Ethyl maltol continuous reaction device

Abstract

The utility model discloses a continuous reaction device for ethyl maltol. The continuous reaction device comprises a Grignard reagent storage tank, a furfural storage tank, a magnesium chloride aqueous solution storage tank, a temperature control device and three groups of liquid level detection devices, according to the continuous reaction device, the characteristic of high mass transfer efficiency of the continuous flow micro-channel reactor is effectively utilized, the rotary-cut tubular reactor is combined, the continuous reaction at the addition stage and the hydrolysis stage of ethyl maltol is realized, the reaction temperature can be stabilized through the temperature control device and the temperature detection structure, the production efficiency and the product quality are improved, and the production cost is reduced. And the device is easy to control, high in safety and suitable for application requirements of industrial continuous production.

Description

TECHNICAL FIELD

[0001] The utility model relates to organic synthesis equipment technical field especially relates to a kind of ethyl maltol continuous reaction device. BACKGROUND

[0002] In the preparation process of ethyl maltol, addition and hydrolysis reaction are key steps. Traditional reaction kettle process has many drawbacks, for example, material adding speed is not easy to accurately control, reaction heat is difficult to transfer in time, heat exchange is uneven, etc. These factors are easy to cause the increase of side reaction, affect the yield and purity of ethyl maltol. However, the micro-channel reactor gradually gets application in the related synthesis field by virtue of its high mass transfer efficiency, accelerated reaction rate, shortened reaction time and the advantages of avoiding uneven mixing, low heat transfer efficiency and local overheating in traditional reaction device. However, at present, there is lack of a high-efficiency reaction device specially adapted for the addition and hydrolysis stages of ethyl maltol for continuous production, so as to better utilize the advantages of micro-channel reactor to improve production efficiency, product quality and ensure the safety and stability of production, and meet the needs of industrial continuous production. SUMMARY

[0003] The utility model aims at solving the shortcoming in prior art, and provides an ethyl maltol continuous reaction device.

[0004] In order to achieve the above-mentioned purpose, the utility model adopts the following technical scheme: an ethyl maltol continuous reaction device, comprising Grignard reagent storage tank, furfural storage tank, magnesium chloride aqueous solution storage tank, temperature control device and three sets of liquid level detection devices, the outlet end of the Grignard reagent storage tank, the outlet end of the furfural storage tank are connected with continuous flow micro-channel reactor, the outlet end of the continuous flow micro-channel reactor is fixedly connected with addition reagent buffer tank, the outlet end of the addition reagent buffer tank and the outlet end of the magnesium chloride aqueous solution storage tank are fixedly connected with rotary cutting pipe reactor, the outer wall of the continuous flow micro-channel reactor and the rotary cutting pipe reactor is provided with temperature detection structure for detecting internal reaction temperature, the temperature control device is through first heat pipe, first reflux pipe and continuous flow micro-channel reactor internal penetration, the temperature control device is through second heat pipe, second reflux pipe and rotary cutting pipe reactor internal penetration, the internal temperature of the continuous flow micro-channel reactor and the rotary cutting pipe reactor is controlled by temperature control device, the upper end of the Grignard reagent storage tank, the furfural storage tank and the magnesium chloride aqueous solution storage tank is provided with vent, three sets of liquid level detection devices are arranged in the Grignard reagent storage tank, the furfural storage tank and the magnesium chloride aqueous solution storage tank respectively.

[0005] As a further description of the above technical solution:

[0006] The temperature detection structure comprises a first temperature sensor and a second temperature sensor, which are arranged on the upper wall of the continuous flow micro-channel reactor and the upper wall of the rotary cutting pipe reactor respectively, the first temperature sensor is provided with a first detection end at one end of the continuous flow micro-channel reactor, the first detection end penetrates the upper wall of the continuous flow micro-channel reactor and extends into the inside of the continuous flow micro-channel reactor at an end away from the first temperature sensor, and the second temperature sensor is provided with a second detection end at one end of the rotary cutting pipe reactor, and the second detection end penetrates the upper wall of the rotary cutting pipe reactor and extends into the inside of the rotary cutting pipe reactor at an end away from the second temperature sensor.

[0007] As a further description of the above technical solution:

[0008] The first connecting pipe is fixedly connected with a first metering pump outside the wall, the second connecting pipe is fixedly connected with a second metering pump outside the wall, the fourth connecting pipe is fixedly connected with a third metering pump outside the wall, and the fifth connecting pipe is fixedly connected with a fourth metering pump outside the wall.

[0009] As a further description of the above technical solution:

[0010] The first connecting pipe is fixedly connected with a first metering pump outside the wall, the second connecting pipe is fixedly connected with a second metering pump outside the wall, the fourth connecting pipe is fixedly connected with a third metering pump outside the wall, and the fifth connecting pipe is fixedly connected with a fourth metering pump outside the wall.

[0011] As a further description of the above technical solution:

[0012] The continuous flow micro-channel reactor comprises a first shell, and the first shell is composed of a first outer shell, a first heat preservation layer and a first inner shell distributed in sequence from outside to inside, and the first inner shell is a babbitt alloy.

[0013] As a further description of the above technical solution:

[0014] The rotary cutting pipe reactor comprises a second shell, and the second shell is composed of a second outer shell, a second heat preservation layer and a second inner shell distributed in sequence from outside to inside, and the second inner shell is a babbitt alloy.

[0015] As a further description of the above technical solution:

[0016] The outlet end of the rotary cutting pipe reactor is fixedly connected with a liquid outlet pipe.

[0017] The utility model has the advantages of the following beneficial effects:

[0018] Compared with the prior art, the ethyl maltol continuous reaction device effectively utilizes the characteristics of high mass transfer efficiency of the continuous flow micro-channel reactor, combines the rotary cutting pipe reactor, realizes the continuous reaction of the ethyl maltol addition and hydrolysis stages, can stabilize the reaction temperature through the temperature control device and the temperature detection structure, improves the production efficiency and the product quality, and the device is easy to control, high in safety, and suitable for the application requirements of industrial continuous production. BRIEF DESCRIPTION OF DRAWINGS

[0019] Fig. 1 An overall structure schematic view of an ethyl maltol continuous reaction device is provided for the utility model.

[0020] Fig. 2 A continuous flow micro-channel reactor and a first temperature sensor connection structure partial section view schematic view of an ethyl maltol continuous reaction device is provided for the utility model.

[0021] Fig. 3 A rotary cutting pipe reactor and a second temperature sensor connection structure partial section view schematic view of an ethyl maltol continuous reaction device is provided for the utility model.

[0022] LEGEND:

[0023] 1, Grignard reagent storage tank; 2, furfural storage tank; 3, continuous flow micro-channel reactor; 3001, first shell; 3002, first heat preservation layer; 3003, first inner shell; 31, addition reagent buffer tank; 4, magnesium chloride aqueous solution storage tank; 5, rotary cutting pipe reactor; 5001, second shell; 5002, second heat preservation layer; 5003, second inner shell; 6, temperature control device; 7, first connecting pipe; 8, second connecting pipe; 9, third connecting pipe; 10, fourth connecting pipe; 11, fifth connecting pipe; 12, first heat conduction pipe; 13, first reflux pipe; 14, second heat conduction pipe; 15, second reflux pipe; 16, first temperature sensor; 1601, first detection end; 17, second temperature sensor; 1701, second detection end; 101, first metering pump; 201, second metering pump; 301, third metering pump; 401, fourth metering pump; 51, liquid outlet pipe. DETAILED DESCRIPTION

[0024] The technical solutions in the embodiments of the utility model will be clearly and completely described below with reference to the drawings in the embodiments of the utility model. Obviously, the described embodiments are only part of the embodiments of the utility model, rather than all the embodiments. Based on the embodiments in the utility model, all other embodiments obtained by those skilled in the art without creative labor fall within the scope of protection of the utility model.

[0025] REFERENCEFigs. 1 to 3 The utility model provides a kind of ethyl maltol continuous reaction device provided by the utility model: including Grignard reagent storage tank 1, furfural storage tank 2, magnesium chloride aqueous solution storage tank 4, temperature control device 6 and three groups of liquid level detection device, Grignard reagent storage tank 1 export end, furfural storage tank 2 export end are connected with continuous flow microchannel reactor 3 in common, Grignard reagent storage tank 1 is connected between continuous flow microchannel reactor 3 by first connecting pipe 7, furfural storage tank 2 is connected between continuous flow microchannel reactor 3 by second connecting pipe 8, continuous flow microchannel reactor 3 export end is fixedly connected with addition reagent buffer tank 31, continuous flow microchannel reactor 3 is connected between addition reagent buffer tank 31 by third connecting pipe 9, addition reagent buffer tank 31 export end, magnesium chloride aqueous solution storage tank 4 export end are fixedly connected with rotary cutting pipe type reactor 5 in common, rotary cutting pipe type reactor 5 export end is fixedly connected with liquid outlet pipe 51, addition reagent buffer tank 31 is connected between rotary cutting pipe type reactor 5 by fourth connecting pipe 10, magnesium chloride aqueous solution storage tank 4 is connected between rotary cutting pipe type reactor 5 by fifth connecting pipe 11, Grignard reagent storage tank 1 is Grignard reagent storage unit, furfural storage tank 2 is furfural storage unit, magnesium chloride aqueous solution storage tank 4 is magnesium chloride aqueous solution storage unit;

[0026] To accurately control delivery flow, first connecting pipe 7 outer wall is fixedly connected with first metering pump 101, second connecting pipe 8 outer wall is fixedly connected with second metering pump 201, fourth connecting pipe 10 outer wall is fixedly connected with third metering pump 301, fifth connecting pipe 11 outer wall is fixedly connected with fourth metering pump 401, by first metering pump 101, Grignard reagent can be accurately delivered from Grignard reagent storage tank 1 to continuous flow microchannel reactor 3, second metering pump 201 can accurately deliver furfural to continuous flow microchannel reactor 3, to ensure that Grignard reagent and furfural can participate in addition reaction in continuous flow microchannel reactor 3 according to appropriate amount, third metering pump 301 is used to accurately send addition reagent generated after reaction in continuous flow microchannel reactor 3 into rotary cutting pipe type reactor 5, fourth metering pump 401 is used to deliver magnesium chloride aqueous solution from magnesium chloride aqueous solution storage tank 4 to rotary cutting pipe type reactor 5, to ensure that magnesium chloride aqueous solution and addition reagent can participate in hydrolysis reaction in rotary cutting pipe type reactor 5 according to process requirement amount;

[0027] In order to detect the reaction temperature, the outer wall of the continuous flow micro-channel reactor 3 and the rotary cutting tube reactor 5 is provided with a temperature detection structure for detecting the internal reaction temperature, which comprises a first temperature sensor 16 and a second temperature sensor 17. The first temperature sensor 16 and the second temperature sensor 17 are arranged on the upper wall of the continuous flow micro-channel reactor 3 and the upper wall of the rotary cutting tube reactor 5 respectively. The first temperature sensor 16 is provided with a first detection end 1601 at one end thereof facing the continuous flow micro-channel reactor 3. The first detection end 1601 penetrates through the upper wall of the continuous flow micro-channel reactor 3 and extends into the interior of the continuous flow micro-channel reactor 3. The second temperature sensor 17 is provided with a second detection end 1701 at one end thereof facing the rotary cutting tube reactor 5. The second detection end 1701 penetrates through the upper wall of the rotary cutting tube reactor 5 and extends into the interior of the rotary cutting tube reactor 5. The internal reaction temperature of the continuous flow micro-channel reactor 3 is below 35℃, which can be accurately monitored by the first temperature sensor 16. The internal reaction temperature of the rotary cutting tube reactor 5 is below 30℃, which can be accurately monitored by the second temperature sensor 17.

[0028] In order to control the reaction temperature, the temperature control device 6 penetrates through the interior of the continuous flow micro-channel reactor 3 through the first heat conduction pipe 12 and the first backflow pipe 13. The temperature control device 6 penetrates through the interior of the rotary cutting tube reactor 5 through the second heat conduction pipe 14 and the second backflow pipe 15. The continuous flow micro-channel reactor 3 and the rotary cutting tube reactor 5 control the internal temperature through the temperature control device 6. The temperature control device 6 can control the reaction temperature in the interior of the continuous flow micro-channel reactor 3 and the rotary cutting tube reactor 5 respectively, so as to ensure that the entire addition and hydrolysis reaction is continuous, stable and efficient.

[0029] In order to facilitate ventilation and control the liquid level, the upper end of the Grignard reagent storage tank 1, the furfural storage tank 2 and the magnesium chloride aqueous solution storage tank 4 is provided with a ventilation port. Three groups of liquid level detection devices are arranged in the interior of the Grignard reagent storage tank 1, the furfural storage tank 2 and the magnesium chloride aqueous solution storage tank 4 respectively. The ventilation port is a common liquid storage tank ventilation structure provided with a filter component.

[0030] In order to guarantee the safety and stability of production, the continuous flow micro-channel reactor 3 comprises a first shell composed of a first outer shell 3001, a first heat preservation layer 3002 and a first inner shell 3003 distributed in sequence from outside to inside, the first inner shell 3003 is a babbitt alloy, the rotary cut tube reactor 5 comprises a second shell composed of a second outer shell 5001, a second heat preservation layer 5002 and a second inner shell 5003 distributed in sequence from outside to inside, the second inner shell 5003 is a babbitt alloy, the babbitt alloy has excellent corrosion resistance to various acids of different temperatures, and has good heat transfer and pressure resistance, the maximum bearing pressure can reach 2.0-2.5 MPa, which can effectively guarantee the safety of the reaction, and the cost is moderate, which is beneficial to industrial promotion, the first heat preservation layer 3002 and the second heat preservation layer 5002 can effectively avoid the influence of external temperature on the reaction temperature and improve the stability of the reaction.

[0031] Working principle: the Grignard reagent storage tank 1 is a Grignard reagent storage unit, the furfural storage tank 2 is a furfural storage unit, and the magnesium chloride aqueous solution storage tank 4 is a magnesium chloride aqueous solution storage unit; the first metering pump 101 can accurately deliver the Grignard reagent from the Grignard reagent storage tank 1 to the continuous flow micro-channel reactor 3, the second metering pump 201 can accurately deliver the furfural to the continuous flow micro-channel reactor 3, so that the Grignard reagent and the furfural can participate in the addition reaction in the continuous flow micro-channel reactor 3 in the appropriate amount, the third metering pump 301 is used to accurately send the addition reagent generated after the reaction of the continuous flow micro-channel reactor 3 into the rotary cut tube reactor 5, and the fourth metering pump 401 is used to deliver the magnesium chloride aqueous solution from the magnesium chloride aqueous solution storage tank 4 to the rotary cut tube reactor 5, so that the magnesium chloride aqueous solution and the addition reagent can participate in the hydrolysis reaction in the rotary cut tube reactor 5 in the required amount; the internal reaction temperature of the continuous flow micro-channel reactor 3 is below 35℃, which can be accurately monitored by the first temperature sensor 16, and the internal reaction temperature of the rotary cut tube reactor 5 is below 30℃, which can be accurately monitored by the second temperature sensor 17; the continuous flow micro-channel reactor 3 and the rotary cut tube reactor 5 are controlled by the temperature control device 6, the temperature control device 6 can control the reaction temperature in the continuous flow micro-channel reactor 3 and the rotary cut tube reactor 5 respectively, so that the whole addition and hydrolysis reaction can be continuously, stably and efficiently carried out; the first inner shell 3003 and the second inner shell 5003 are both babbitt alloys, the babbitt alloy has excellent corrosion resistance to various acids of different temperatures, and has good heat transfer and pressure resistance, the maximum bearing pressure can reach 2.0-2.5 MPa, which can effectively guarantee the safety of the reaction, and the cost is moderate, which is beneficial to industrial promotion, the first heat preservation layer 3002 and the second heat preservation layer 5002 can effectively avoid the influence of external temperature on the reaction temperature and improve the stability of the reaction.

[0032] Finally, it should be noted that: the above only for the preferred embodiments of the present application, and is not intended to limit the present application, although the foregoing embodiments of the present application has been described in detail, for the skilled in the art, it still can be modified, or for part of the technical features of the equivalent replacement, the spirit and principles of the present application, made any modification, equivalent replacement, improvement, etc., should be included within the scope of the present application.

Claims

1. A continuous reaction apparatus for ethyl maltol, characterized by: The temperature detection structure includes a first temperature sensor (16) and a second temperature sensor (17), the first temperature sensor (16) and the second temperature sensor (17) are arranged on the upper wall of the continuous flow micro-channel reactor (3) and the upper wall of the rotary cutting pipe reactor (5) respectively, the first temperature sensor (16) is provided with a first detection end (1601) at one end facing the continuous flow micro-channel reactor (3), the first detection end (1601) penetrates the upper wall of the continuous flow micro-channel reactor (3) and extends into the inside of the continuous flow micro-channel reactor (3) at the end away from the first temperature sensor (16), the second temperature sensor (17) is provided with a second detection end (1701) at one end facing the rotary cutting pipe reactor (5), the second detection end (1701) penetrates the upper wall of the rotary cutting pipe reactor (5) and extends into the inside of the rotary cutting pipe reactor (5) at the end away from the second temperature sensor (17).

2. The ethyl maltol continuous reaction device according to claim 1, characterized in that: The Grignard reagent storage tank (1) and the continuous flow micro-channel reactor (3) are connected through the first connecting pipe (7), the furfural storage tank (2) and the continuous flow micro-channel reactor (3) are connected through the second connecting pipe (8), the continuous flow micro-channel reactor (3) and the addition reagent buffer tank (31) are connected through the third connecting pipe (9), the addition reagent buffer tank (31) and the rotary cutting pipe reactor (5) are connected through the fourth connecting pipe (10), and the magnesium chloride aqueous solution storage tank (4) and the rotary cutting pipe reactor (5) are connected through the fifth connecting pipe (11).

3. The ethyl maltol continuous reaction device according to claim 1, characterized in that: The temperature detection structure includes a first temperature sensor (16) and a second temperature sensor (17), the first temperature sensor (16) and the second temperature sensor (17) are arranged on the upper wall of the continuous flow micro-channel reactor (3) and the upper wall of the rotary cutting pipe reactor (5) respectively, the first temperature sensor (16) is provided with a first detection end (1601) at one end facing the continuous flow micro-channel reactor (3), the first detection end (1601) penetrates the upper wall of the continuous flow micro-channel reactor (3) and extends into the inside of the continuous flow micro-channel reactor (3) at the end away from the first temperature sensor (16), the second temperature sensor (17) is provided with a second detection end (1701) at one end facing the rotary cutting pipe reactor (5), the second detection end (1701) penetrates the upper wall of the rotary cutting pipe reactor (5) and extends into the inside of the rotary cutting pipe reactor (5) at the end away from the second temperature sensor (17). The Grignard reagent storage tank (1) and the continuous flow micro-channel reactor (3) are connected through the first connecting pipe (7), the furfural storage tank (2) and the continuous flow micro-channel reactor (3) are connected through the second connecting pipe (8), the continuous flow micro-channel reactor (3) and the addition reagent buffer tank (31) are connected through the third connecting pipe (9), the addition reagent buffer tank (31) and the rotary cutting pipe reactor (5) are connected through the fourth connecting pipe (10), and the magnesium chloride aqueous solution storage tank (4) and the rotary cutting pipe reactor (5) are connected through the fifth connecting pipe (11).

4. The ethyl maltol continuous reaction device according to claim 3, characterized in that: The outer wall of the first connecting pipe (7) is fixedly connected with a first metering pump (101), the outer wall of the second connecting pipe (8) is fixedly connected with a second metering pump (201), the outer wall of the fourth connecting pipe (10) is fixedly connected with a third metering pump (301), and the outer wall of the fifth connecting pipe (11) is fixedly connected with a fourth metering pump (401).

5. The ethyl maltol continuous reaction device according to claim 1, characterized in that: The continuous flow micro-channel reactor (3) comprises a first shell which is composed of a first outer shell (3001), a first heat preservation layer (3002) and a first inner shell (3003) distributed in sequence from outside to inside, and the first inner shell (3003) is a babbitt alloy.

6. The ethyl maltol continuous reaction device according to claim 1, characterized in that: The rotary cut pipe reactor (5) comprises a second shell which is composed of a second outer shell (5001), a second heat preservation layer (5002) and a second inner shell (5003) distributed in sequence from outside to inside, and the second inner shell (5003) is a babbitt alloy.

7. The ethyl maltol continuous reaction device according to claim 1, characterized in that: The rotary cut pipe reactor (5) is fixedly connected with a liquid outlet pipe (51) at an outlet end.

Images