Vanillin synthesis equipment

Abstract

The utility model discloses vanillin synthesis equipment which comprises a bromination reaction device, a separation device and a synthesis device, the bromination reaction device is communicated with the separation device, and a classification device is communicated with the synthesis device. According to the vanillin synthesis equipment provided by the utility model, a bromination device is used for centrifuging, drying and purifying to obtain a high-purity intermediate product, so that the problem of separation and purification of bromide is solved, the production quality of vanillin is improved, and vanillin is synthesized after the intermediate product is purified, so that the production efficiency of vanillin is improved. Therefore, the complicated purification process of subsequent products is avoided.

Description

TECHNICAL FIELD

[0001] The utility model belongs to the technical field of chemical synthesis, specifically relates to a vanillin synthesis equipment. BACKGROUND

[0002] Ethyl vanillin is 3-ethoxy-4-hydroxybenzaldehyde, molecular formula C9H10O3, molecular weight 166.147, melting point 77-78 DEG C. Because it has the same fragrance as vanillin, and the fragrance is 3-4 times of vanillin, it is the upgraded variety of vanillin at present. Ethyl vanillin is one of the most important spices in the world at present. Because it has the same fragrance as vanillin, and the fragrance is 3-4 times of vanillin, it is the upgraded variety of vanillin at present.

[0003] In the prior art, vanillin and ethyl vanillin are synthesized by the process route of first bromination and then etherification with hydroxybenzaldehyde as raw material, but the bromide after bromination is difficult to separate, so that high-purity products are difficult to obtain. UTILITY MODEL CONTENT

[0004] The utility model aims at providing a vanillin synthesis equipment, and solves the problem of high-purity products being difficult to obtain due to the difficulty in separating bromide after bromination in the related art.

[0005] Therefore, the utility model provides a vanillin synthesis equipment, which comprises a bromination reaction device, a separation device and a synthesis device, the bromination reaction device is communicated with the separation device, and the classification device is communicated with the synthesis device.

[0006] Preferably, the bromination reaction device comprises a first reaction kettle and an absorption kettle, and the first reaction kettle is communicated with the first absorption kettle.

[0007] Preferably, the bromination reaction device further comprises a first vacuum pump and a first vacuum buffer tank, the first vacuum pump is communicated with the first vacuum buffer tank, and the first vacuum buffer tank is communicated with the first reaction kettle and the absorption kettle.

[0008] Preferably, the bromination reaction device further comprises a raw material storage tank, and the raw material storage tank is communicated with the first reaction kettle.

[0009] Preferably, the separation device comprises a second reaction kettle, a first centrifugal machine, a first single-cone dryer and a melt crystallizer, the second reaction kettle is communicated with the first centrifugal machine, the first centrifugal machine is communicated with the first single-cone dryer, and the first single-cone dryer is communicated with the melt crystallizer.

[0010] Preferably, the centrifugal machine is connected with a fourth storage tank.

[0011] Preferably, the synthesis device comprises a third reactor, a second centrifuge and a second single-cone dryer, the third reactor being in communication with the second centrifuge, and the second centrifuge being in communication with the second single-cone dryer.

[0012] Preferably, the third reactor is connected with a reactant storage tank, and the reactant storage tank is in communication with the third reactor.

[0013] Preferably, the third reactor is connected with a condenser, and the condenser is connected with a seventh storage tank.

[0014] Preferably, the seventh storage tank is connected with a second buffer tank, and the second buffer tank is connected with a second vacuum pump.

[0015] Beneficial effects:

[0016] 1. The utility model provides a vanillin synthesis equipment, through bromination device carries out centrifugation, drying and purifies, obtains high purity intermediate product, solves the problem of bromide separation and purification, improves the production quality of vanillin, and synthesizes vanillin after purifying the intermediate product, thereby avoiding the complicated purification process of subsequent products. BRIEF DESCRIPTION OF DRAWINGS

[0017] In order to more clearly illustrate the technical scheme in the embodiment of the utility model or prior art, the following will briefly introduce the drawings needed to be used in the embodiment or prior art description, obviously, the drawings in the following description only some embodiments of the utility model, for ordinary skilled person in the art, under the premise of not paying creative labor, still can obtain other drawings according to these drawings.

[0018] Figure 1 It is the structure schematic drawing of embodiment 1 of a vanillin synthesis equipment provided by the utility model.

[0019] In the drawing, 1 is bromination reaction device, 11 is first reactor, 12 is absorption kettle, 13 is first vacuum pump, 14 is first vacuum buffer tank, 15 is first storage tank, 16 is second storage tank, 17 is third storage tank, 2 is separation device, 21 is second reactor, 22 is first centrifuge, 23 is first single-cone dryer, 24 is melt crystallizer, 25 is fourth storage tank, 3 is synthesis device, 31 is third reactor, 32 is second centrifuge, 33 is second single-cone dryer, 34 is condenser, 35 is seventh storage tank, 36 is second buffer tank, 37 is second vacuum pump, 38 is fifth storage tank, 39 is sixth storage tank. DETAILED DESCRIPTION

[0020] The content of the present application can be more easily understood by referring to the following detailed description of the preferred embodiments of the present application and included examples. Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs. In case of conflict, the present specification, including definitions, controls.

[0021] Example 1

[0022] Provided is a vanillin synthesis device as shown in Figure 1 The vanillin synthesis device includes a bromination reaction device 1, a separation device 2, and a synthesis device 3. The bromination reaction device 1 is in communication with the separation device 2, and the separation device 2 is in communication with the synthesis device 3. The bromination reaction device 1 is used to perform bromination reactions on raw materials, the separation device 2 is used to purify intermediate products, and the synthesis device 3 is used to synthesize vanillin.

[0023] The bromination reaction device 1 includes a first reaction kettle 11 and an absorption kettle 12, and the first reaction kettle 11 is in communication with the first absorption kettle 12. The bromination reaction device 1 also includes a first vacuum pump 13 and a first vacuum buffer tank 14, and the first vacuum pump 13 is in communication with the first vacuum buffer tank 14. The first vacuum pump 13 is in communication with the first reaction kettle 11 and the absorption kettle 12. The bromination reaction device 1 also includes a raw material storage tank, which is in communication with the first reaction kettle 11. In this embodiment, the raw material storage tank has three storage tanks, namely a first storage tank 15, a second storage tank 16, and a third storage tank 17. The first storage tank 15 is used to store hydroxybenzaldehyde, the second storage tank 16 is used to store dichloromethane, and the third storage tank 17 is used to store bromine. The first vacuum pump 13 generates a small amount of negative pressure to place the first reaction kettle 11 in a negative pressure environment. The absorption kettle 12 stores water for absorbing acidic gases generated during the reaction, and the water can be recovered as a solvent after the reaction is completed.

[0024] The separation device 2 includes a second reaction kettle 21, a first centrifuge 22, a first single-cone dryer 23, and a melt crystallizer 24. The second reaction kettle 21 is in communication with the first centrifuge 22, the first centrifuge 22 is in communication with the first single-cone dryer 23, and the first single-cone dryer 23 is in communication with the melt crystallizer 24. The centrifuge is connected to a fourth storage tank 25. The second reaction kettle 21 is connected to a water inlet pipe. The solid bromide is centrifuged through the first centrifuge 22 and then dried through the first single-cone dryer 23 to obtain high-purity 3,5-dibromo-4-hydroxybenzaldehyde. The liquid bromide enters the second reaction kettle 21, is cooled and crystallized, and then is dried in the first centrifuge 22 to obtain crude purified bromide. The crude purified bromide is crystallized in the melt crystallizer 24 to obtain high-purity 3-bromo-4-hydroxybenzaldehyde. The high-purity 3,5-dibromo-4-hydroxybenzaldehyde and the high-purity 3-bromo-4-hydroxybenzaldehyde are used in the synthesis device 3 to synthesize vanillin.

[0025] The synthesis device 3 comprises a third reaction kettle 31, a second centrifugal machine 32 and a second single-cone dryer 33, the third reaction kettle 31 is communicated with the second centrifugal machine 32, and the second centrifugal machine 32 is communicated with the second single-cone dryer 33. The third reaction kettle 31 is connected with a reactant storage tank, and the reactant storage tank is communicated with the third reaction kettle 31. The third reaction kettle 31 is connected with a condenser 34, and the condenser 34 is connected with a seventh storage tank 35. The seventh storage tank 35 is connected with a second buffer tank 36, and the second buffer tank 36 is connected with a second vacuum pump 37. The third reaction kettle 31 is connected with a water inlet pipe. The reactant storage tank is used for storing reactants, and in the embodiment, the reactant storage tank has two, which are a fifth storage tank 38 and a sixth storage tank 39, the fifth storage tank 38 is used for storing DMF, and the sixth storage tank 39 is used for storing hydrochloric acid. High-purity 3,5-dibromo-4-hydroxybenzaldehyde and high-purity 3-bromo-4-hydroxybenzaldehyde enter the third reaction kettle 31, DMF and hydrochloric acid are added, stirring reaction is carried out, then centrifugation is carried out in the second centrifugal machine 32, and drying is carried out in the second single-cone dryer 33 to obtain ethyl vanillin.

[0026] Working principle: methanol in the first storage tank 15 and dichloromethane in the second storage tank 16 are added to the first reaction kettle 11, then bromine in the third storage tank 17 is slowly added for reaction. During the reaction process, a micro-negative pressure environment is provided for the reaction process through the first vacuum pump 13 through the first buffer tank, and water in the absorption kettle 12 absorbs acidic gas in the reaction process. After the reaction is completed, the bromide in the first reaction kettle 11 is added to the second reaction kettle 21 for separation.

[0027] The solid bromide is centrifuged through the first centrifugal machine 22 and dried through the first single-cone dryer 23 to obtain high-purity 3,5-dibromo-4-hydroxybenzaldehyde; the liquid bromide enters the second reaction kettle 21, after cooling and crystallization, the crude purified bromide is dried through the first centrifugal machine 22, and then the crude purified bromide enters the melt crystallizer 24 for crystallization to obtain high-purity 3-bromo-4-hydroxybenzaldehyde.

[0028] High-purity 3,5-dibromo-4-hydroxybenzaldehyde and high-purity 3-bromo-4-hydroxybenzaldehyde enter the third reaction kettle 31, DMF in the fifth storage tank 38 is added for stirring reaction, then hydrochloric acid in the sixth storage tank 39 is added for acidification and stirring crystallization. After crystallization, centrifugation is carried out through the second centrifugal machine 32, and then drying is carried out in the second single-cone dryer 33 to obtain ethyl vanillin.

[0029] It should be noted that the above embodiments are only used to illustrate the technical solutions of the present application, and are not intended to limit the present application. Although the present application has been described in detail with reference to the foregoing embodiments, those skilled in the art should understand that they can still modify the technical solutions recorded in the foregoing embodiments, or make equivalent replacements for part or all of the technical features. These modifications or replacements do not make the essence of the corresponding technical solutions deviate from the scope of the technical solutions of the embodiments of the present application.

Claims

1. A vanillin synthesis apparatus, characterized in that, The application relates to a bromination reaction device, a separation device and a synthesis device, wherein the bromination reaction device is communicated with the separation device, and the separation device is communicated with the synthesis device. The separation device comprises a second reaction kettle, a first centrifugal machine, a first single-cone dryer and a melt crystallizer, the second reaction kettle is communicated with the first centrifugal machine, the first centrifugal machine is communicated with the first single-cone dryer, and the first single-cone dryer is communicated with the melt crystallizer. The first centrifugal machine is connected with a fourth storage tank. The bromination reaction device comprises a first reaction kettle and an absorption kettle, and the first reaction kettle is communicated with the absorption kettle.

2. The vanillin synthesis apparatus according to claim 1, wherein The bromination reaction device further comprises a first vacuum pump and a first vacuum buffer tank, the first vacuum pump is communicated with the first vacuum buffer tank, the first vacuum buffer tank is communicated with the first reaction kettle and the absorption kettle.

3. A vanillin synthesis apparatus according to claim 2, wherein The bromination reaction device further comprises a raw material storage tank, and the raw material storage tank is communicated with the first reaction kettle.

4. The vanillin synthesis apparatus according to claim 2, wherein The synthesis device comprises a third reaction kettle, a second centrifugal machine and a second single-cone dryer, the third reaction kettle is communicated with the second centrifugal machine, and the second centrifugal machine is communicated with the second single-cone dryer.

5. The vanillin synthesis apparatus according to claim 1, wherein The third reaction kettle is connected with a reactant storage tank, and the reactant storage tank is communicated with the third reaction kettle.

6. A vanillin synthesis apparatus according to claim 5, wherein The third reaction kettle is connected with a condenser, and the condenser is connected with a seventh storage tank.

7. The vanillin synthesis apparatus according to claim 5, wherein The seventh storage tank is connected with a second buffer tank, and the second buffer tank is connected with a second vacuum pump.

8. The vanillin synthesis apparatus according to claim 7, wherein ​

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