a reaction container C by using a negative pressure pipeline; a magnetic field is introduced into the reaction container C, and the liquid drops of the vitamin B12 concentrated solution and the liquid drops of the potassium ferrocyanide solution in the reaction container C react in an atomized state. The method for producing the vitamin B12 by using the potassium ferrocyanide has the advantages that the conversion rate of the vitamin B12 is high, an additional sterilization step is not needed, and the method is worthy of popularization.

Description

Technical Field

[0001] The present invention relates to the technical field of vitamin B12 production, and particularly relates to a method for producing vitamin B12 using yellow prussiate of potash. Background Art

[0002] Vitamin B12, also known as cobalamin, is a polycyclic compound containing trivalent cobalt. Deficiency of vitamin B12 in humans can lead to pernicious anemia, which is characterized by a large reduction in the number of red blood cells due to interference in the red blood cell maturation process. This pernicious anemia is accompanied by neurological symptoms, including: glossitis, weakness, loss of appetite, loss of taste, memory loss, and mild depression. In most cases, pernicious anemia is caused by a reduction in vitamin B12 absorption due to a lack of mucoprotein. Higher plants and animals cannot produce vitamin B12, and all vitamin B12 in nature is synthesized by microorganisms.

[0003] In the prior art, CN103103235A uses a low-toxic iron cyanide complex as a cyanidation reagent, achieving non-toxic operation during the conversion process and reducing production risks and safety management risks. However, this method still has the problem of low conversion rate, which is mainly reflected in the following aspects: (1) The contact area of the reactants is limited, and the reaction efficiency is low; (2) There is a lack of an effective catalytic mechanism, and the reaction rate is slow; (3) The energy utilization efficiency during the reaction process is not high. Summary of the Invention

[0004] Based on the deficiencies of the prior art, the present invention provides a method for producing vitamin B12 using yellow prussiate of potash, solving the problem of low conversion efficiency in the prior art.

[0005] The method for producing vitamin B12 using yellow prussiate of potash provided by the present invention includes the following steps: Step 1: Transfer the vitamin B12 fermentation broth into a rotary evaporator for concentration, transfer the concentrated vitamin B12 fermentation broth into reaction vessel A for cooling, add the yellow prussiate of potash solution into reaction vessel B, and set aside. Step 2: Ultrasonically atomize the liquids in reaction vessel A and reaction vessel B, and transfer the atomized liquids in reaction vessel A and reaction vessel B to reaction vessel C using a negative pressure pipeline. Step 3: A magnetic field is applied in reaction vessel C, and the droplets of the vitamin B12 concentrated solution and the droplets of the yellow prussiate of potash solution in reaction vessel C react in an atomized state. Step 4: Condense the atomized solution after the reaction in Step 3 through a condensation section pipeline and then enter it into collection container D. Add the flocculant polyaluminum chloride and the filter aid activated carbon, filter, and obtain the finished vitamin B12 solution.

[0006] Preferably, the vitamin B12 fermentation broth contains methylcobalamin, adenosylcobalamin, hydroxocobalamin, microorganisms, inorganic salts and water.

[0007] Preferably, in step one, the vitamin B12 fermentation broth is added to a rotary evaporator, the temperature in the rotary evaporator is controlled at 60 °C, the concentrated solution is concentrated to a concentration of 500 - 3000 μg / ml, the concentrated solution in the rotary evaporator is transferred to reaction vessel A and cooled to 25 °C for use, and a 0.05 mol / L yellow prussiate solution is added to reaction vessel B for use.

[0008] Preferably, in step one, the yellow prussiate solution is one of potassium ferrocyanide solution and sodium ferrocyanide solution.

[0009] Preferably, in step two, the vitamin B12 fermentation concentrated solution in reaction vessel A and the yellow prussiate solution in reaction vessel B are ultrasonically atomized using an ultrasonic nebulizer. The frequency of the ultrasound is 30 - 40 kHz. The ultrasound increases the surface tension of the solution, causing the solution to atomize. At the same time, the fog-like droplets generated by the atomization of the solution have a large amount of ultrasonic cavitation energy inside. The atomized liquids in reaction vessel A and reaction vessel B are transferred to reaction vessel C through a negative pressure pipeline. Among them, the pressure in the negative pressure pipeline is 20 - 30 kPa, and the mass ratio of the fog-like droplets from reaction vessel A to the fog-like droplets from reaction vessel B in reaction vessel C is controlled to be 2:3 - 5.

[0010] Preferably, in step three, the temperature in reaction vessel C is adjusted to 50 - 90 °C. The droplets of the vitamin B12 concentrated solution and the droplets of the yellow prussiate solution in reaction vessel C react in an atomized state. There is a magnetic field in reaction vessel C with an intensity of 3 - 7 T. Under the action of the magnetic field, the ferrocyanide ions in the droplets of the yellow prussiate solution are dispersed to the surface of the droplets, increasing the reaction contact area. At the same time, under the action of the magnetic field, the ions are promoted to align along the magnetic field lines, making the reaction more orderly, thereby accelerating the reaction rate.

[0011] Preferably, in step four, the atomized solution after the reaction in step three is condensed through a condensation section pipeline and then enters collection container D. The condensation temperature of the condensation section pipeline is -5 - 20 °C. Poly aluminum chloride is added as a flocculant and activated carbon is added as a filter aid, and then filtered to obtain the finished vitamin B12 solution.

[0012] Preferably, the total mass of the added flocculant and filter aid accounts for 0.5% of the mass of the solution in collection container D.

[0013] Preferably, the mass ratio of poly aluminum chloride to activated carbon is 1 - 10:10 - 1.

[0014] Through the synergistic effect of atomization reaction and magnetic field, the conversion efficiency of vitamin B12 is significantly improved, having the following technical advantages: (1) Through the ultrasonic atomization technology, the reactants are transformed into tiny droplets, greatly increasing the contact area of the reactants and improving the reaction efficiency; (2) The introduction of the magnetic field enables the ferrocyanide ions to be arranged directionally on the droplet surface, improving the orderliness and rate of the reaction; (3) The release of ultrasonic cavitation energy provides additional energy support for the reaction, further promoting the progress of the reaction; Compared with the prior art, the method of the present invention can increase the conversion efficiency of vitamin B12 by 30% - 40%, and the product purity can reach more than 98%, which is significantly better than the traditional method. Brief Description of the Drawings

[0015] Figure 1 It is a schematic process flow diagram of the present invention. Detailed Embodiments

[0016] The technical solutions of the present invention will be clearly and completely described below in conjunction with the embodiments. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all of the embodiments. All other embodiments obtained by those of ordinary skill in the art based on the embodiments of the present invention without making creative efforts belong to the scope of protection of the present invention. In addition, the technical features involved in the various embodiments of the present invention described below can be combined with each other as long as they do not conflict with each other.

[0017] The present invention provides a method for producing vitamin B12 using yellow prussiate of potash, comprising the following steps: Step 1: Transfer the vitamin B12 fermentation broth into a rotary evaporator for concentration, transfer the concentrated vitamin B12 fermentation broth into reaction vessel A for cooling, and add the yellow prussiate of potash solution into reaction vessel B for standby; Step 2: Atomize the liquids in reaction vessel A and reaction vessel B ultrasonically, and transfer the atomized liquids in reaction vessel A and reaction vessel B to reaction vessel C using a negative pressure pipeline; Step 3: A magnetic field is applied in reaction vessel C, and the droplets of the concentrated vitamin B12 solution and the droplets of the yellow prussiate of potash solution in reaction vessel C react in the atomized state; Step 4: Condense the atomized solution after the reaction in Step 3 through a condensation section pipeline and then enter it into collection vessel D, add the flocculant polyaluminum chloride and the filter aid activated carbon, and filter to obtain the finished vitamin B12 solution.

[0018] In an embodiment of the present invention, the vitamin B12 fermentation broth contains methylcobalamin, adenosylcobalamin, hydroxocobalamin, microorganisms, inorganic salts and water.

[0019] In one embodiment of the present invention, in step one, the vitamin B12 fermentation broth is added to a rotary evaporator, the temperature in the rotary evaporator is controlled at 60°C, the concentrated solution is concentrated to a concentration of 500 - 3000 μg / ml, the concentrated solution in the rotary evaporator is transferred to reaction vessel A and cooled to 25°C for standby, and a 0.05 mol / L potassium ferrocyanide solution is added to reaction vessel B for standby.

[0020] In one embodiment of the present invention, in step one, the potassium ferrocyanide solution is one of potassium ferrocyanide solution and sodium ferrocyanide solution.

[0021] In one embodiment of the present invention, in step two, the vitamin B12 fermentation concentrated solution in reaction vessel A and the potassium ferrocyanide solution in reaction vessel B are ultrasonically atomized using an ultrasonic nebulizer. The frequency of the ultrasound is 30 - 40 kHz. The ultrasound increases the surface tension of the solution and atomizes the solution. At the same time, the fog-like droplets generated by the atomization of the solution have a large amount of ultrasonic cavitation energy inside. The atomized liquids in reaction vessel A and reaction vessel B are transferred to reaction vessel C through a negative pressure pipeline. Among them, the pressure in the negative pressure pipeline is 20 - 30 kPa, and the mass ratio of the fog-like droplets from reaction vessel A to the fog-like droplets from reaction vessel B in reaction vessel C is controlled to be 2:3 - 5.

[0022] In one embodiment of the present invention, in step three, the temperature in reaction vessel C is adjusted to 50 - 90°C, and the droplets of the vitamin B12 concentrated solution and the droplets of the potassium ferrocyanide solution in reaction vessel C react in an atomized state. There is a magnetic field in reaction vessel C with an intensity of 3 - 7 T. Under the action of the magnetic field, the ferrocyanide ions in the droplets of the potassium ferrocyanide solution are dispersed to the surface of the droplets, increasing the reaction contact area. At the same time, under the action of the magnetic field, the ions are induced to align along the magnetic field lines, making the reaction more orderly, thereby accelerating the reaction rate.

[0023] In one embodiment of the present invention, in step four, the atomized solution after the reaction in step three is condensed through a condensation section pipeline and then enters collection container D. The condensation temperature of the condensation section pipeline is -5 - 20°C. Polyaluminum chloride is added as a flocculant and activated carbon is added as a filter aid, and then filtered to obtain the finished vitamin B12 solution.

[0024] In one embodiment of the present invention, the total mass of the added flocculant and filter aid accounts for 0.5% of the mass of the solution in collection container D.

[0025] In one embodiment of the present invention, the mass ratio of polyaluminum chloride to activated carbon is 1 - 10:10 - 1.

[0026] Example 1 This embodiment provides a method for producing vitamin B12 using yellow prussiate of potash. In step one, the vitamin B12 fermentation broth is added to a rotary evaporator, and the temperature in the rotary evaporator is controlled at 60 °C. The concentrated solution is concentrated to a concentration of 500 μg / ml. The concentrated solution in the rotary evaporator is transferred to reaction vessel A and cooled to 25 °C for standby. A 0.05 mol / L potassium yellow prussiate solution is added to reaction vessel B for standby.

[0027] In step two, the vitamin B12 fermentation concentrated solution in reaction vessel A and the potassium yellow prussiate solution in reaction vessel B are ultrasonically atomized using an ultrasonic nebulizer. The frequency of the ultrasound is 30 kHz. The ultrasound increases the surface tension of the solution and atomizes the solution. At the same time, the fog-like droplets generated by the atomization of the solution have a large amount of ultrasonic cavitation energy inside. The atomized liquids in reaction vessel A and reaction vessel B are transferred to reaction vessel C through a negative pressure pipeline. Among them, the pressure in the negative pressure pipeline is 20 kPa. The mass ratio of the fog-like droplets from reaction vessel A to the fog-like droplets from reaction vessel B in reaction vessel C is controlled at 2:3.

[0028] In step three, the temperature in reaction vessel C is adjusted to 50 °C. The droplets of the vitamin B12 concentrated solution and the droplets of the potassium yellow prussiate solution in reaction vessel C react in an atomized state. There is a magnetic field in reaction vessel C with an intensity of 3 T. Under the action of the magnetic field, the ferrocyanide ions in the droplets of the potassium yellow prussiate solution are dispersed to the surface of the droplets, increasing the reaction contact area. At the same time, under the action of the magnetic field, the ions are promoted to align along the magnetic field lines, making the reaction more orderly, thereby accelerating the reaction rate.

[0029] In step four, the atomized solution after the reaction in step three is condensed through a condensation section pipeline and then enters collection container D. The condensation temperature of the condensation section pipeline is -5 °C. Poly aluminum chloride is added as a flocculant and activated carbon is added as a filter aid, and then filtration is carried out to obtain the finished vitamin B12 solution. The total mass of poly aluminum chloride and activated carbon added accounts for 0.5% of the mass of the solution in collection container D. The mass ratio of poly aluminum chloride to activated carbon is 1:10.

[0030] In this embodiment, the conversion efficiency of vitamin B12 is 85%, and the product purity is 96%.

[0031] Example 2 This embodiment provides a method for producing vitamin B12 using yellow prussiate of potash. In step one, the vitamin B12 fermentation broth is added to a rotary evaporator, and the temperature in the rotary evaporator is controlled at 60 °C. The concentrated solution is concentrated to a concentration of 3000 μg / ml. The concentrated solution in the rotary evaporator is transferred to reaction vessel A and cooled to 25 °C for standby. A 0.05 mol / L potassium yellow prussiate solution is added to reaction vessel B for standby.

[0032] In step two, the vitamin B12 fermentation concentrate in reaction vessel A and the potassium ferrocyanide solution in reaction vessel B are ultrasonically atomized using an ultrasonic atomizer. The frequency of the ultrasound is 40 kHz. The ultrasound increases the surface tension of the solution, causing the solution to atomize. At the same time, the mist droplets generated by the atomization of the solution have a large amount of ultrasonic cavitation energy inside. The atomized liquids in reaction vessel A and reaction vessel B are transferred to reaction vessel C through a negative pressure pipeline. Among them, the pressure in the negative pressure pipeline is 0 kPa. The mass ratio of the mist droplets from reaction vessel A to the mist droplets from reaction vessel B in reaction vessel C is controlled to be 2:5.

[0033] In step three, the temperature in reaction vessel C is adjusted to 90 °C. The droplets of the vitamin B12 concentrate and the droplets of the potassium ferrocyanide solution in reaction vessel C react in the atomized state. There is a magnetic field in reaction vessel C with an intensity of 7 T. Under the action of the magnetic field, the ferrocyanide ions in the droplets of the potassium ferrocyanide solution are dispersed to the surface of the droplets, increasing the reaction contact area. At the same time, under the action of the magnetic field, the ions are induced to align along the magnetic field lines, making the reaction more orderly, thereby accelerating the reaction rate.

[0034] In step four, the atomized solution after the reaction in step three is condensed through a condensation section pipeline and then enters the collection container D. The condensation temperature of the condensation section pipeline is 20 °C. Poly aluminum chloride is added as a flocculant and activated carbon is added as a filter aid, and then filtration is carried out to obtain the finished vitamin B12 solution. The total mass of the poly aluminum chloride and the activated carbon added accounts for 0.5% of the mass of the solution in the collection container D. The mass ratio of the poly aluminum chloride to the activated carbon is 10:1.

[0035] In this embodiment, the conversion efficiency of vitamin B12 is 92%, and the product purity is 97.5%.

[0036] Example 3 This embodiment provides a method for producing vitamin B12 using potassium ferrocyanide In step one, the vitamin B12 fermentation broth is added to a rotary evaporator. The temperature in the rotary evaporator is controlled to be 60 °C, and the concentrate is concentrated to a concentration of 1000 μg / ml. The concentrate in the rotary evaporator is transferred to reaction vessel A and cooled to 25 °C for use. A 0.05 mol / L potassium ferrocyanide solution is added to reaction vessel B for use.

[0037] In Step 2, use an ultrasonic nebulizer to ultrasonically nebulize the vitamin B12 fermentation concentrate in reaction vessel A and the potassium ferrocyanide solution in reaction vessel B. The frequency of the ultrasound is 35 kHz. The ultrasound increases the surface tension of the solution to atomize the solution. At the same time, the fog-like droplets generated by the atomization of the solution have a large amount of ultrasonic cavitation energy inside. Transfer the atomized liquids in reaction vessel A and reaction vessel B to reaction vessel C through a negative pressure pipeline. Among them, the pressure in the negative pressure pipeline is 25 kPa. Control the mass ratio of the fog-like droplets from reaction vessel A to the fog-like droplets from reaction vessel B in reaction vessel C to be 2:4.

[0038] In Step 3, adjust the temperature in reaction vessel C to 70 °C. The droplets of the vitamin B12 concentrate and the droplets of the potassium ferrocyanide solution in reaction vessel C react in the atomized state. There is a magnetic field in reaction vessel C with an intensity of 5 T. Under the action of the magnetic field, the ferrocyanide ions in the droplets of the potassium ferrocyanide solution are dispersed to the surface of the droplets, increasing the reaction contact area. At the same time, under the action of the magnetic field, it promotes the ions to arrange along the magnetic force lines, making the reaction more orderly, thereby accelerating the reaction rate.

[0039] In Step 4, condense the atomized solution after the reaction in Step 3 through a condensation section pipeline and then enter the collection container D. The condensation temperature of the condensation section pipeline is 10 °C. Add polyaluminum chloride as a flocculant and activated carbon as a filter aid, and filter to obtain the finished vitamin B12 solution. The total mass of the added polyaluminum chloride and activated carbon accounts for 0.5% of the mass of the solution in collection container D. The mass ratio of polyaluminum chloride to activated carbon is 5:5.

[0040] In this embodiment, the conversion efficiency of vitamin B12 is 95%, and the product purity is 98.5%.

[0041] Comparative experiment To verify the technical effect of the present invention, compare Example 2 with the traditional method: Traditional method: Use raw materials with the same concentration, but adopt a conventional liquid-liquid mixing reaction method, without ultrasonic atomization treatment and without the action of a magnetic field.

[0042] Test results: The conversion efficiency of vitamin B12 by the traditional method is 65%, and the product purity is 94%.

[0043] The comparison results show that compared with the traditional method, the conversion efficiency of the method of the present invention is increased by 27 percentage points, and the product purity is increased by 3.5 percentage points. This fully proves that the synergistic effect of ultrasonic atomization and magnetic field adopted in the present invention significantly improves the production efficiency of vitamin B12.

[0044] The embodiments of the present invention have been described in detail with reference to the accompanying drawings, but the present invention is not limited to the described embodiments. For those skilled in the art, without departing from the principle and spirit of the present invention, various changes, modifications, substitutions, and variations to these embodiments still fall within the protection scope of the present invention.

[0045] In the description of the specification, the description referring to terms such as "one embodiment", "example", "specific example", etc. means that the specific features, structures, materials, or characteristics described in connection with the embodiment or example are included in at least one embodiment or example of the present invention. In this specification, the schematic expressions of the above terms do not necessarily refer to the same embodiment or example. Moreover, the specific features, structures, materials, or characteristics described can be combined in a suitable manner in any one or more embodiments or examples.

[0046] As mentioned above, it is only the preferred specific embodiment of the present invention, but the protection scope of the present invention is not limited thereto. Any person skilled in the art within the technical scope disclosed by the present invention, according to the technical solution and inventive concept of the present invention, makes equivalent substitutions or changes, and all should be covered by the protection scope of the present invention.

[0047] The above content is only an example and explanation of the present invention. Those skilled in the art can make various modifications or supplements to the described specific embodiments or use similar methods for substitution, as long as they do not deviate from the invention or exceed the scope defined by the claims, and all should belong to the protection scope of the present invention.

[0048] Although the embodiments of the present invention have been shown and described, for those of ordinary skill in the art, it can be understood that various changes, modifications, substitutions, and variations can be made to these embodiments without departing from the principle and spirit of the present invention. All equivalent changes and improvements made within the scope of the application of the present invention should still fall within the scope covered by the patent of the present invention.

Claims

1. A method for producing vitamin B12 using yellow prussiate of potash, characterized in that, It includes the following steps: Step 1: Transfer the vitamin B12 fermentation broth into a rotary evaporator for concentration. Transfer the concentrated vitamin B12 fermentation broth into reaction vessel A for cooling. Add the yellow prussiate of potash solution into reaction vessel B for standby. Step 2: Ultrasonically atomize the liquids in reaction vessel A and reaction vessel B, and transfer the atomized liquids in reaction vessel A and reaction vessel B to reaction vessel C by using a negative pressure pipeline. Step 3: A magnetic field is applied in reaction vessel C, and the droplets of the vitamin B12 concentrated solution and the droplets of the yellow prussiate of potash solution in reaction vessel C react in the atomized state. Step 4: Condense the atomized solution after the reaction in Step 3 through a condensation section pipeline and then enter it into collection container D. Add the flocculant polyaluminum chloride and the filter aid activated carbon, and filter to obtain the finished vitamin B12 solution.

2. The method for producing vitamin B12 using yellow prussiate of potash according to claim 1, characterized in that, The vitamin B12 fermentation broth contains methylcobalamin, adenosylcobalamin, hydroxocobalamin, microorganisms, inorganic salts and water.

3. A method for producing vitamin B12 using yellow prussiate of potash according to claim 1, characterized in that, In Step 1, add the vitamin B12 fermentation broth into the rotary evaporator, control the temperature in the rotary evaporator at 60 °C, concentrate the concentrated solution to a concentration of 500 - 3000 μg / ml, transfer the concentrated solution in the rotary evaporator to reaction vessel A and cool it to 25 °C for standby. Add the 0.05 mol / L yellow prussiate of potash solution into reaction vessel B for standby.

4. A method for producing vitamin B12 using yellow prussiate of potash according to claim 1, characterized in that, In Step 1, the yellow prussiate of potash solution is one of potassium ferrocyanide solution and sodium ferrocyanide solution.

5. A method for producing vitamin B12 using yellow prussiate of potash according to claim 1, characterized in that, In Step 2, ultrasonically atomize the concentrated vitamin B12 fermentation broth in reaction vessel A and the yellow prussiate of potash solution in reaction vessel B with an ultrasonic atomizer. The frequency of the ultrasound is 30 - 40 kHz. The ultrasound increases the surface tension of the solution, atomizes the solution. At the same time, the fog-like droplets generated by the atomization of the solution have a large amount of ultrasonic cavitation energy inside. Transfer the atomized liquids in reaction vessel A and reaction vessel B to reaction vessel C through a negative pressure pipeline. Among them, the pressure in the negative pressure pipeline is 20 - 30 kPa, and control the mass ratio of the fog-like droplets from reaction vessel A and the fog-like droplets from reaction vessel B in reaction vessel C to be 2:3 - 5.

6. The method for producing vitamin B12 using yellow prussiate of potash according to claim 1, wherein, In Step 3, adjust the temperature in reaction vessel C to 50 - 90 °C. The droplets of the vitamin B12 concentrated solution and the droplets of the yellow prussiate of potash solution in reaction vessel C react in the atomized state. A magnetic field is provided in reaction vessel C with an intensity of 3 - 7 T. Under the action of the magnetic field, the ferrocyanide ions in the droplets of the yellow prussiate of potash solution are dispersed to the surface of the droplets, increasing the reaction contact area. At the same time, under the action of the magnetic field, the ions are induced to align along the magnetic field lines, making the reaction more orderly, thereby accelerating the reaction rate.

7. A method for producing vitamin B12 using yellow prussiate of potash according to claim 1, characterized in that, In Step 4, condense the atomized solution after the reaction in Step 3 through a condensation section pipeline and then enter it into collection container D. The condensation temperature of the condensation section pipeline is -5 - 20 °C. Add polyaluminum chloride as the flocculant and activated carbon as the filter aid, and filter to obtain the finished vitamin B12 solution.

8. A method for producing vitamin B12 using yellow prussiate of potash according to claim 7, characterized in that, The total mass of the added flocculant and filter aid accounts for 0.5% of the mass of the solution in collection container D.

9. A method for producing vitamin B12 using yellow prussiate of potash according to claim 7, characterized in that, The mass ratio of the polyaluminum chloride to the activated carbon is 1 - 10:10 - 1.

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