A method for preparing l-α-glycerophosphocholine

Abstract

The application belongs to the field of biological medicine, and proposes a preparation method of L-alpha-glycerylphosphocholine, which comprises esterification, neutralization, spray drying, condensation, filtration, concentration, crystallization, redissolution and decolorization, resin impurity removal, secondary filtration and concentration, secondary crystallization, drying and packaging according to a process route. The esterification is performed by using polyphosphoric acid and choline chloride. The reaction product after the esterification is diluted with pure water, and then neutralized with alkali. The neutralized liquid is dried in a spray drying tower to obtain an intermediate product. The intermediate product obtained by spray drying is put into a condensation kettle, and then ethanol and R-3-chloro-1,2-propanediol are added dropwise until L-alpha-glycerylphosphocholine, a metal chloride and a metal phosphate are generated. The application has the advantages of reasonable design, reduced process difficulty between esterification and condensation, shortened process cycle, reduced consumption of R-3-chloro-1,2-propanediol, ensured product purity and suitability for large-scale promotion.

Description

Technical Field

[0001] This invention belongs to the field of biomedicine, and particularly relates to a method for preparing L-α-glucosinolate. Background Technology

[0002] Glycerylphosphocholine (GPC) is a normally present water-soluble small molecule in the human body and a precursor in the biosynthesis of acetylcholine, an important neurotransmitter. The most important function of GPC is that the choline it produces is a water-soluble B vitamin, playing a vital role in the brain and nervous system. Studies have shown that GPC plays a crucial role in the production of certain hormones and neurotransmitters such as acetylcholine and human growth hormone, thereby supporting brain and nervous system function. L-α-glycerylphosphocholine has important applications in many fields, such as medicine and healthcare, food nutrition, cosmetics, and bioscience research.

[0003] Traditional synthetic routes involve complex multi-step processes, such as "esterification to produce phosphorylcholine chloride → synthesis and purification to produce calcium phosphorylcholine chloride → synthesis and purification to produce potassium phosphorylcholine chloride → synthesis of L-α-glycine phosphate". Purification of different salts in this route requires complex steps, such as "reaction of calcium phosphorylcholine chloride with potassium carbonate or potassium hydroxide to produce crude potassium phosphorylcholine chloride → filtration to remove calcium carbonate → purification → drying to obtain pure potassium phosphorylcholine chloride" and "reaction of calcium phosphorylcholine chloride with potassium carbonate or potassium hydroxide to produce crude potassium phosphorylcholine chloride → filtration to remove calcium carbonate → purification → drying to obtain pure potassium phosphorylcholine chloride". Furthermore, these processes are time-consuming.

[0004] The traditional synthesis process uses a large amount of R-3-chloro-1,2-propanediol, which also has several drawbacks, such as its toxicity and difficulty in degradation in the environment. It may remain and accumulate in environmental media such as soil and water, causing long-term potential harm to the ecological environment and affecting ecological balance and biodiversity.

[0005] In traditional processes, esterification is carried out using phosphoric acid and choline chloride for synthesis. This method has some drawbacks, such as harsh reaction conditions, complex product separation and purification processes, and the potential generation of a lot of waste. It is necessary to control the reaction conditions and carry out effective product separation and purification in order to obtain high-purity choline phosphate. Summary of the Invention

[0006] This invention addresses the technical problems existing in the traditional synthesis process of L-α-glucosinolate, and proposes a rationally designed method for preparing L-α-glucosinolate that is conducive to shortening the process cycle, reducing the consumption of R-3-chloro-1,2-propanediol, and ensuring product purity.

[0007] To achieve the above objectives, the technical solution adopted by the present invention is as follows: The present invention provides a method for preparing L-α-glucosidic choline, which includes esterification reaction, condensation reaction, filtration, concentration, crystallization, resolution and decolorization, resin impurity removal, secondary crystallization, drying and packaging according to the process route. The esterification reaction and condensation reaction also include neutralization reaction and spray drying, and the resin impurity removal and secondary crystallization also include secondary filtration and concentration.

[0008] Esterification reaction: Polyphosphoric acid and choline chloride are used for esterification reaction. The feed ratio of polyphosphoric acid to choline chloride is 400 kg: 320 kg to 450 kg by mass. The optimal reaction temperature range is 120℃ to 145℃.

[0009] Neutralization reaction: Dilute the reaction product after esterification reaction with pure water, then neutralize with alkali to a pH of 8.5-11.5; after the reaction is complete, add 1.5 molar amounts of calcium chloride (inorganic phosphate), react fully for 4 hours, and then send the reaction filtrate into the spray drying process.

[0010] Spray drying: The neutralized liquid is dried in a spray drying tower to obtain an intermediate product, which is a mixture of phosphorylcholine chloride metal salt, phosphorylcholine phosphate metal salt and phosphate metal salt;

[0011] Condensation reaction: The intermediate obtained by spray drying was put into a condensation vessel, and 4000L of ethanol was added as the reaction solvent. R-3-chloro-1,2-propanediol was added dropwise to the reaction vessel. The reaction temperature was 75℃~85℃, and the reaction was refluxed for 50~65h. The reaction endpoint was confirmed by thin-layer chromatography until L-α-glucosinolate, metal chloride salt, and metal phosphate salt were generated.

[0012] Crystallization: The concentrated liquid was cooled to the range of -0℃ to -15℃ and crystallized for 6 to 8 hours with stirring. Then it was centrifuged to obtain crude L-α-glucosinolate.

[0013] Preferably, the filtration process specifically includes: separating insoluble substances such as metal phosphate salts and metal chloride salts in ethanol as filter cakes through plate filtration; and transferring the ethanol solution containing L-α-glucosinolate to a concentration process.

[0014] Preferably, the concentration process specifically includes: concentrating an ethanol solution of L-α-glucosinolate under vacuum at a temperature of 80℃~95℃; distilling for 4~6 hours to distill off 3000L of ethanol.

[0015] Preferably, the resin impurity removal process specifically includes: removing ionizable impurities from the feed solution using anion and cation exchange resins, with a conductivity of ≤50μs / cm.

[0016] Preferably, the secondary filtration and concentration process specifically includes: filtering the filtrate after resin impurity removal through a precision filter, concentrating the filtrate under reduced pressure, controlling the temperature at 90℃~98℃, and achieving a maximum concentrated output of 1850L~1950L.

[0017] Preferably, the secondary crystallization process specifically includes: transferring the concentrated 90°C liquid after secondary filtration to a crystallization vessel, adding 4000-5000L of ethanol, cooling to the range of 8°C to -15°C, and crystallizing for 3-4 hours with stirring.

[0018] Preferably, the drying process specifically includes vacuum drying at a temperature of 90℃~120℃ until the moisture content is ≤1.0%.

[0019] Preferably, the exhaust gas generated by the spray drying tower is used to preheat the filtrate that is about to enter the spray drying tower. The spray drying tower includes a waste discharge pipe, and a preheater is provided at the discharge end of the waste discharge pipe. The preheater has a preheating chamber for the filtrate to pass through.

[0020] Preferably, the spray drying tower includes a hot air distributor and an atomizer disposed at its top. The hot air distributor includes a hot air duct, the end of which is spiral-shaped and has rotating blades and fixed blades disposed on its inner side. The atomizer is disposed at the spiral center of the hot air duct and includes an outer cone and an inner cone. The top of the outer cone is provided with a filtrate inlet, and the bottom of the inner cone is provided with a rotating component. The top of the rotating component is provided with a power source that is connected to it for transmission. The sides and bottom of the rotating component are provided with spray holes for spraying towards the outlet side of the hot air distributor.

[0021] Preferably, the rotating component includes a rotating shaft, a rotating body is provided on the side of the rotating shaft, a plurality of spiral-shaped guide vanes are provided on the rotating body, and a plurality of guide channels corresponding one-to-one with the guide vanes are provided on the rotating body. The guide channels are spiral-shaped and their sides and bottom surfaces are open. The cross-section of the guide channel is trapezoidal and the small bottom end of the trapezoid is distributed on the side of the rotating body. An atomizing plate is provided in the guide channel. The atomizing plate includes a spiral section and a bottom plate section, and the nozzles are distributed on the spiral section and the bottom plate section.

[0022] Preferably, the rotating body includes a first-stage inverted cone segment that rotatably engages with the bottom of the inner cone, the side of the first-stage inverted cone segment being located on the same inverted cone surface as the side of the inner cone, and a second-stage inverted cone segment that rotatably engages with the bottom of the outer cone at the bottom of the first-stage inverted cone segment, the side of the second-stage inverted cone segment being located on the same inverted cone surface as the side of the outer cone, the top surface of the second-stage inverted cone segment being an inclined surface, and the top surface of the second-stage inverted cone segment and the bottom surface of the first-stage inverted cone segment having a rounded transition.

[0023] Compared with the prior art, the advantages and positive effects of the present invention are as follows:

[0024] 1. The present invention provides a method for preparing L-α-glucosylcholine, which realizes the process of "esterification reaction to generate phosphorylcholine chloride → synthesis of phosphorylcholine chloride alkali metal salt → synthesis of L-α-glucosylcholine", which simplifies the production process and helps to shorten the process cycle.

[0025] 2. The present invention provides a method for preparing L-α-glucosylcholine, which adopts an innovative spray drying process to obtain crude solid phosphorylcholine alkali metal salt. This method enables the direct condensation reaction of crude solid phosphorylcholine alkali metal salt to synthesize L-α-glucosylcholine, which is beneficial to shortening the process cycle and reducing the consumption of R-3-chloro-1,2-propanediol, thus ensuring product quality.

[0026] 3. The present invention provides a method for preparing L-α-glucosinolate, which can recover the heat of the waste gas generated in the spray drying tower by using a preheater, thus saving energy. Moreover, the atomizer provided by the present invention has a good atomization effect and can fully contact the hot air in the hot air duct to ensure the quality of the product.

[0027] 4. The present invention is reasonably designed, which helps to shorten the process cycle, reduce the consumption of R-3-chloro-1,2-propanediol, and help to ensure product purity, making it suitable for large-scale promotion. Attached Figure Description

[0028] To more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings used in the following description of the embodiments will be briefly introduced. Obviously, the drawings described below are some embodiments of the present invention. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0029] Figure 1 A process diagram illustrating a method for preparing L-α-glucosinolate provided as an example;

[0030] Figure 2 A schematic diagram of the preheater and exhaust pipe provided for an embodiment;

[0031] Figure 3 Axonometric view of the hot air distributor and atomizer provided in the embodiment;

[0032] Figure 4 A front view of the hot air distributor and atomizer provided for an embodiment;

[0033] Figure 5 A front view of the atomizer provided for an embodiment;

[0034] Figure 6 A cross-sectional view of the atomizer provided in the embodiment along the BB direction;

[0035] Figure 7 A bottom view of the rotating component, atomizing plate, and nozzle provided in the embodiment;

[0036] Figure 8 Exploded view of the rotating component, atomizing plate, and nozzle provided in the embodiment;

[0037] Figure 9 A cross-sectional view of the hot air distributor provided in the embodiment;

[0038] In the above figures, 1. Preheater; 2. Waste discharge pipe; 3. Hot air distributor; 31. Hot air duct; 32. Rotating blade; 33. Fixed blade; 4. Atomizer; 41. Outer cone; 42. Inner cone; 43. Filtrate inlet; 44. Rotating component; 441. Shaft; 442. Rotating body; 4421. First-stage inverted cone section; 4422. Second-stage inverted cone section; 443. Guide vane; 444. Guide channel; 45. Power source; 46. Nozzle; 47. Atomizing plate; 471. Spiral section; 472. Bottom plate section. Detailed Implementation

[0039] To better understand the above-mentioned objectives, features, and advantages of the present invention, the present invention will be further described below in conjunction with the accompanying drawings and embodiments. It should be noted that, unless otherwise specified, the embodiments and features described in these embodiments can be combined with each other. For ease of description, the terms "upper," "lower," "left," and "right" appearing below only indicate that they correspond to the upper, lower, left, and right directions in the accompanying drawings and do not limit the structure.

[0040] Numerous specific details are set forth in the following description in order to provide a full understanding of the invention. However, the invention may also be practiced in other ways than those described herein, and therefore the invention is not limited to the specific embodiments disclosed in the following specification.

[0041] Examples, such as Figure 1 As shown, the present invention provides a method for preparing L-α-glycine choline, which includes esterification, condensation, filtration, concentration, crystallization, resolution and decolorization, resin purification, secondary crystallization, drying, and packaging according to the process route. The esterification and condensation reactions further include neutralization and spray drying, and the resin purification and secondary crystallization processes include secondary filtration and concentration. Specific details of some steps, such as esterification, neutralization, spray drying, and condensation, are as follows:

[0042] Esterification reaction: Polyphosphoric acid and choline chloride are used for esterification reaction. The feed ratio of polyphosphoric acid to choline chloride is 400 kg: 320 kg to 450 kg by mass. The optimal reaction temperature range is 120℃ to 145℃.

[0043] Neutralization reaction: Dilute the reaction product after esterification with pure water, then neutralize with alkali to a pH of 8.5–11.5; after the reaction is complete, add 1.5 molar amounts of calcium chloride (an inorganic phosphate), react fully for 4 hours, and then send the filtrate into the spray drying process; the neutralizing agent is any one of the alkali metal alkaline substances such as potassium hydroxide, sodium hydroxide, sodium carbonate, or potassium carbonate.

[0044] Spray drying: The neutralized liquid is dried in a spray drying tower to obtain an intermediate product, which is a mixture of phosphorylcholine chloride metal salt, phosphorylcholine phosphate metal salt and phosphate metal salt;

[0045] Condensation reaction: The intermediate obtained by spray drying was put into a condensation vessel, and 4000L of ethanol was added as the reaction solvent. R-3-chloro-1,2-propanediol was added dropwise to the reaction vessel. The reaction temperature was 75℃~85℃, and the reaction was refluxed for 50~65h. The reaction endpoint was confirmed by thin-layer chromatography until L-α-glucosinolate, metal chloride salt, and metal phosphate salt were generated.

[0046] Crystallization: The concentrated liquid was cooled to the range of -0℃ to -15℃ and crystallized for 6 to 8 hours with stirring. Then it was centrifuged to obtain crude L-α-glucosamine choline.

[0047] Resolution and decolorization: The hydrogen chloride gas produced by the esterification reaction can be absorbed by pure water in the resolution and filtration steps, and can be reacted with calcium carbonate, calcium oxide, or calcium hydroxide to obtain an aqueous solution of calcium chloride;

[0048] This invention breaks through the traditional complex multi-step synthetic route of "esterification reaction to generate phosphorylcholine chloride → synthesis and purification to produce calcium phosphorylcholine chloride → synthesis and purification to produce potassium phosphorylcholine chloride → synthesis of L-α-glucosinolate choline", and realizes "esterification reaction to generate phosphorylcholine chloride → synthesis of alkali metal salt of phosphorylcholine chloride → synthesis of L-α-glucosinolate choline", effectively simplifying the production process.

[0049] More specifically: First, it eliminates the need to synthesize pure phosphorylcholine potassium salt; L-α-glycine phosphate is directly synthesized from crude phosphorylcholine alkali metal salt. Second, it omits numerous process steps that previously involved synthesizing crude phosphorylcholine calcium salt, followed by filtration to separate calcium phosphate, ceramic filtration, concentration, crystallization, filtration to separate crystals, drying, and pulverization to obtain pure phosphorylcholine calcium salt. Third, it omits numerous steps involved in synthesizing and purifying pure phosphorylcholine calcium salt to produce pure phosphorylcholine potassium salt, such as "chlorination..." The process involves four steps: First, the reaction of calcium phosphorylcholine salt with potassium carbonate or potassium hydroxide produces crude potassium phosphorylcholine chloride salt. This is followed by filtration to remove calcium carbonate, purification, and drying to obtain pure potassium phosphorylcholine chloride salt. Second, after esterification, neutralization with an alkali metal yields an aqueous solution of phosphorylcholine chloride alkali metal salt. Spray drying is then used to rapidly and efficiently obtain crude phosphorylcholine chloride alkali metal salt solid. This approach facilitates the direct condensation reaction of crude phosphorylcholine chloride metal salt solid to synthesize L-α-glucosinolate. In this way, aside from subsequent purification steps, the synthesis pathway for L-α-glucosinolate effectively shortens the process chain and reduces the process cycle.

[0050] This invention directly synthesizes L-α-glycine choline from crude phosphorylcholine alkali metal salts; the phosphorylcholine alkali metal salts include any one of sodium phosphorylcholine chloride, potassium phosphorylcholine chloride, etc.

[0051] Furthermore, thin-layer chromatography (TLC) offers several advantages in determining reaction endpoints: Firstly, it is simple and rapid to operate, requiring no complex instruments. Simply spot the sample onto a TLC plate, develop it in the solvent, and then use a suitable method for colorimetric analysis to observe the separation of each component. The entire process is typically completed quickly, significantly improving experimental efficiency. Secondly, it provides excellent separation, enhanced visual clarity, and facilitates simultaneous comparison of multiple samples, particularly enabling the identification of L-α-glucosinolates, metal chlorides, and metal phosphates in this process.

[0052] To improve the quality of the final product prepared by the method of this invention, the invention also includes corresponding designs for processes such as filtration, concentration, resin impurity removal, secondary filtration and concentration, and secondary crystallization, as detailed below:

[0053] The filtration process specifically includes: separating insoluble substances such as metal phosphate salts and metal chloride salts in ethanol into filter cakes through plate filtration, and the separated filter cakes can be sold as by-products; the ethanol solution containing L-α-glucosinolate is then transferred to the concentration process for corresponding concentration treatment.

[0054] The concentration process specifically includes: concentrating an ethanol solution of L-α-glucosinolate under vacuum at a temperature of 80℃~95℃; distilling for 4~6 hours to distill off 3000L of ethanol.

[0055] The resin impurity removal process specifically includes: removing ionizable impurities from the feed solution through anion and cation exchange resins with a conductivity of ≤50μs / cm. At this conductivity, metal cations such as calcium and sodium ions in the solution can be removed, achieving the purpose of separation and purification.

[0056] The secondary filtration and concentration process specifically includes: filtering the resin-removed filtrate through a precision filter, concentrating the filtrate under reduced pressure, controlling the temperature at 90℃~98℃, and achieving a maximum concentrated output of 1850L~1950L.

[0057] The secondary crystallization process specifically includes: transferring the concentrated 90°C liquid after secondary filtration to a crystallization vessel, adding 4000-5000L of ethanol, cooling to the range of 8°C to -15°C, and crystallizing for 3-4 hours with stirring.

[0058] The drying process specifically includes using vacuum drying at a temperature of 90℃~120℃ until the moisture content is ≤1.0%.

[0059] The purity of L-α-glucosinolate can be effectively improved by using plate filtration, concentration, crystallization, resin impurity removal, secondary filtration concentration, and secondary crystallization. In particular, the temperature of secondary filtration concentration is higher than that of the filtration and concentration processes, and the temperature of secondary crystallization also shows a stepwise change compared to the first crystallization. Moreover, the stirring time is extended accordingly. Finally, after vacuum drying, the yield can be controlled at 70-78%, which meets the requirements of industrial production.

[0060] like Figure 2 As shown, considering the heat utilization issue in the spray drying tower, in order to improve the heat utilization rate, the waste gas generated by the spray drying tower provided by the present invention is used to preheat the filtrate that is about to enter the spray drying tower. Specifically, the spray drying tower includes a waste discharge pipe 2, and a preheater 1 is provided at the discharge end of the waste discharge pipe 2. The preheater 1 has a preheating chamber for the filtrate to pass through. The filtrate generated in the filtration process of the preparation process of the present invention is pumped upward into the preheating chamber of the preheater 1. During the process of the waste discharge pipe 2 passing through the preheater 1, the filtrate can be preheated to a certain extent. The preheated filtrate then flows to the atomizer 4 of the spray drying tower. In this way, heat can be recovered and utilized, and the efficiency of rapid evaporation of the atomized filtrate after contact with hot air can be improved, thereby improving the quality of the intermediate product.

[0061] like Figures 3-9As shown, to improve the atomization and drying performance of the spray drying tower for the filtrate, the spray drying tower provided by this invention includes a hot air distributor 3 and an atomizer 4 disposed at its top. The hot air distributor 3 includes a hot air duct 31, the end of which is spiral-shaped and has rotating blades 32 and fixed blades 33 disposed on its inner side. An exhaust port is disposed at the end of the hot air duct 31, facing the rotating blades 32. The rotating blades 32 and the fixed blades 33 are distributed vertically and horizontally, with an inner and outer staggered arrangement. A hollow support is disposed at the bottom of the fixed blades 33, and the support is connected to the bottom surface of the hot air duct 31 by a support rod. The rotating blades 32 are engaged with the support through a support bushing at their bottom. In this way, the rotating blades 32 can rotate continuously relative to the fixed blades 33 driven by the hot air, and the hot air can flow to the bottom of the atomizer 4 through the uniform distribution of the fixed blades 33 and the rotating blades 32.

[0062] Furthermore, the atomizer 4 is located at the spiral center of the hot air duct 31. The atomizer 4 includes an outer cone 41 and an inner cone 42. The top of the outer cone 41 is provided with a filtrate inlet 43, and the bottom of the inner cone 42 is provided with a rotating component 44. The top of the rotating component 44 is provided with a power source 45 that is connected to it for transmission. The sides and bottom of the rotating component 44 are provided with spray holes 46 that spray towards the outlet side of the hot air distributor 3. The outer cone 41 and the inner cone 42 are kept fixed. The filtrate is continuously pumped from the filtrate inlet 43 between the outer cone 41 and the inner cone 42. The rotating component 44 is driven by the power source 45 to guide the filtrate at high speed to the spray holes 46. The high-speed centrifugal force of the filtrate and the sharp reduction in the orifice diameter of the spray holes 46 can generate spray on the sides and bottom of the rotating component 44. The spray can fully contact the hot air with a moving tendency, thereby achieving rapid drying. The exhaust gas generated in this process enters the heat recovery path and is then discharged separately.

[0063] To improve the atomization effect of the rotating component 44 in the atomizer 4, the rotating component 44 provided by the present invention includes a rotating shaft 441, a rotating body 442 is provided on the side of the rotating shaft 441, a plurality of spiral-shaped guide vanes 443 are provided on the rotating body 442, and a plurality of guide channels 444 corresponding one-to-one with the guide vanes 443 are provided on the rotating body 442. The guide channels 444 are spiral-shaped and their sides and bottom surfaces are open. The cross-section of the guide channels 444 is trapezoidal and the small bottom end of the trapezoid is distributed on the side of the rotating body 442. An atomizing plate 47 is provided in the guide channel 444. The atomizing plate 47 includes a spiral section 471 and a bottom plate section 472, and nozzles 46 are distributed on the spiral section 471 and the bottom plate section 472. Among them, the guide vane 443 can make the high-speed rotating filtrate form a continuous water flow in the direction of the guide channel 444. The guide channel 444 utilizes the spatial distribution characteristics of the centrifugal filtrate to compress the centrifugal filtrate in the centrifugal direction. In particular, the space of the nozzle 46 on the atomizing plate 47 changes sharply compared with the cross section of the guide channel 444, thereby realizing high-pressure centrifugal atomization. In addition, the spiral section 471 and the bottom plate section 472 have nozzles 46 to control the direction and distribution uniformity of the spray. Therefore, this spray drying tower has good atomization performance and drying performance.

[0064] To improve the fit performance between the rotating body 442 and the outer cone 41 and inner cone 42, the rotating body 442 provided by the present invention includes a first-stage inverted cone section 4421 that rotatably fits with the bottom of the inner cone 42. The side surface of the first-stage inverted cone section 4421 is located on the same inverted cone surface as the side surface of the inner cone 42. The bottom of the first-stage inverted cone section 4421 is provided with a second-stage inverted cone section 4422 that rotatably fits with the bottom of the outer cone 41. The side surface of the second-stage inverted cone section 4422 is located on the same inverted cone surface as the side surface of the outer cone 41. The top surface of the second-stage inverted cone section 4422 is an inclined surface, and the top surface of the second-stage inverted cone section 4422 and the bottom surface of the first-stage inverted cone section 4421 are rounded. On the one hand, the first-stage inverted cone section 4421 and the inner cone 42, and the second-stage inverted cone section 4422 and the outer cone 41 can maintain good rotational sealing. On the other hand, it allows the filtrate to enter the centrifugation path quickly. The second-stage inverted cone section 4422 has a slope and rounded corner transition between itself and the first-stage inverted cone section 4421. This design allows the filtrate to enter different guide channels 444 more effectively during centrifugation, which is conducive to ensuring the formation of a continuous supply route and to ensuring the uniformity and fullness of atomization of the atomizer 4.

[0065] The above description is merely a preferred embodiment of the present invention and is not intended to limit the present invention in any other way. Any person skilled in the art may make changes or modifications to the above-disclosed technical content to create equivalent embodiments for application in other fields. However, any simple modifications, equivalent changes, and modifications made to the above embodiments based on the technical essence of the present invention without departing from the scope of the present invention shall still fall within the protection scope of the present invention.

Claims

1. A method for preparing L-α-glycine choline, comprising the following process steps: esterification reaction, condensation reaction, filtration, concentration, crystallization, resolution and decolorization, resin purification, secondary crystallization, drying and packaging, characterized in that, The process route from esterification to the synthesis of phosphorylcholine chloride alkali metal salt and then to the synthesis of L-α-glucosinolate choline is achieved through esterification, neutralization, spray drying and condensation. The resin impurity removal and secondary crystallization process also includes secondary filtration and concentration. Esterification reaction: Polyphosphoric acid and choline chloride are used for esterification reaction. The feed ratio of polyphosphoric acid to choline chloride is 400 kg: 320 kg to 450 kg by mass. The optimal reaction temperature range is 120℃ to 145℃. Neutralization reaction: Dilute the reaction product after esterification reaction with pure water, then neutralize with alkali to a pH of 8.5-11.5; after the reaction is complete, add 1.5 molar amounts of calcium chloride (inorganic phosphate), react fully for 4 hours, and then send the reaction filtrate into the spray drying process. Spray drying: The neutralized liquid is dried in a spray drying tower to obtain an intermediate product, which is a mixture of phosphorylcholine chloride metal salt, phosphorylcholine phosphate metal salt, and phosphate metal salt. The exhaust gas generated by the spray drying tower is used to preheat the filtrate to be fed into the spray drying tower. The spray drying tower includes a waste discharge pipe, and a preheater is provided at the discharge end of the waste discharge pipe. The preheater has a preheating chamber for the filtrate to pass through. The spray drying tower includes a hot air distributor and an atomizer at its top. The hot air distributor includes a hot air duct. The end of the hot air duct is spiral-shaped and has rotating blades and fixed blades on its inner side. The atomizer is located at the spiral center of the hot air duct. The atomizer includes an outer cone and an inner cone. The top of the outer cone has a filtrate inlet. The bottom of the inner cone has a rotating component. The top of the rotating component has a power source connected to it. The sides and bottom of the rotating component have spray holes for spraying towards the outlet side of the hot air distributor. Condensation reaction: The intermediate obtained by spray drying was put into a condensation vessel, and 4000L of ethanol was added as the reaction solvent. R-3-chloro-1,2-propanediol was added dropwise to the reaction vessel. The reaction temperature was 75℃~85℃, and the reaction was refluxed for 50~65h. The reaction endpoint was confirmed by thin-layer chromatography until L-α-glucosinolate, metal chloride salt, and metal phosphate salt were generated. Crystallization: The concentrated liquid was cooled to the range of -0℃ to -15℃ and crystallized for 6 to 8 hours with stirring. Then it was centrifuged to obtain crude L-α-glucosinolate.

2. The method for preparing L-α-glycine phosphate according to claim 1, characterized in that, The filtration process specifically includes: separating insoluble substances such as metal phosphate salts and metal chloride salts from ethanol in the form of a filter cake through plate filtration; and transferring the ethanol solution containing L-α-glucosinolate to a concentration process.

3. The method for preparing L-α-glycine phosphate according to claim 2, characterized in that, The concentration process specifically includes: concentrating an ethanol solution of L-α-glucosinolate under vacuum at a temperature of 80℃~95℃; distilling for 4~6 hours to distill off 3000L of ethanol.

4. The method for preparing L-α-glycine phosphate according to claim 3, characterized in that, The secondary filtration and concentration process specifically includes: filtering the resin-removed filtrate through a precision filter, concentrating the filtrate under reduced pressure, controlling the temperature at 90℃~98℃, and achieving a maximum concentrated output of 1850L~1950L.

5. The method for preparing L-α-glycine phosphate according to claim 4, characterized in that, The secondary crystallization process specifically includes: transferring the concentrated 90°C liquid after secondary filtration to a crystallization vessel, adding 4000-5000 L of ethanol, cooling to the range of 8°C to -15°C, and crystallizing for 3-4 hours with stirring.

6. The method for preparing L-α-glycine phosphate according to claim 5, characterized in that, The drying process specifically includes using vacuum drying at a temperature of 90℃~120℃ until the moisture content is ≤1.0%.

7. The method for preparing L-α-glycine phosphate according to claim 1, characterized in that, The rotating component includes a rotating shaft, a rotating body is provided on the side of the rotating shaft, a plurality of spiral-shaped guide vanes are provided on the rotating body, and a plurality of guide channels corresponding one-to-one with the guide vanes are provided on the rotating body. The guide channels are spiral-shaped and their sides and bottom surfaces are open. The cross-section of the guide channel is trapezoidal and the small bottom end of the trapezoid is distributed on the side of the rotating body. An atomizing plate is provided in the guide channel. The atomizing plate includes a spiral section and a bottom plate section, and the nozzles are distributed on the spiral section and the bottom plate section.

8. The method for preparing L-α-glycine phosphate according to claim 7, characterized in that, The rotating body includes a first-stage inverted cone segment that rotatably engages with the bottom of the inner cone. The side surface of the first-stage inverted cone segment is located on the same inverted cone surface as the side surface of the inner cone. The bottom of the first-stage inverted cone segment is provided with a second-stage inverted cone segment that rotatably engages with the bottom of the outer cone. The side surface of the second-stage inverted cone segment is located on the same inverted cone surface as the side surface of the outer cone. The top surface of the second-stage inverted cone segment is an inclined surface, and the top surface of the second-stage inverted cone segment and the bottom surface of the first-stage inverted cone segment have a rounded transition.

Images