Folic acid preparation device

Abstract

The invention relates to a folic acid preparation device, in particular to a reaction device integrating reaction and separation, belonging to the technical field of chemical production equipment. The reactor is mainly divided into three parts: a reaction kettle, a precipitation separator and a filter press. The folic acid generated by the reaction is timely separated out of the reaction system by utilizing the characteristic of low solubility of the folic acid, so that the influence of the raw materials on the purity of the folic acid is avoided, and meanwhile, the possibility that the folic acid wraps the 2, 4, 5-triamino-6-hydroxypyrimidine sulfate is reduced. Reaction liquid enters a deposition hopper at the lower part of the precipitation separator, clear liquid at the upper part is re-pumped into the reaction kettle through a pipeline, the precipitate is filtered to obtain filtrate and solid, the solid is a product, and the filtrate is re-pumped into the reaction kettle, so that the aim of separating while reacting is fulfilled. The product folic acid obtained by the reaction device is high in purity, and the reactant 2, 4, 5-triamino-6-hydroxypyrimidine sulfate is high in utilization rate.

Description

Technical Field

[0001] The invention belongs to the technical field of chemical production equipment, and relates to a reaction and separation integrated equipment, and in particular to a folic acid preparation device. Background Art

[0002] Folic acid, also known as vitamin B9, is a yellowish, crystalline compound. Folic acid is less stable and easily decomposes at room temperature. It is also very sensitive to changes in pH, and acidic conditions accelerate its decomposition. Folic acid is an important carrier of carbon metabolism and participates in the daily amino acid metabolism of the human body, as well as the synthesis of pyrimidine, purine and the main methylating agent S-adenosylmethionine (SAM). There are many synthetic routes for folic acid, among which the most widely used is the one using p-aminobenzoylglutamic acid, trichloroacetone and 2,4,5-triamino-6-hydroxypyrimidine sulfate as the main raw materials and water as the solvent. Due to the low solubility of 2,4,5-triamino-6-hydroxypyrimidine sulfate and the product folic acid in water, the product folic acid precipitates and mixes with the unreacted 2,4,5-triamino-6-hydroxypyrimidine sulfate. What's worse, folic acid precipitates on the surface of 2,4,5-triamino-6-hydroxypyrimidine sulfate to form a wrap, thereby affecting the further reaction of 2,4,5-triamino-6-hydroxypyrimidine sulfate and reducing the purity of folic acid.

[0003] At present, the Chinese patent with application number CN202123104950.3 proposes a new type of environmentally friendly mixing device for folic acid production. In order to solve the problems of poor folic acid mixing effect and easy clogging during discharging, the folic acid raw materials are fully mixed by synchronously rotating the spiral stirring rod, so that the folic acid raw materials are stirred and mixed more evenly, effectively ensuring the quality of the mixing of folic acid raw materials. The scraper plate rotates synchronously through the movement of the transmission shaft, which can scrape off the folic acid raw materials adhering to the inner wall of the mixing tank, thereby improving the processing efficiency of the mixing of folic acid raw materials. Due to the low solubility of 2,4,5-triamino-6-hydroxypyrimidine sulfate, the phenomenon of incomplete reaction cannot be fundamentally changed.

[0004] At present, the Chinese patent with application number CN202211573629.6 proposes a method for preparing folic acid. In view of the long reaction time (generally 6-8 hours), large amount of water (water consumption is more than 120 times based on the mass of folic acid produced), incomplete reaction of raw materials, low product purity and low yield, a continuous flow tubular reactor with at least two feed ports is used as a reaction device, and the reaction liquid a and the reaction liquid b are respectively connected to the two feed ports of the continuous flow tubular reactor. The reaction liquids collide violently in the continuous flow tubular reactor, and the reaction is completed instantly to generate a crude folic acid feed liquid, which is filtered to obtain a crude folic acid product. Although the reaction is completed instantly to increase the reaction rate, the product obtained by the reaction cannot be removed from the reaction system in time, and there is still folic acid encapsulating 2,4,5-triamino-6-hydroxypyrimidine sulfate, which cannot fundamentally change the problem of incomplete reaction.

[0005] Therefore, in the process of preparing folic acid, the dissolution rate is increased by reducing the encapsulation, 2,4,5-triamino-6-hydroxypyrimidine sulfate is continuously added, and the generated folic acid precipitate is separated in time during the reaction, thereby increasing the utilization rate of 2,4,5-triamino-6-hydroxypyrimidine sulfate and improving the yield and purity of folic acid, which is of great significance. Summary of the invention

[0006] According to the shortcomings of the existing devices, the present invention utilizes the low solubility of folic acid to separate the folic acid generated by the reaction from the reaction system in a timely manner, thereby avoiding the influence of the raw materials on the purity of folic acid and reducing the possibility of folic acid encapsulating 2,4,5-triamino-6-hydroxypyrimidine sulfate, thereby solving the problems raised in the background technology. Specifically, the technical solution of the present invention includes the following contents: In order to achieve the above object, the present invention provides a folic acid preparation device: The preparation device includes a reaction kettle, a sedimentation separator and a filter press, so as to achieve the effect of preparing and separating at the same time.

[0007] Furthermore, the reactor cover is provided with 8 feed ports, all of which are evenly distributed, including a water feed port, a 2,4,5-triamino-6-hydroxypyrimidine sulfate feed port, a p-aminobenzoylglutamate feed port, a trichloroacetone feed port, a sodium pyrosulfite feed port, a sodium carbonate aqueous solution feed port, an upper clear liquid feed port, and a filtrate feed port.

[0008] Furthermore, a stirring device is installed on the top of the reactor, and the stirring device is a frame-type stirring device. The reactor body is provided with a heat transfer oil inlet and a heat transfer oil outlet to achieve temperature control. A temperature measuring device is provided in the reactor, which is evenly distributed in the upper, middle and lower parts of the reactor to accurately control the temperature.

[0009] Furthermore, the 2,4,5-triamino-6-hydroxypyrimidine sulfate is continuously fed by a peristaltic pump, the feeding of water, the feeding of p-aminobenzoylglutamate, the feeding of trichloroacetone, and the feeding of sodium pyrosulfite are all one-time feedings, and the feeding of sodium carbonate aqueous solution is intermittent feeding, which is mainly used to adjust the pH of the solution to 3.2±0.2, and the feeding rate of the peristaltic pump is 50-150r / min.

[0010] Furthermore, a sedimentation discharge port is provided at the bottom of the reactor, the lower end of the sedimentation discharge port is connected to the inlet of the sedimentation separator through a pipeline, a sedimentation discharge pipe is installed at the bottom of the sedimentation separator, the sedimentation discharge pipe is a pipe for collecting materials in the sedimentation bucket, the upper part of the sedimentation discharge pipe is connected to a sedimentation bucket with an angle of 45°, the upper part of the sedimentation bucket is connected to a sedimentation tank with a closed structure, and the upper part of the sedimentation tank is connected to an inclined pipe with an inclination angle of 30°-40°.

[0011] Furthermore, liquid enters one side of the sedimentation tank, and liquid flows out on the other side through a pipeline and is connected to the inlet of the fluid pump. The outlet of the fluid pump is connected to the feed port of the reactor cover through a pipeline. The fluid pump speed is 100-200r / min, so that the flow of the fluid in the sedimentation tank is laminar, which facilitates the rapid sedimentation of the precipitate.

[0012] Furthermore, the discharge outlet in the discharge sink pipe is connected to the inlet of a diaphragm pump through a pipeline, the outlet of the diaphragm pump is connected to the inlet of a filter press through a pipeline, and the speed of the diaphragm pump is 30-80r / min.

[0013] Furthermore, the filter press is a plate and frame filter press, and the pore size of the filter cloth is 5-30 μm.

[0014] Furthermore, the outlet of the filter press is connected to the inlet of the lifting pump via a pipeline, the outlet of the lifting pump is connected to the feed port of the reactor cover via a pipeline, and the rotation speed of the lifting pump is 50-200r / min.

[0015] Furthermore, the fluid pump, diaphragm pump and lift pump are all in continuous operation to ensure that folic acid is separated from the reaction system in time, and the supernatant and filtrate are returned to the reactor to continue to participate in the folic acid synthesis reaction.

[0016] The benefits of the present invention are as follows: (1) utilizing the low solubility of folic acid to timely separate the folic acid generated by the reaction from the reaction system, avoiding the influence of the raw materials on the purity of folic acid, improving the purity of the product folic acid, and simplifying the subsequent steps and difficulty. (2) folic acid is timely separated from the reaction system, reducing the possibility of folic acid encapsulating 2,4,5-triamino-6-hydroxypyrimidine sulfate, and improving the utilization rate of 2,4,5-triamino-6-hydroxypyrimidine sulfate. (3) the device is composed of a reactor, a precipitation separator and a filter press, and performs continuous reaction-separation operation to achieve separation while reacting, reducing the amount of water used, and the overall structure is simple, the design is reasonable, and it is easy to manufacture and later operation and maintenance, and is suitable for large-scale industrial preparation.

[0017] By reducing raw material waste and lowering the encapsulation phenomenon of folic acid, the folic acid preparation process has been greatly optimized, thereby improving the yield and purity of folic acid. BRIEF DESCRIPTION OF THE DRAWINGS

[0018] In order to explain the present invention more clearly, the drawings required for the description will be briefly introduced below. For ordinary technicians in this field, other drawings can be obtained based on the drawings without paying any creative work.

[0019] Figure 1 The figure is a schematic diagram of the structure of a folic acid preparation device.

[0020] In the figure: 1. Reactor; 2. Stirring device; 3. Temperature measuring device; 4. Heat transfer oil inlet; 5. Heat transfer oil outlet; 6. Feed inlet; 7. Sedimentation outlet; 8. Sedimentation separator; 9. Sedimentation tank; 10. Sedimentation pipe; 11. Inclined pipe; 12. Sedimentation bucket; 13. Diaphragm pump; 14. Filter press; 15. Fluid pump; 16. Lifting pump; 17. Peristaltic pump. DETAILED DESCRIPTION

[0021] In order to facilitate the understanding of the present invention, the present invention is further described below in conjunction with examples and comparative examples. The following examples are only for a better understanding of the present invention and do not mean that the present invention is limited to the following examples.

[0022] like Figure 1 As shown, the folic acid preparation device of the present invention mainly includes a reaction kettle 1, a precipitation separator 8 and a filter press 14. Different from the traditional folic acid preparation method, the present invention can achieve separation while reacting, effectively improve the yield and purity of folic acid, and reduce subsequent steps. The specific implementation steps are as follows: Example 1: Improvement of stirring device 2 The reactor 1 is equipped with a frame stirring device 2 to increase the stirring speed. The temperature measuring device 3 realizes temperature control (40±2°C) through the heat transfer oil inlet 4 and the heat transfer oil outlet 5.

[0023] Reaction process: 2L of water and 1000g of p-aminobenzoylglutamic acid were added to the reactor 1 through the feed port 6 in sequence, the stirring device 2 was adjusted to 200r / min, and stirred until fully dissolved. The temperature of the temperature measuring device 3 of the reactor 1 was controlled at 40±2°C through the heat transfer oil inlet 4 and the heat transfer oil outlet 5. 535.4g of sodium pyrosulfite was added at one time through the feed port 6. After the sodium pyrosulfite was fully dissolved, 1508.5g of dichloroacetone was added at one time, and the stirring device 2 continued to stir until the materials were fully dissolved and mixed. 2,4,5-triamino-6-hydroxypyrimidine sulfate was continuously added through the feed port 6 using a peristaltic pump 17 at a speed of 80r / min. During the addition of 2,4,5-triamino-6-hydroxypyrimidine sulfate, sodium carbonate aqueous solution was intermittently added through the feed port 6 to adjust the pH value of the solution to 3.2±0.2.

[0024] Separation by precipitation: As the reaction proceeds, sediment is generated at the bottom of the reactor 1, and the sediment enters the sedimentation separator 8 through the sedimentation discharge port 7 connected to the bottom of the reactor 1. The fluid pump 15 is adjusted to a flow rate of 100 r / min, and the fluid pump 15 extracts the clear liquid on the top of the sedimentation tank 9, and enters the reactor 1 through the feed port 6 via the fluid pump 15. During the sedimentation process, the inclination angle of the inclined tube 11 is set to 30°, and the angle of the sedimentation bucket 12 is 45°. The sediment is transported to the filter press 14 for further filtration through the sedimentation discharge pipe 10 and the diaphragm pump 13, and the rotation speed of the diaphragm pump 13 is 70 r / min.

[0025] Filtration and recovery: The filter cloth has a pore size of 20 μm. The solid material separated by precipitation is further separated by a filter press 14. The filter press 14 can effectively remove the reaction liquid in the folic acid solid. The washing water volume is 2 L / time. After two washings, the filtered filtrate and washing liquid are refluxed to the reactor 1 via a lifting pump 16 at a speed of 150 r / min for recycling, thereby further improving the raw material utilization rate and the preparation efficiency of folic acid.

[0026] The solid produced by filtration is the high-purity folic acid product. After collection and drying, the content is detected by HPLC, and the purity and yield are calculated.

[0027] Advantages: The speed of stirring device 2 is increased, the stirring efficiency is significantly improved, the folic acid yield is 89.32%, and the purity of product folic acid reaches 98.11%.

[0028] Example 2: Improved design of sedimentation separator 8 A sedimentation hopper 12 with an angle of 45° is installed at the bottom of the sedimentation separator 8, and the inclination angle of the inclined pipe 11 is set to 35°.

[0029] Reaction process: the same as that in Example 1.

[0030] Separation by precipitation: As the reaction proceeds, sediment is generated at the bottom of the reactor 1, and enters the sedimentation separator 8 through the sedimentation outlet 7 connected to the bottom of the reactor 1. The fluid pump 15 is adjusted to a flow rate of 120 r / min, and the fluid pump 15 extracts the clear liquid on the top of the sedimentation tank 9, and enters the reactor 1 through the feed port 6 via the fluid pump 15. During the sedimentation process, the inclination angle of the inclined tube 11 is set to 35°, and the angle of the sedimentation bucket 12 is 45°. The sediment is transported to the filter press 14 for further filtration through the sedimentation discharge pipe 10 and the diaphragm pump 13, and the rotation speed of the diaphragm pump 13 is 70 r / min.

[0031] Filtration and recovery: Same as the filtration and recovery process in Example 1.

[0032] Advantages: The improvement of sedimentation separator 8 avoids the blockage of filter cloth caused by particle accumulation, the folic acid yield is 90.05%, and the purity of product folic acid reaches 98.77%.

[0033] Example 3: Optimization of filter press 14 Reaction process: the same as that in Example 1.

[0034] Separation by precipitation: Same as the separation by precipitation process in Example 2.

[0035] Filtration recovery: The filter cloth has a pore size of 10 μm. The solid material separated by precipitation is further separated by a filter press 14. The filter press 14 can effectively remove the reaction liquid in the folic acid solid. The washing water volume is 2 L / time. After two washings, the filtered filtrate and washing liquid are refluxed to the reactor 1 via a lifting pump 16 at a speed of 150 r / min for recycling, thereby further improving the raw material utilization rate and the preparation efficiency of folic acid.

[0036] Advantages: Reduced filtrate waste, folic acid yield of 90.75%, product folic acid purity of 98.82%.

[0037] Example 4: Temperature measuring device 3 A temperature measuring device 3 is installed in the reactor 1 to monitor the temperature gradient in the reactor in real time. The heat transfer oil inlet 4 and the heat transfer oil outlet 5 dynamically adjust the heat flow to control the temperature difference within 1°C.

[0038] Reaction process: 2L of water and 1000g of p-aminobenzoylglutamic acid were added to the reactor 1 through the feed port 6 in sequence, the stirring device 2 was adjusted to 200r / min, and stirred until fully dissolved. The temperature of the temperature measuring device 3 of the reactor 1 was controlled at 40±0.5°C through the heat transfer oil inlet 4 and the heat transfer oil outlet 5. 535.4g of sodium pyrosulfite was added at one time through the feed port 6. After the sodium pyrosulfite was fully dissolved, 1508.5g of dichloroacetone was added at one time, and the stirring device 2 continued to stir until the materials were fully dissolved and mixed. 2,4,5-triamino-6-hydroxypyrimidine sulfate was continuously added through the feed port 6 using the peristaltic pump 17, and the speed of the peristaltic pump 17 was 80r / min. During the addition of 2,4,5-triamino-6-hydroxypyrimidine sulfate, sodium carbonate aqueous solution was intermittently added through the feed port 6 to adjust the pH value of the solution to 3.2±0.2.

[0039] Separation by precipitation: Same as the separation by precipitation process in Example 2.

[0040] Filtration and recovery: Same as the filtration and recovery process in Example 3.

[0041] Advantages: Precisely control the temperature to avoid local overheating that may lead to folic acid degradation. The folic acid yield is 91.56% and the folic acid purity of the product is 99.03%.

[0042] Comparative Example: A reaction kettle 1 is used without a subsequent precipitation separator 8, and the precipitate is filtered once after the reaction is completed.

[0043] 2L of water was added to the reactor 1, and the stirring device 2 was started to stir. The temperature of the temperature measuring device 3 was controlled at 40°C±2°C through the heat transfer oil inlet 4 and the heat transfer oil outlet 5. 1000g of p-aminobenzoylglutamate was added at one time. After stirring until fully dissolved, 535.4g of sodium metabisulfite was added at one time. After the sodium metabisulfite was fully dissolved, 1508.5g of dichloroacetone was added at one time. After reacting for 1h, 987g of 2,4,5-triamino-6-hydroxypyrimidine sulfate was added at one time. After reacting for 1h, sodium carbonate solution was added to adjust the pH value to 3.2. The reaction was fully reacted for 6h. The reaction solution was filtered by a filter press 14 and washed twice with 2L of pure water. The solid was dried. The folic acid yield was 69.85%, and the product folic acid purity was 73.11%.

Claims

1. A folic acid preparation device, characterized in that: The reactor (1) comprises a reactor cover with 8 feed ports (6), all of which are evenly distributed, and are respectively a water feed port, a 2,4,5-triamino-6-hydroxypyrimidine sulfate feed port, a p-aminobenzoylglutamic acid feed port, a trichloroacetone feed port, a sodium pyrosulfite feed port, a sodium carbonate aqueous solution feed port, an upper clear liquid feed port, and a filtrate feed port.

2. A folic acid preparation device according to claim 1, characterized in that: A stirring device (2) is installed on the top of the reactor (1), and the stirring device (2) is a frame-type stirring device. The reactor (1) is provided with a heat transfer oil inlet (4) and a heat transfer oil outlet (5). The reactor (1) is provided with a temperature measuring device (3) which is evenly distributed at the top, middle and bottom of the reactor (1).

3. A folic acid preparation device according to claim 1, characterized in that: The 2,4,5-triamino-6-hydroxypyrimidine sulfate is continuously fed via a peristaltic pump (17); the water, p-aminobenzoylglutamic acid, trichloroacetone, and sodium pyrosulfite are all fed once; the sodium carbonate aqueous solution is fed intermittently; and the feeding rate of the peristaltic pump (17) is 50-150 r / min.

4. A folic acid preparation device according to claim 1, characterized in that: The bottom of the reactor (1) is provided with a sedimentation discharge port (7), the lower end of the sedimentation discharge port (7) is connected to the inlet of a sedimentation separator (8) through a pipeline, a sedimentation discharge pipe (10) is installed at the bottom of the sedimentation separator (8), the upper part of the sedimentation discharge pipe (10) is connected to a sedimentation bucket (12) with an angle of 45 degrees, the upper part of the sedimentation bucket (12) is connected to a sedimentation tank (9) with a closed structure, and the upper part of the sedimentation tank (9) is connected to an inclined pipe (11) with an inclination angle of 30 degrees to 40 degrees.

5. A folic acid preparation device according to claim 4, characterized in that: Liquid enters one side of the sedimentation tank (9), and liquid flows out on the other side through a pipeline connected to the inlet of a fluid pump (15). The outlet of the fluid pump (15) is connected to the feed port (6) of the reactor cover of the reaction kettle (1) through a pipeline. The speed of the fluid pump (15) is 100-200 r / min.

6. A folic acid preparation device according to claim 5, characterized in that: The discharge outlet in the discharge sink pipe (10) is connected to the inlet of a diaphragm pump (13) via a pipeline, and the outlet of the diaphragm pump (13) is connected to the inlet of a filter press (14) via a pipeline. The speed of the diaphragm pump (13) is 30-80 r / min.

7. A folic acid preparation device according to claim 6, characterized in that: The filter press (14) is a plate-and-frame filter press, and the pore size of the filter cloth is 5-30 μm.

8. A folic acid preparation device according to claim 6, characterized in that: The outlet of the filter press (14) is connected to the inlet of the lifting pump (16) via a pipeline, and the outlet of the lifting pump (16) is connected to the feed port (6) of the reactor cover of the reaction kettle (1) via a pipeline. The rotation speed of the lifting pump (16) is 50-200 r / min.

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