Method for preparing glycerophosphate by using microchannel continuous flow method
By combining microchannel continuous flow method with catalyst, the problem of water treatment in traditional batch reaction was solved, realizing the efficient preparation of glycerophosphate and reducing energy consumption and cost.
Patent Information
- Application Number
- CN202511684575.4
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-11-17
- Publication Date
- 2026-01-23
AI Technical Summary
Traditional batch reactors generate a large amount of wastewater during the preparation of glycerophosphates, requiring the addition of dehydrating agents, resulting in high reaction costs, long reaction times, and high energy consumption.
The microchannel continuous flow method is adopted, and the esterification reaction is carried out in a microchannel reactor using a combination of phosphate and organic acid catalysts. Moisture is removed in time to improve the reaction efficiency.
It significantly shortens reaction time, reduces energy consumption, improves synthesis efficiency, and reduces dependence on water, making it green and environmentally friendly.
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Abstract
Description
Technical Field
[0001] This invention relates to the field of microchannel and synthesis technology, specifically to a self-healing nanocapsule hybrid cottonseed insulating oil and its preparation method. Background Technology
[0002] Glycerophosphates are widely found in living organisms and are one of the main components of cell membranes, playing a crucial role in maintaining cell structure and function. In nature, glycerophosphates and their derivatives are diverse, possessing unique physicochemical properties and biological activities. Glycerophosphates can be used as raw materials for synthesizing nutrient fortifiers such as calcium glycerophosphate, sodium glycerophosphate, and calcium glycerophosphate, and their market prospects are broad.
[0003] Guo Hongchao et al. disclosed their research on the synthesis process of glycerophosphate, which uses phosphoric acid and glycerol as raw materials and adopts a direct esterification method to prepare glycerophosphate. The reaction formula is as follows:
[0004] In traditional batch reactors, as the reaction proceeds, a large amount of wastewater is generated, which inhibits the further occurrence of the reaction. Therefore, a large amount of dehydrating agent such as cyclohexane needs to be added, which increases the reaction cost, prolongs the reaction time, and requires high energy consumption. Summary of the Invention
[0005] To address the aforementioned problems, this invention provides a method for preparing glycerophosphates using a microchannel continuous flow method, which significantly reduces reaction time, energy consumption, and improves synthesis efficiency.
[0006] This invention provides a method for preparing glycerophosphates using a microchannel continuous flow method, comprising the following steps: S1. Add the catalyst to phosphoric acid and mix well to form feed solution A, wherein the catalyst contains phosphate and organic acid; S2. Mix glycerin with water to prepare solution B; S3. Feed solution A and feed solution B are respectively introduced into a microchannel reactor, and an esterification reaction occurs under heating conditions to obtain a glycerol phosphate solution.
[0007] Furthermore, the phosphate is one or more of sodium dihydrogen phosphate, sodium hydrogen phosphate, potassium hydrogen phosphate, potassium dihydrogen phosphate, lithium hydrogen phosphate, and lithium dihydrogen phosphate.
[0008] Furthermore, the organic acid is one or more of citric acid, malic acid, and tartaric acid.
[0009] Furthermore, the molar ratio of the phosphate to the organic acid is 1:(0.8-1.2); the amount of catalyst added is 0.5-10 wt% of phosphoric acid.
[0010] Furthermore, the concentration of phosphoric acid in the feed solution A is 40-85 wt%.
[0011] Furthermore, the concentration of glycerol in the feed solution B is 80~100 wt%.
[0012] Furthermore, the reaction temperature of the microchannel reactor in S3 is 25-90℃, and the back pressure is controlled at 1-5 bar.
[0013] Furthermore, the reaction temperature of the microchannel reactor is 60-90℃.
[0014] Furthermore, the flow rates of feed liquid A and feed liquid B in the microchannel reactor in S3 are both controlled at 5-30 ml / min.
[0015] Furthermore, the molar ratio of phosphoric acid in feed solution A to glycerol in feed solution B is 1:(1-1.3).
[0016] The present invention has the following beneficial effects: Unlike traditional batch reactors, this invention uses a microchannel reactor as the reaction device to remove moisture in a timely manner. It does not rely on dehydrating agents and has a higher tolerance for water present in the raw materials, thus improving the versatility of the reaction. Furthermore, this invention uses a certain proportion of organic acids and phosphates to form a catalyst. The chelation effect of several organic acids increases the solubility of phosphates in the reaction system, making the reaction occur more rapidly.
[0017] This invention utilizes a microchannel continuous flow method to prepare glycerophosphate, which can significantly shorten the reaction time, reduce energy consumption compared to traditional batch reactions, and is environmentally friendly. Detailed Implementation Unless otherwise specified, the experimental methods used in the following embodiments are conventional methods. Unless otherwise specified, the materials used in the following embodiments are commercially available products. The implementation schemes of the present invention will be described in detail below with reference to the embodiments; however, those skilled in the art will understand that the following embodiments are for illustrative purposes only and should not be considered as limiting the scope of the invention.
[0018] Example 1 After verifying that the reaction apparatus was operating normally, 115.3 g of 85wt% phosphoric acid solution was taken, and 1.56 g of sodium dihydrogen phosphate solid and 1.92 g of citric acid solid were weighed and dissolved in the phosphoric acid solution. The mixture was thoroughly mixed and recorded as feed solution A. Separately, 92.1 g of glycerol was prepared into an aqueous solution of the same volume as the phosphoric acid solution, recorded as feed solution B. Both feed solutions A and B were heated to 90 °C, and two feed pumps were started simultaneously at a rate of 1 ml / min. After reacting through four modules (90 °C), the reaction solution flowed out of the reactor. The effluent was collected, extracted with dichloromethane, and concentrated by evaporation to obtain glycerol phosphate ester. The yield was 97%, and the purity was 99%.
[0019] Example 2 After verifying that the reaction apparatus was operating normally, 115.3 g of 85wt% phosphoric acid solution was taken, and 1.56 g of sodium dihydrogen phosphate solid and 1.92 g of citric acid solid were weighed and dissolved in the phosphoric acid solution, mixed thoroughly, and recorded as feed solution A. Separately, 92.1 g of glycerol was prepared into an aqueous solution of the same volume as the phosphoric acid solution, recorded as feed solution B. Both feed solutions A and B were heated to 80 °C, and two feed pumps were started simultaneously to feed the solution at a rate of 1 ml / min through four reaction modules (80 °C). The resulting solution flowed out of the reactor, was collected, extracted with dichloromethane, evaporated, and concentrated to obtain glycerol phosphate ester. The yield was 90%, and the purity was 95%.
[0020] Example 3 After verifying that the reaction apparatus was operating normally, 115.3 g of 85wt% phosphoric acid solution was taken, and 1.42 g of sodium hydrogen phosphate solid and 1.92 g of citric acid solid were weighed and dissolved in the phosphoric acid solution, mixed thoroughly, and recorded as feed solution A. Separately, 92.1 g of glycerol was prepared into an aqueous solution of the same volume as the phosphoric acid solution, recorded as feed solution B. Both feed solutions A and B were heated to 90 °C, and two feed pumps were started simultaneously to feed the solution at a rate of 1 ml / min through four reaction modules (90 °C). The resulting solution flowed out of the reactor, was collected, extracted with dichloromethane, evaporated, and concentrated to obtain glycerol phosphate ester. The yield was 95%, and the purity was 93%.
[0021] Example 4 After verifying that the reaction apparatus was operating normally, 115.3 g of 85wt% phosphoric acid solution was taken, and 1.36 g of potassium dihydrogen phosphate solid and 1.92 g of citric acid solid were weighed and dissolved in the phosphoric acid solution. The mixture was thoroughly mixed and recorded as feed solution A. Separately, 92.1 g of glycerol was prepared into an aqueous solution of the same volume as the phosphoric acid solution, recorded as feed solution B. Both feed solutions A and B were heated to 90 °C, and two feed pumps were started simultaneously to feed the solution at a rate of 1 ml / min through four reaction modules (90 °C). The resulting solution flowed out of the reactor, was collected, extracted with dichloromethane, and concentrated by evaporation to obtain glycerol phosphate ester. The yield was 88%, and the purity was 92%.
[0022] Example 5 After verifying that the reaction apparatus was operating normally, 115.3 g of 85wt% phosphoric acid solution was taken, and 1.25 g of potassium dihydrogen phosphate solid and 1.54 g of citric acid solid were weighed and dissolved in the phosphoric acid solution. The mixture was thoroughly mixed and recorded as feed solution A. Separately, 92.1 g of glycerol was prepared into an aqueous solution of the same volume as the phosphoric acid solution, recorded as feed solution B. Both feed solutions A and B were heated to 90 °C, and two feed pumps were started simultaneously to feed the solution at a rate of 1 ml / min through four reaction modules (90 °C). The resulting solution flowed out of the reactor, was collected, extracted with dichloromethane, and concentrated by evaporation to obtain glycerol phosphate ester. The yield was 85%, and the purity was 90%.
[0023] Example 6 After verifying that the reaction apparatus was operating normally, 115.3 g of 85wt% phosphoric acid solution was taken, and 1.56 g of sodium dihydrogen phosphate solid and 1.92 g of citric acid solid were weighed and dissolved in the phosphoric acid solution, mixed thoroughly, and recorded as feed solution A. Separately, 92.1 g of glycerol was prepared into an aqueous solution of the same volume as the phosphoric acid solution, recorded as feed solution B. Both feed solutions A and B were heated to 60 °C, and two feed pumps were started simultaneously to feed the solution at a rate of 1 ml / min through four reaction modules (60 °C). The resulting solution flowed out of the reactor, was collected, extracted with dichloromethane, evaporated, and concentrated to obtain glycerol phosphate ester. The yield was 61%, and the purity was 90%.
[0024] Example 7 After verifying that the reaction apparatus was operating normally, 140.0 g of 70wt% phosphoric acid solution was taken, and 1.25 g of potassium dihydrogen phosphate solid and 1.54 g of citric acid solid were weighed and dissolved in the phosphoric acid solution. The mixture was thoroughly mixed and recorded as feed solution A. Separately, 92.1 g of glycerol was prepared into an aqueous solution of the same volume as the phosphoric acid solution, recorded as feed solution B. Both feed solutions A and B were heated to 90 °C, and two feed pumps were started simultaneously to feed the solution at a rate of 1 ml / min through four reaction modules (90 °C). The resulting solution flowed out of the reactor, was collected, extracted with dichloromethane, and concentrated by evaporation to obtain glycerol phosphate ester. The yield was 85%, and the purity was 90%.
[0025] Comparative Example 1 Compared with Example 1, only sodium dihydrogen phosphate was used as a catalyst and citric acid was not added. After the reaction, the yield of the product was 9% and the purity was 95%.
[0026] Comparative Example 2 Compared to Example 1, only citric acid was used as a catalyst without the addition of phosphate, and the reaction did not occur.
[0027] Comparative Example 3 Compared to Example 1, when a combination of glutamic acid and sodium dihydrogen phosphate was used as a catalyst without the addition of phosphate, the reaction did not occur.
[0028] Comparative Example 4 Compared to Example 1, the reaction did not occur when citric acid and sodium sulfate / sodium chloride combination was used as a catalyst and no phosphate was added.
[0029] The above examples demonstrate the preparation of glycerol phosphate esters. The combination of phosphate and organic acid enables the reaction to proceed efficiently and rapidly.
[0030] The above embodiments describe preferred embodiments of the present invention, but the present invention is not limited thereto. Within the scope of the inventive concept, various simple modifications can be made to the technical solutions of the present invention, including combinations of various technical features in any other way. These simple modifications and combinations should also be considered as the content disclosed in the present invention and are all within the protection scope of the present invention. Therefore, the protection scope of this patent should be determined by the appended claims.
Claims
1. A method for preparing glycerophosphates using a microchannel continuous flow method, characterized in that, Includes the following steps: S1. Add the catalyst to phosphoric acid and mix well to form feed solution A, wherein the catalyst contains phosphate and organic acid; S2. Use a certain concentration of glycerol as feed solution B; S3. Feed solution A and feed solution B are respectively introduced into a microchannel reactor, and an esterification reaction occurs under heating conditions to obtain a glycerol phosphate solution.
2. The method according to claim 1, characterized in that: The phosphate is one or more of sodium dihydrogen phosphate, sodium hydrogen phosphate, potassium hydrogen phosphate, potassium dihydrogen phosphate, lithium hydrogen phosphate, and lithium dihydrogen phosphate.
3. The method according to claim 1, characterized in that: The organic acid is one or more of citric acid, malic acid, and tartaric acid.
4. The method according to any one of claims 1 to 3, characterized in that: The molar ratio of the phosphate to the organic acid is 1:(0.8-1.2); the amount of catalyst added is 0.5-10 wt% of phosphoric acid.
5. The method according to claim 1, characterized in that: The concentration of phosphoric acid in the feed solution A is 40-85 wt%.
6. The method according to claim 1, characterized in that: The concentration of glycerol in the feed solution B is 80~100 wt%.
7. The method according to claim 1, characterized in that: The reaction temperature in the S3 microchannel reactor is 25-90℃, and the back pressure is controlled at 1-5 bar.
8. The method according to claim 7, characterized in that: The reaction temperature of the microchannel reactor is 60-90℃.
9. The method according to claim 1, characterized in that: In the S3 microchannel reactor, the flow rates of feed solutions A and B are both controlled at 5-30 ml / min.
10. The method according to claim 9, characterized in that: The molar ratio of phosphoric acid in feed solution A to glycerol in feed solution B is 1:(1-1.3).