Continuous flow synthesis system for stigmasterol ester

Abstract

The utility model relates to the technical field of chemical equipment, and discloses a stigmasterol ester continuous flow synthesis system. The stigmasterol ester continuous flow synthesis system comprises a mixing unit, a reaction unit, a quenching unit and a separation unit. The mixing unit comprises a first mixing unit and a second mixing unit, and the first mixing unit is connected with the gas storage device through a gas conveying pipe and connected with the first liquid storage device through a material conveying pipe; the second mixing unit is connected with a second liquid storage device through a solution conveying pipe; the reaction unit comprises a reactor and a third temperature control device; the quenching unit comprises a quencher and a fourth temperature control device; and the separation unit is connected with the quencher through a material output pipeline. When the stigmasterol ester continuous flow synthesis system is used for synthesizing stigmasterol ester, the reaction temperature and the reaction time can be obviously reduced, the esterification rate equivalent to or even higher than that of a kettle reaction can be obtained, the reaction efficiency is greatly improved, and the stability of a product is improved.

Description

TECHNICAL FIELD

[0001] The utility model relates to a chemical equipment technical field, concretely relates to a continuous flow synthesis system of stigmasterol ester. BACKGROUND

[0002] Stigmasterol is a kind of tricyclic sterol, has high nutritional value, strong physiological activity and other characteristics, has extensive application in biological, medical and other fields. Research shows that stigmasterol has antioxidant, anti-inflammatory, antitumor, cholesterol-lowering, mental state protection, analgesic and other pharmacological activities and its application. Phytosterol cannot be synthesized in the human body, can only be taken from food. But from the structure of stigmasterol, its water solubility and fat solubility are poor, so that its solubility in the human body is limited, resulting in low bioavailability. Phytosterol ester (PSE) is the derivative of phytosterol, has good fat solubility under the premise of not changing the biological efficacy of phytosterol, has the double efficacy of phytosterol and fatty acid. Stigmasterol ester can be used to replace stigmasterol and added to food, medicine, to increase biological activity.

[0003] Phytosterol ester is generally prepared by enzymatic synthesis method and chemical synthesis method. The advantages of enzymatic synthesis method are mild conditions, non-toxic, and high and specific catalytic performance of enzyme, but there are problems such as high cost, long reaction time, need to add organic solvent, and difficult to realize industrialization, so chemical synthesis method is still the main preparation method of phytosterol ester. According to the different reaction substrates and acyl donors, chemical synthesis method can be divided into alcohol ester exchange method, direct esterification method, acid anhydride esterification method and acyl chloride esterification method. Among the many chemical synthesis methods of phytosterol ester, direct esterification reaction has good universality and is very important in chemical synthesis method.

[0004] At present, the preparation of stigmasterol by direct esterification method is mainly based on batch kettle reaction. Although the traditional batch kettle reaction is simple in operation, easy to control, strong in adaptability to raw materials and low in equipment investment. But each reaction needs to be loaded and unloaded after the end of the reaction and other auxiliary operations, and the production efficiency is low. And the heat and mass transfer efficiency of kettle reaction is low, the reaction conditions such as temperature, pressure, residence time and stirring speed cannot be accurately controlled, not only the energy consumption is high, the reaction rate is slow, the conversion rate is low, but also there are many by-products such as etherification and polymerization, which will affect the purity, yield and product quality stability of the product.

[0005] In addition, the reaction of direct esterification method has reversibility, usually needs to separate one component from the product or make one component of the reactant excessive, to make the reaction proceed to esterification direction, and the reaction is slow, usually needs to occur under the condition of high temperature and catalyst participation. UTILITY MODEL CONTENT

[0006] In order to overcome the prior art, the utility model discloses a kind of stigmasterol ester continuous flow synthesis systems, can be obtained with kettle formula reaction even higher esterification rate while significantly reducing reaction temperature and reaction time, greatly improve reaction efficiency, reduce side reaction, increase the stability of product.

[0007] To solve the above problems, the utility model adopts the technical scheme as follows:

[0008] A kind of stigmasterol ester continuous flow synthesis system, comprising:

[0009] Mixing unit, the mixing unit includes first mixing unit and second mixing unit, the first mixing unit and the second mixing unit are connected by pipeline;The first mixing unit is connected with gas storage device by gas delivery pipe, is connected with first storage device by material delivery pipe, and first temperature control device is arranged on the first storage device;The second mixing unit is connected with second storage device by solution delivery pipe, and second temperature control device is arranged on the second storage device;The first mixing unit is externally equipped with fifth temperature control device;The second mixing unit is externally equipped with sixth temperature control device;

[0010] Reaction unit, the reaction unit includes reactor and third temperature control device;The reactor of the reaction unit is connected with the second mixing unit by pipeline;

[0011] Quenching unit, the quenching unit includes quencher and fourth temperature control device;The quencher of the quenching unit is connected with the reactor;

[0012] Separation unit, the separation unit is connected with the quencher by material output pipeline.

[0013] The stigmasterol ester continuous flow synthesis system described above, the first flow control device is arranged on the gas delivery pipe, for controlling the flow of gas (such as nitrogen).

[0014] The stigmasterol ester continuous flow synthesis system described above, the second flow control device is arranged on the material delivery pipe, for controlling the flow when material is added.

[0015] The stigmasterol ester continuous flow synthesis system described above, the third flow control device is arranged on the solution delivery pipe, for controlling the flow when solvent or liquid catalyst is added.

[0016] The stigmasterol ester continuous flow synthesis system described above, pressure control device is arranged on the material output pipeline, for monitoring and controlling the pressure of reaction system.

[0017] The stigmasterol ester continuous flow synthesis system described above, the separation unit includes gas-liquid separation device, cooling device and centrifugal separation device connected in sequence, and product discharge port is arranged on the centrifugal separation device.

[0018] The continuous flow synthesis system of stigmasterol ester, the waste gas treatment device is further connected to the gas-liquid separation device, and the gas separated by the gas-liquid separation device enters the waste gas treatment device for treatment.

[0019] The continuous flow synthesis system of stigmasterol ester, a sample sampling port is further arranged on the gas-liquid separation device, so that sampling and monitoring of the esterification rate can be conveniently performed at any time.

[0020] The continuous flow synthesis system of stigmasterol ester, the centrifugal separation device is further connected with a solvent recovery pipe, and the solvent recovery pipe is connected with the second liquid storage device, and is used for recovering the solvent.

[0021] Compared with the prior art, the continuous flow synthesis system of stigmasterol ester has the advantages that:

[0022] (1) The continuous flow synthesis system of stigmasterol ester comprises a mixing unit, a reaction unit, a quenching unit and a separation unit, wherein the mixing unit, the reaction unit and the quenching unit are continuous flow regions.

[0023] (2) Compared with a kettle type reaction, the continuous flow synthesis system of stigmasterol ester can achieve similar or higher conversion rate under more moderate reaction conditions (lower reaction temperature) and less residence time (shorter reaction time).

[0024] (3) The continuous flow synthesis system of stigmasterol ester can significantly reduce the reaction temperature and the reaction time while achieving similar or higher esterification rate compared with the kettle type reaction, thereby greatly improving the reaction efficiency and increasing the stability of the product.

[0025] The utility model will be further described in detail in combination with the drawings and specific embodiments. BRIEF DESCRIPTION OF DRAWINGS

[0026] Figure 1 The schematic diagram of the continuous flow synthesis system of stigmasterol ester provided by the utility model embodiment is shown in the figure.

[0027] Explanation of reference numerals:

[0028] mixing unit-100, first mixing unit-110, gas storage device-111, gas delivery pipe-112, first flow control device-113, first liquid storage device-114, material delivery pipe-115, second flow control device-116, first temperature control device-117, fifth temperature control device-118, second mixing unit-120, second liquid storage device-121, solution delivery pipe-122, third flow control device-123, second temperature control device-124, sixth temperature control device-125;

[0029] reaction unit-200, reactor-210, third temperature control device-220;

[0030] quenching unit-300, quencher-310, fourth temperature control device-320, material output pipe-330, pressure control device-340;

[0031] separation unit-400, gas-liquid separation device-410, waste gas treatment device-411, sample sampling port-412, cooling device-420, centrifugal separation device-430, solvent recovery pipe-431, finished product discharge port-440. DETAILED DESCRIPTION

[0032] The embodiments of the present application will be described in detail below, with reference to Figure 1 The embodiments of the present application provide a stigmasterol ester continuous flow synthesis system, comprising: a mixing unit 100, a reaction unit 200, a quenching unit 300 and a separation unit 400. The mixing unit 100 comprises a first mixing unit 110 and a second mixing unit 120, and the first mixing unit 110 and the second mixing unit 120 are connected by a pipe. The first mixing unit 110 is connected with a gas storage device 111 through a gas delivery pipe 112, and is also connected with a first liquid storage device 114 through a material delivery pipe 115. It should be understood that the first mixing unit 110 is provided with a fifth temperature control device 118 on the outside, which is used to control the temperature in the first mixing unit 110, such as precise temperature control through the heat conduction oil on the outside. Further, the gas delivery pipe 112 is provided with a first flow control device 113 for controlling the flow of gas (such as nitrogen). According to the actual production needs, a pressure reducing valve can also be installed on the gas delivery pipe 112. The gas (such as nitrogen) is reduced in pressure from the gas storage device 111, then calibrated in flow through the first flow control device 113 after flow calibration, and then sent into the first mixing unit 110, so as to accurately control the flow of gas (such as nitrogen). In some embodiments, the first flow control device 113 can adopt a high-precision digital mass flowmeter.

[0033] Further, the material conveying pipe 115 is provided with a second flow control device 116 for controlling the flow rate of the material when added. In some embodiments, the second flow control device 116 adopts a Coriolis mass flowmeter, which can achieve precise control of the material. According to the actual production needs, a valve, a feeding pump, etc. can also be installed on the material conveying pipe 115. The first liquid storage device 114 is provided with a first temperature control device 117 for controlling the temperature of the liquid material in the first liquid storage device 114. In some embodiments, the first liquid storage device 114 is also provided with a stirring device, such as a stirrer, for mixing the material. Before continuous reaction, the material (such as oleic acid, linoleic acid, octanoic acid, lauric acid, palmitic acid, etc.) for synthesizing stigmastanol ester is mixed with stigmastanol in the first liquid storage device 114, and the temperature of the material in the first liquid storage device 114 is controlled by the first temperature control device 117, so that the material is fully dissolved, mixed, and kept in a liquid or slurry state for standby. During reaction, the mixed material is conveyed to the first mixing unit 110 after flow calibration by the second flow control device 116, and in the first mixing unit 110, the gas (such as nitrogen) is fully mixed with the mixed material.

[0034] The second mixing unit 120 is connected to the second liquid storage device 121 through a solution conveying pipe 122; the second mixing unit 120 is provided with a sixth temperature control device 125 outside for controlling the temperature in the second mixing unit 120, such as precise temperature control by the heat conduction oil outside.

[0035] The solution conveying pipe 122 is provided with a third flow control device 123 for controlling the flow rate of the solvent or liquid catalyst when added. In some embodiments, the third flow control device 123 can adopt a Coriolis mass flowmeter, which can achieve precise control of the solvent or liquid catalyst. According to the actual production needs, a valve, a liquid feeding pump, etc. can also be installed on the solution conveying pipe 122. The second liquid storage device 121 is provided with a second temperature control device 124 for controlling the temperature of the liquid material in the second liquid storage device 124. According to the actual production needs, the second liquid storage device 121 is also provided with a stirring device, such as a stirrer, for mixing the solvent or liquid catalyst. Before continuous reaction, the liquid catalyst (such as deep eutectic solvent) is heated in the second liquid storage device 121 by the second temperature control device 124, dissolved, mixed, and kept in a liquid state for standby. During reaction, the liquid catalyst (such as deep eutectic solvent) is conveyed to the second mixing unit 120 after flow calibration by the third flow control device 123 through the solution conveying pipe 122, and in the second mixing unit 120, it is fully mixed with the material conveyed from the first mixing unit 110, and enters the reaction unit 200.

[0036] The reaction unit 200 comprises a reactor 210 and a third temperature control device 220; the reactor 210 of the reaction unit 200 is connected with the second mixing unit 120 through a pipeline. After the gas (such as nitrogen), the mixed material and the liquid catalyst (such as deep eutectic solvent) enter the reaction unit 200, an esterification reaction occurs, and water vapor is generated. Under the blowing of the gas (such as nitrogen), the water vapor is carried out to improve the esterification rate at the reaction equilibrium. The length of the reaction unit 200 can be appropriately increased or decreased according to the actual production situation. The length of the reaction unit 200 can control the reaction residence time, and further control the reaction process. After the reaction in the reaction unit 200, the material enters the quenching unit 300 for quenching and ends the reaction.

[0037] The quenching unit 300 comprises a quencher 310 and a fourth temperature control device 320, and the quencher 310 of the quenching unit 300 is connected with the reactor 210 of the reaction unit 200. The reacted material enters the quencher 310 of the quenching unit 300, and is cooled and quenched by the fourth temperature control device 320. After quenching, the material enters the separation unit 400 for separation. Further, the quencher 310 of the quenching unit 300 is connected with the separation unit 400 through a material output pipeline 330, and a pressure control device 340 is arranged on the material output pipeline 330, which is used for monitoring and controlling the system pressure, such as the combination of a pressure gauge and a pressure regulating valve. It should be understood that the mixing unit 100, the reaction unit 200 and the quenching unit 300 are continuous flow regions. At the end of the continuous flow region, that is, on the material output pipeline 330 between the quenching unit 300 and the separation unit 400, the pressure control device 340 is arranged, which can be used for monitoring the pressure of the system, and also can adjust the back pressure according to the actual reaction situation, so as to adjust the flow rate of the gas (such as nitrogen) and the material by controlling the pressure, and then to fine-tune the residence time of the reaction, thereby improving the stability of the reaction. Through the design of each unit in the continuous flow region, precise temperature control can be realized, and through precise material flow control and adding or reducing the length of the continuous flow region, the residence time can be precisely controlled, so as to ensure the stability and repeatability of the reaction process.

[0038] The separation unit 400 is connected with the quencher 310, and the separation unit 400 comprises a gas-liquid separation device 410, a cooling device 420 and a centrifugal separation device 430 connected in sequence, and the centrifugal separation device 430 is provided with a finished product discharge port 440. The quenched material is sent into the gas-liquid separation device 410. According to the actual production needs, a pressure gauge and an exhaust port can be arranged above the gas-liquid separation device 410, and a sample sampling port 412 can be arranged below the gas-liquid separation device 410, so as to facilitate sampling at any time and monitoring the esterification rate.

[0039] The material is subjected to gas-liquid separation in the gas-liquid separation device 410, gas (such as nitrogen) and water vapor are discharged through the upper exhaust orifice, and can be collected and treated, such as by the exhaust treatment device 411 connected to the gas-liquid separation device 410; the separated liquid material is sent to the cooling device 420 for cooling treatment, and finally enters the centrifugal separation device 430 for centrifugal separation, and the crude bean sterol ester obtained by separation is discharged from the finished product discharge port 440. In some embodiments, the centrifugal separation device 430 is also connected with a solvent recovery pipe 431 connected with the second liquid storage device 121, for recovering the solvent or liquid catalyst (such as a deep eutectic solvent) separated by the centrifugal separation device 430.

[0040] It should be noted that, in the description of the utility model, if there is a description of the orientation, such as the orientation or positional relationship indicated by the upper, lower, front, rear, left, right and the like, it is based on the orientation or positional relationship shown in the drawing, and is only for the convenience of describing the utility model and simplifying the description, and does not indicate or imply that the indicated device or element must have a specific orientation, be constructed or operated in a specific orientation, and cannot be understood as a limitation on the utility model.

[0041] In the description of the utility model, the meaning of several is one or more, the meaning of multiple is two and more than two, greater than, less than, more than and the like are not included in the number, above, below, within and the like are included in the number. If there is a description of the first or second and the like, it is only for the purpose of distinguishing technical features, and cannot be understood as indicating or implying relative importance or implicitly indicating the number of indicated technical features or the sequence of indicated technical features.

[0042] In the description of the utility model, unless otherwise explicitly limited, the words such as setting, installing and connecting should be broadly understood, and the person skilled in the art can reasonably determine the specific meaning of the above words in the utility model according to the specific content of the technical scheme.

[0043] The above-mentioned embodiments are only preferred embodiments of the utility model, and cannot be used to limit the scope of protection of the utility model, and any non-substantial changes and replacements made by the person skilled in the art on the basis of the utility model all belong to the scope of protection claimed by the utility model.

Claims

1. A continuous flow synthesis system for stigmasterol esters, characterized in that, include: A mixing unit (100) includes a first mixing unit (110) and a second mixing unit (120), which are connected by pipes. The first mixing unit (110) is connected to a gas storage device (111) via a gas delivery pipe (112) and to a first liquid storage device (114) via a material delivery pipe (115). The first liquid storage device (114) is equipped with a first temperature control device (117). The second mixing unit (120) is connected to a second liquid storage device (121) via a solution delivery pipe (122). The second liquid storage device (121) is equipped with a second temperature control device (124). A fifth temperature control device (118) is provided outside the first mixing unit (110). A sixth temperature control device (125) is provided outside the second mixing unit (120). The reaction unit (200) includes a reactor (210) and a third temperature control device (220); the reactor (210) of the reaction unit (200) is connected to the second mixing unit (120) through a pipeline; Quenching unit (300), the quenching unit (300) includes a quencher (310) and a fourth temperature control device (320); the quencher (310) of the quenching unit (300) is connected to the reactor (210); A separation unit (400) is connected to the quencher (310) via a material output pipe (330).

2. The continuous flow synthesis system for stigmasterol esters according to claim 1, characterized in that, The gas delivery pipe (112) is equipped with a first flow control device (113) for controlling the flow rate of the gas.

3. The continuous flow synthesis system for stigmasterol esters according to claim 1, characterized in that, The material conveying pipe (115) is equipped with a second flow control device (116) for controlling the flow rate when the material is added.

4. The continuous flow synthesis system for stigmasterol esters according to claim 1, characterized in that, The solution delivery pipe (122) is equipped with a third flow control device (123) for controlling the flow rate when the solvent or liquid catalyst is added.

5. The continuous flow synthesis system for stigmasterol esters according to claim 1, characterized in that, The material output pipeline (330) is equipped with a pressure control device (340) for monitoring and controlling the pressure of the reaction system.

6. A continuous flow synthesis system for stigmasterol esters according to any one of claims 1-5, characterized in that, The separation unit (400) includes a gas-liquid separation device (410), a cooling device (420) and a centrifugal separation device (430) connected in sequence, and the centrifugal separation device (430) is provided with a finished product outlet (440).

7. The continuous flow synthesis system for stigmasterol esters according to claim 6, characterized in that, The gas-liquid separator (410) is also connected to a waste gas treatment device (411), and the gas separated by the gas-liquid separator (410) enters the waste gas treatment device (411) for treatment.

8. The continuous flow synthesis system for stigmasterol esters according to claim 6, characterized in that, The centrifugal separation device (430) is also connected to a solvent recovery pipe (431), which is connected to the second liquid storage device (121).

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