Soybean flavone continuous synthesis system

Abstract

The utility model discloses a soybean flavone continuous synthesis system which comprises a reaction kettle, the bottom of the reaction kettle is connected with a first discharge pipe, and a first bottom valve is arranged on the first discharge pipe; the bottom of the storage tank is connected with a second discharging pipe; a second bottom valve is arranged on the second discharging pipe; the mixing unit is communicated with the first discharging pipe and the second discharging pipe, and a first temperature control assembly is arranged on the mixing unit; and a second temperature control assembly is arranged on the reaction unit. According to the utility model, the problems of violent heat release in the Bass process reaction and long intermittent time, low space-time efficiency and low product yield of the kettle type batch reaction in the prior art are solved, and the original kettle type synthesis process which needs longer time and tedious steps is changed into a continuous synthesis process; the first temperature control assembly and the second temperature control assembly are used for controlling and adjusting the temperature in the mixing process and the reaction process respectively.

Description

Technical Field

[0001] The utility model relates to the technical field of daidzein production, in particular to a continuous daidzein synthesis system. Background Art

[0002] Daidzein, also known as daidzin, glycitein and daidzin, crystallizes as white to grayish-white crystalline powder in 50% ethanol and as flaky crystals in acetone. It can sublime under high vacuum, is easily soluble in ethanol and ether, and has a melting point of 315 - 323 °C (decomposition). Daidzein is one of the isoflavone compounds contained in soybean seeds and is widely present in leguminous plants such as kudzu vine and alfalfa. Therefore, soybeans, kudzu vine, alfalfa and their processed foods, soy products and kudzu powder products are regarded as foods with rich nutritional value and livestock feed.

[0003] Regarding the synthesis methods of daidzein, there are many reports in the literature and the methods are basically the same. Generally, the deoxybenzoin reaction is adopted: using p-hydroxyphenylacetic acid and resorcinol as raw materials, a Friedel-Crafts acylation reaction occurs in the presence of boron trifluoride to obtain 2,4-dihydroxyphenyl-4'-hydroxybenzyl ketone, and then the Bass process is used to cyclize with N,N-dimethylformamide (DMF) to synthesize daidzein.

[0004] In the prior art, the Friedel-Crafts acylation reaction conditions are mild, and the yield and quality are relatively stable. In the process of preparing daidzein by the second-step Bass process, there are problems of intense exothermic reaction and difficult reaction temperature control; however, the batch operation time of the batch reaction in a kettle is long, the space-time efficiency is low, the product yield is low and the quality fluctuates greatly. Summary of the Utility Model

[0005] The technical problem to be solved by the utility model is that the Bass process has an intense exothermic reaction and the batch reaction in a kettle has a long intermittent time, low space-time efficiency, low product yield and large quality fluctuation. The purpose is to provide a continuous daidzein synthesis system, which solves the problems of intense exothermic reaction in the existing Bass process, long intermittent time of the batch reaction in a kettle, low space-time efficiency, low product yield and large quality fluctuation.

[0006] The utility model is realized by the following technical solutions:

[0007] A continuous daidzein synthesis system, comprising:

[0008] A reaction kettle, the bottom of the reaction kettle is connected with a first discharge pipe, and a first bottom valve is arranged on the first discharge pipe;

[0009] A storage tank, the bottom of the storage tank is connected with a second discharge pipe, and a second bottom valve is arranged on the second discharge pipe;

[0010] Mixing unit, the mixing unit is communicated with both the first discharge pipe and the second discharge pipe, and a first temperature control component for adjusting the temperature is arranged on the mixing unit;

[0011] Reaction unit, the reaction unit is communicated with the outlet end of the mixing unit through a connecting pipe, and a second temperature control component is arranged on the reaction unit.

[0012] Further optimization, the mixing unit is a Venturi ejector, the Venturi ejector includes a mixing chamber communicated with the first discharge pipe and the second discharge pipe, and the outer wall of the Venturi ejector is connected with the first temperature control component.

[0013] Further optimization, a jet pump located on the first discharge pipe is also communicated between the reaction kettle and the Venturi ejector.

[0014] Further optimization, a pipeline flowmeter is also arranged on the second discharge pipe near the Venturi ejector side.

[0015] Further optimization, for facilitating monitoring and timely adjusting the mixing temperature, it is set that: the first temperature control component includes a refrigerating jacket arranged on the outer wall of the Venturi ejector, a first refrigerant outlet valve and a first refrigerant inlet valve are arranged on the refrigerating jacket, and a first thermometer is arranged on the connecting pipe.

[0016] Further optimization, a reaction liquid sight glass is arranged on the first discharge pipe below the first bottom valve.

[0017] Further optimization, a phosphorus oxychloride sight glass is arranged on the second discharge pipe below the second bottom valve.

[0018] Further optimization, the reaction unit is a microchannel tubular reactor communicated with the outlet end of the Venturi ejector.

[0019] Further optimization, for facilitating monitoring and timely adjusting the reaction temperature, it is set that: the second temperature control component includes a second refrigerant inlet valve and a second refrigerant outlet valve arranged on the microchannel tubular reactor, a feeding pipe is communicated with the outlet end of the microchannel tubular reactor, and a second thermometer is arranged on the feeding pipe.

[0020] Further optimization, the reaction kettle is a jacketed reaction kettle, and a heat medium inlet valve and a heat medium outlet valve are arranged on the jacketed reaction kettle.

[0021] Compared with the prior art, the utility model has the following advantages and beneficial effects:

[0022] 1. The mixing process and the reaction process are carried out continuously, changing the original batch synthesis process that requires a long time and has complicated steps into a continuous synthesis process, with high mass transfer efficiency, high process safety, good process repeatability, stable product quality, continuous and automatic operation, and high space-time efficiency.

[0023] 2. Use the first temperature control component and the second temperature control component to control and adjust the temperature of the mixing process and the reaction process respectively, so as to solve the problem of intense heat release and difficult temperature control. BRIEF DESCRIPTION OF THE DRAWINGS

[0024] The drawings described herein are used to provide a further understanding of the embodiments of the present invention, form a part of this application, and do not constitute a limitation on the embodiments of the present invention. In the drawings:

[0025] Figure 1 is a schematic structural diagram of an embodiment of the present invention;

[0026] Reference numerals in the drawings and corresponding component names:

[0027] 1 - reaction kettle, 2 - reaction liquid sight glass, 3 - first bottom valve, 4 - heat medium inlet valve, 5 - heat medium outlet valve, 6 - storage tank, 7 - phosphorus oxychloride sight glass, 8 - second bottom valve, 9 - Venturi ejector, 10 - jet pump, 11 - first thermometer, 12 - second refrigerant inlet valve, 13 - second refrigerant outlet valve, 14 - microchannel tubular reactor, 15 - second thermometer, 16 - pipeline flowmeter, 17 - first refrigerant inlet valve, 18 - first refrigerant outlet valve, 19 - refrigeration jacket. DETAILED DESCRIPTION OF THE EMBODIMENTS

[0028] To make the objectives, technical solutions, and advantages of the present invention clearer and more understandable, the present invention will be further described in detail below with reference to the embodiments and the drawings. The illustrative embodiments and descriptions thereof of the present invention are only used to explain the present invention and do not constitute a limitation on the present invention.

[0029] Embodiment 1 of the present invention provides a continuous synthesis system for daidzein, as Figure 1 shown, including:

[0030] A reaction kettle 1, the bottom of the reaction kettle 1 is connected with a first discharge pipe, and a first bottom valve 3 is arranged on the first discharge pipe;

[0031] A storage tank 6, the bottom of the storage tank 6 is connected with a second discharge pipe, and a second bottom valve 8 is arranged on the second discharge pipe;

[0032] A mixing unit, the mixing unit is communicated with both the first discharge pipe and the second discharge pipe, and a first temperature control component for adjusting the temperature is arranged on the mixing unit;

[0033] A reaction unit, the reaction unit is communicated with the outlet end of the mixing unit through a connecting pipe, and a second temperature control component is arranged on the reaction unit.

[0034] In the prior art, the Friedel-Crafts acylation reaction has mild conditions, and the yield and quality are relatively stable. In the process of preparing daidzein by the second-step Bass process, there are problems such as intense exothermic reaction and difficult control of reaction temperature; however, the batch operation time of the batch reaction in a kettle is long, the space-time efficiency is low, and the product yield and quality fluctuate greatly.

[0035] To solve the above problems, in this embodiment, a mixing unit and a reaction unit are used to make the mixing process and the reaction process proceed continuously, and at the same time, a first temperature control component and a second temperature control component are used to control and adjust the temperatures of mixing and reaction respectively to avoid the occurrence of intense exotherm.

[0036] Specifically, the working process of this embodiment is as follows:

[0037] The reaction kettle 1 is filled with an N,N-dimethylformamide solution of 4,6-dihydroxy-4'-hydroxyacetophenone intermediate, and the storage tank 6 is filled with phosphorus oxychloride; the first bottom valve 3 and the second bottom valve 8 are opened, and the materials enter the mixing unit for mixing, and then enter the reaction unit for reaction, so that the mixing and reaction processes proceed continuously.

[0038] During this process, the first temperature control component controls and adjusts the temperature of mixing, and the second temperature control component controls and adjusts the temperature of reaction.

[0039] Furthermore, the mixing unit is a Venturi ejector 9, and the Venturi ejector 9 includes a mixing chamber communicated with the first discharge pipe and the second discharge pipe, and the outer wall of the Venturi ejector 9 is connected to the first temperature control component.

[0040] Furthermore, a jet pump 10 is also communicated between the reaction kettle 1 and the Venturi ejector 9 and is located on the first discharge pipe.

[0041] Furthermore, the reaction kettle is a jacketed reaction kettle, and a heat medium inlet valve and a heat medium outlet valve are provided on the jacketed reaction kettle.

[0042] In this embodiment, the jet pump 10 can be used to lift and transport various liquids, so that the N,N-dimethylformamide solution of 4,6-dihydroxy-4'-hydroxyacetophenone intermediate in the reaction kettle 1 enters the mixing chamber in the Venturi ejector 9 after passing through the jet pump 10.

[0043] In addition, the Venturi ejector 9 can generate sufficient negative pressure, so as to suck the phosphorus oxychloride in the storage tank 6 into the mixing chamber.

[0044] Furthermore, a pipeline flowmeter 16 is also provided on the second discharge pipe near the Venturi ejector 9. The pipeline flowmeter 16 is used to monitor the flow rate transported by the storage tank 6, so as to adjust the opening degree of the first bottom valve 3 on the first discharge pipe.

[0045] Further, a reaction liquid sight glass 2 is provided on the first discharge pipe and is located below the first bottom valve 3. A phosphorus oxychloride sight glass 7 is provided on the second discharge pipe and is located below the second bottom valve 8. In this embodiment, the reaction liquid sight glass 2 is used to observe whether the liquid in the reaction kettle 1 is normally transported, and the phosphorus oxychloride sight glass 7 is used to observe whether the phosphorus oxychloride in the storage tank 6 is normally transported.

[0046] To facilitate monitoring and timely adjustment of the mixing temperature, it is set that: the first temperature control component includes a refrigerating jacket 19 provided on the outer wall of the Venturi ejector 9. A first refrigerant outlet valve 18 and a first refrigerant inlet valve 17 are provided on the refrigerating jacket 19. A first thermometer 11 is provided on the connecting pipe. Specifically, the heat generated during the mixing reaction is exchanged through the refrigerant in the refrigerating jacket 19. The refrigerant can enter from the first refrigerant inlet valve 17 and exit from the first refrigerant outlet valve 18. In addition, the first thermometer 11 is used to monitor the temperature generated by the mixing.

[0047] To facilitate monitoring and timely adjustment of the reaction temperature, it is set that: the second temperature control component includes a second refrigerant inlet valve 12 and a second refrigerant outlet valve 13 provided on the microchannel tubular reactor 14. The outlet end of the microchannel tubular reactor 14 is communicated with a feeding pipe, and a second thermometer 15 is provided on the feeding pipe. Specifically, the heat generated during the reaction is exchanged through the refrigerant of the microchannel tubular reactor 14. The refrigerant can enter from the second refrigerant inlet valve 12 and exit from the second refrigerant outlet valve 13. In addition, the second thermometer 15 is used to monitor the temperature generated by the reaction.

[0048] The specific operation process of the present utility model is as follows:

[0049] First, open the second refrigerant inlet valve 12 and the second refrigerant outlet valve 13 of the microchannel tubular reactor 14, and then open the first bottom valve 3 on the first discharge pipe.

[0050] While starting the injection pump 10, open the second bottom valve 8. The N,N-dimethylformamide solution of the 4,6-dihydroxy-4'-hydroxyacetophenone intermediate in the reaction kettle 1 enters the Venturi ejector 9 through the injection pump 10 and is rapidly and fully uniformly mixed with the phosphorus oxychloride sucked in under the negative pressure formed in the Venturi ejector 9 in the Venturi mixing chamber. The heat generated during the mixing reaction is exchanged through the refrigerant of the refrigerating jacket 19. The mixing reaction temperature is monitored by the temperature displayed by the first thermometer 11 at the outlet end of the Venturi ejector 9.

[0051] Subsequently, the N,N-dimethylformamide solution of the 4,6-dihydroxy-4'-hydroxyacetophenone intermediate after mixing and phosphorus oxychloride enter the microchannel tubular reactor 14. The reaction temperature is monitored and adjusted according to the second thermometer 15 at the outlet end of the microchannel tubular reactor 14. The refrigerant inlet valve of the microchannel tubular reactor 14 admits refrigerant to achieve a reaction temperature of 20-30 °C.

[0052] The reaction time is adjusted according to process requirements by controlling the residence time of the N,N-dimethylformamide solution of the 4,6-dihydroxy-4'-hydroxyacetophenone intermediate and phosphorus oxychloride in the microchannel tubular reactor 14. The flow rate and flow volume are controlled by adjusting the opening degrees of the first bottom valve 3 and the second bottom valve 8, thereby achieving the reaction time required by the process.

[0053] Finally, after completion in the microchannel tubular reactor 14, it enters the subsequent separation and purification process to obtain the daidzein product.

[0054] The specific embodiments described above have further elaborated on the purpose, technical solutions, and beneficial effects of the present utility model. It should be understood that the above are only specific embodiments of the present utility model and are not used to limit the protection scope of the present utility model. Any modifications, equivalent replacements, improvements, etc. made within the spirit and principles of the present utility model shall be included within the protection scope of the present utility model.

Claims

1. A continuous synthesis system of soybean flavonoids, characterized in that: include: A reactor, wherein a first discharge pipe is connected to the bottom of the reactor, and a first bottom valve is arranged on the first discharge pipe; A storage tank, wherein the bottom of the storage tank is connected to a second discharge pipe, and the second discharge pipe is provided with a second bottom valve; A mixing unit, the mixing unit is connected to the first discharge pipe and the second discharge pipe, and the mixing unit is provided with a first temperature control component for adjusting the temperature; The reaction unit is connected with the outlet end of the mixing unit through a connecting pipe, and a second temperature control component is arranged on the reaction unit.

2. The continuous synthesis system of soybean flavonoids according to claim 1, characterized in that: The mixing unit is a venturi ejector, which includes a mixing chamber connected to a first discharge pipe and a second discharge pipe, and an outer wall of the venturi ejector is connected to a first temperature control component.

3. The continuous synthesis system of soybean flavonoids according to claim 2, characterized in that: A jet pump located on the first discharge pipe is also connected between the reactor and the venturi ejector.

4. The continuous synthesis system of soybean flavonoids according to claim 2, characterized in that: The second discharge pipe is also provided with a pipeline flow meter close to one side of the venturi ejector.

5. The continuous synthesis system of soybean flavonoids according to claim 2, characterized in that: The first temperature control component includes a refrigeration jacket arranged on the outer wall of the venturi ejector, the refrigeration jacket is provided with a first refrigerant outlet valve and a first refrigerant inlet valve, and the connecting pipe is provided with a first thermometer.

6. The continuous synthesis system of soybean flavonoids according to claim 1, characterized in that: The first discharge pipe is provided with a reaction liquid sight glass located below the first bottom valve.

7. The continuous synthesis system of soybean flavonoids according to claim 1, characterized in that: The second discharge pipe is provided with a phosphorus oxychloride sight glass located below the second bottom valve.

8. The continuous synthesis system of soybean flavonoids according to claim 2, characterized in that: The reaction unit is a microchannel tubular reactor connected to the outlet end of the venturi ejector.

9. The continuous synthesis system of soybean flavonoids according to claim 8, characterized in that: The second temperature control component includes a second refrigerant inlet valve and a second refrigerant outlet valve arranged on the microchannel tubular reactor. The outlet end of the microchannel tubular reactor is connected to a feed pipe, and a second thermometer is arranged on the feed pipe.

10. The continuous synthesis system of soybean flavonoids according to claim 1, characterized in that: The reactor is a jacketed reactor, and a heat medium inlet valve and a heat medium outlet valve are arranged on the jacketed reactor.

Images