CN212549488U - Production device of 5-nitrofurfural diacetate - Google Patents

Abstract

The utility model relates to a production device of 5-nitrofurfural diacetate, including reation kettle, reation kettle pan feeding mouth communicates respectively with furfural storage tank, acetic anhydride storage tank and cobalt methane sulfonate storage tank, reation kettle bottom discharge gate passes through pipeline and vacuum filter intercommunication, and vacuum filter's filter residue discharge gate is through conveying mechanism and dissolving tank intercommunication, dissolving tank bottom organic phase discharge tube communicates through pipeline and first adsorber and second adsorber in proper order, and second adsorber filtrating discharge gate passes through pipeline and desicator intercommunication, the dissolving tank is equipped with 1, 2 dichloroethane pan feeding pipe. The utility model discloses a superacid catalysis system that methanesulfonic acid cobalt, acetic acid are constituteed need not add other solvents again, and the acetic acid has also overcome the problem that adopts sulphuric acid can lose the raw materials, and is low to environmental pollution.

Description

Production device of 5-nitrofurfural diacetate

Technical Field

The utility model relates to a chemical synthesis technical field relates to the apparatus for producing of 5-nitrofurfural diacetate.

Background

5-nitrofurfural diacetate is a medical intermediate used for preparing furan anti-infective drugs. The color of the product is poor, and the product is easy to be oxidized and turn green when being exposed to light or placed in air. Is easily dissolved in ethanol and is not dissolved in water. CN101492434A relates to a production improvement process method of 5-nitrofurfural diacetate, which comprises the steps of putting prepared acetic anhydride into a tank, adding a sulfuric acid catalyst, dropwise adding nitric acid, dropwise adding furfural, then carrying out double dropwise adding, continuing stirring after the materials are added, opening induced air to add prepared mother liquor as soon as possible after the reaction is finished, adding a sodium carbonate aqueous solution when the mother liquor is added to 3/4 of the total amount, filtering out the mother liquor, transferring 5-nitrofurfural diacetate into a centrifuge for centrifugal drying, and obtaining white loose 5-nitrofurfural diacetate as fine crystals. The utility model discloses a through retrieving the mother liquor, effectively strengthened the utilization ratio of raw and other materials, practiced thrift the manufacturing cost who prepares 5-nitrofurfural diacetate to a great extent. However, in actual production, the one-time addition of concentrated sulfuric acid consumes a part of raw materials or reagents.

Disclosure of Invention

In order to solve the technical problem, the utility model provides a production device of 5-nitrofurfural diacetate, which overcomes the problem that the raw materials are lost by adopting sulfuric acid and has low environmental pollution.

The scheme of the utility model is that:

the utility model provides a production device of 5-nitrofurfural diacetate, includes reation kettle, reation kettle pan feeding mouth communicate respectively with furfural storage tank, acetic anhydride storage tank and cobalt methane sulfonate storage tank, reation kettle bottom discharge gate passes through the pipeline and communicates with vacuum filter, and vacuum filter's filter residue discharge gate is through conveying mechanism and dissolving tank intercommunication, dissolving tank bottom organic phase discharge tube passes through the pipeline and communicates in proper order with first adsorber and second adsorber, and second adsorber filtrating discharge gate passes through the pipeline and communicates with the desicator, the dissolving tank is equipped with 1, 2 dichloroethane pan feeding pipe.

Preferably, the filler layer inside the first adsorber and the second adsorber is saturated sodium carbonate.

Preferably, the filler layer filler in the dryer is anhydrous sulfuric acid.

Further preferably, the discharge port of the dryer is communicated with the distillation still through a pipeline, a rectifying tower is arranged above the distillation still, the discharge port of the top of the rectifying tower is communicated with a condenser, the discharge port of the condenser is communicated with a first collecting tank and a second collecting tank through pipelines respectively, and the tops of the first collecting tank and the second collecting tank are communicated with a vacuum pump through pipelines respectively.

Still further preferably, the bottom discharge port of the distillation still communicates with the recrystallization tank through a pipe.

Still further preferably, the recrystallization tank is provided with a cyclohexane feeding pipe.

The utility model discloses beneficial effect:

1. the utility model discloses an adopt the green novel catalyst of cobalt methane sulfonate to and the super acid of constituteing by the acetic acid catalysis system altogether, in reaction process, need not add other solvents again, the acetic acid makes the activity of catalyst obtain very big improvement, reaction time shortens, still can reduce the catalyst quantity, the quantity is at the 0.9mol% of furfural, and the acetic acid has also overcome the problem that adopts sulphuric acid can lose the raw materials, low to environmental pollution, in the aftertreatment process, only need wash organic phase, the drying that anhydrates, the distillation, recrystallization can.

2. The filler layers in the first adsorber and the second adsorber are provided with a saturated sodium carbonate inlet and a saturated sodium carbonate outlet, and can be used for adsorbing impurities and a part of water phase. Anhydrous sodium sulfate in a desiccator was used to dry the organic phase.

3. The distillation still top is equipped with the rectifying column, rectifying column top discharge gate and condenser intercommunication, the condenser discharge gate is respectively through pipeline and first holding vessel and second holding vessel intercommunication, and pipeline and vacuum pump intercommunication are passed through respectively to first holding vessel and second holding vessel top, adopt the reduced pressure distillation mode, retrieve solvent 1, 2 dichloroethane in the organic phase.

4. The discharge outlet at the bottom of the distillation kettle is communicated with a recrystallization tank through a pipeline, and the recrystallization tank is provided with a cyclohexane feeding pipe for carrying out recrystallization purification treatment on the product.

Drawings

FIG. 1 is a schematic view of the apparatus of the present invention;

wherein: the device comprises a reaction kettle 1, a furfural storage tank 2, an acetic anhydride storage tank 3, a cobalt methane sulfonate storage tank 4, a vacuum filter 5, a dissolving tank 6, a first adsorber 7, a second adsorber 8, a dryer 9, a 1, 2 dichloroethane feeding pipe 601, a first adsorber 7, a second adsorber 8, a dryer 9, a distillation kettle 10, a rectifying tower 11, a condenser 12, a first collecting tank 13, a second collecting tank 14, a vacuum pump 15, a recrystallization tank 16 and a cyclohexane feeding pipe 1601.

Detailed Description

The invention is further described with reference to the following examples, but the scope of the invention as claimed is not limited to the scope of the examples.

Example 1

The utility model provides a production device of 5-nitrofurfural diacetate, includes reation kettle 1, 1 pan feeding mouth of reation kettle communicates respectively with furfural storage tank 2, acetic anhydride storage tank 3 and cobalt methane sulfonate storage tank 4 respectively, 1 bottom discharge gate of reation kettle passes through pipeline and 5 intercommunications of vacuum filter, and 5's filter residue discharge gate of vacuum filter communicates with dissolving tank 6 through conveying mechanism, 6 bottom organic phase discharge tubes of dissolving tank communicate through pipeline and first adsorber 7 and second adsorber 8 in proper order, and 8 filtrating discharge gates of second adsorber pass through pipeline and desicator 9 intercommunication, dissolving tank 6 is equipped with 1, 2 dichloroethane pan feeding pipe 601.

Preferably, the inner packing layers of the first adsorber 7 and the second adsorber 8 are provided with a saturated sodium carbonate inlet and outlet.

Preferably, a filling layer inside the dryer 9 is provided with an anhydrous sodium sulfate feeding port and a discharging port.

Further preferably, the discharge port of the dryer 9 is communicated with the distillation still 10 through a pipeline, a rectifying tower 11 is arranged above the distillation still 10, the discharge port at the top of the rectifying tower 11 is communicated with a condenser 12, the discharge port of the condenser 12 is communicated with a first collecting tank 13 and a second collecting tank 14 through pipelines respectively, and the tops of the first collecting tank 13 and the second collecting tank 14 are communicated with a vacuum pump 15 through pipelines respectively.

Still more preferably, the discharge port at the bottom of the distillation still 10 is communicated with the recrystallization tank 16 through a pipe.

Still more preferably, the recrystallization tank 16 is provided with a cyclohexane feeding pipe 1601.

The utility model discloses during the use: adding furfural, acetic anhydride, acetic acid and cobalt methanesulfonate into a reaction kettle 1, wherein the molar ratio of furfural to acetic anhydride to acetic acid to cobalt methanesulfonate is (25-35): (40-50): 15-20): 0.24-0.26, stirring and reacting at 15-25 ℃ for 0.5-1 hour, separating out solid after the reaction is finished, filtering in a vacuum filter 5 to remove filtrate, adding filter residue into a dissolving tank 6, adding 1, 2-dichloroethane to dissolve the filter residue to obtain an organic phase, sequentially adding the obtained organic phase into a first adsorber 7 and a second adsorber 8, washing twice with saturated sodium carbonate, and then adding into a dryer 9 to use anhydrous Na₂SO₄Drying and adsorbing, feeding the dried organic phase into a distillation kettle 10, and distilling the solvent to obtain a crude product. And (3) feeding the solid crude product obtained from the distillation kettle 10 into a recrystallization tank 16, adding cyclohexane for recrystallization to obtain a 5-nitrofurfural diacetate product, wherein the yield is more than 92%.

The above-mentioned embodiments only represent the preferred embodiments of the present invention, and the description thereof is more specific and detailed, but not to be construed as limiting the scope of the present invention. It should be noted that, for those skilled in the art, without departing from the spirit of the present invention, several changes, modifications and substitutions can be made, which are all within the scope of the present invention. Therefore, the protection scope of the present invention should be subject to the appended claims.

Claims (6)

1. The utility model provides a production facility of 5-nitrofurfural diacetate, includes reation kettle (1), its characterized in that: the feed inlet of the reaction kettle (1) is respectively communicated with the furfural storage tank (2), the acetic anhydride storage tank (3) and the cobalt methane sulfonate storage tank (4), the bottom discharge outlet of the reaction kettle (1) is communicated with the vacuum filter (5) through a pipeline, the filter residue discharge outlet of the vacuum filter (5) is communicated with the dissolving tank (6) through a conveying mechanism, the organic phase discharge pipe at the bottom of the dissolving tank (6) is sequentially communicated with the first adsorber (7) and the second adsorber (8) through a pipeline, the filtrate discharge outlet of the second adsorber (8) is communicated with the dryer (9) through a pipeline, and the dissolving tank (6) is provided with a 1, 2-dichloroethane feed pipe (601).

2. The apparatus for producing 5-nitrofurfural diacetate according to claim 1, characterized in that: and the filler of the internal packing layers of the first adsorber (7) and the second adsorber (8) is saturated sodium carbonate.

3. The apparatus for producing 5-nitrofurfural diacetate according to claim 1, characterized in that: the filler of the filler layer in the dryer (9) is anhydrous sulfuric acid.

4. The apparatus for producing 5-nitrofurfural diacetate according to claim 3, characterized in that: the discharge hole of the dryer (9) is communicated with the distillation kettle (10) through a pipeline, a rectifying tower (11) is arranged above the distillation kettle (10), the discharge hole of the top of the rectifying tower (11) is communicated with a condenser (12), the discharge hole of the condenser (12) is communicated with a first collecting tank (13) and a second collecting tank (14) through pipelines respectively, and the tops of the first collecting tank (13) and the second collecting tank (14) are communicated with a vacuum pump (15) through pipelines respectively.

5. The apparatus for producing 5-nitrofurfural diacetate according to claim 4, characterized in that: and a discharge outlet at the bottom of the distillation kettle (10) is communicated with the recrystallization tank (16) through a pipeline.

6. The apparatus for producing 5-nitrofurfural diacetate according to claim 5, characterized in that: the recrystallization tank (16) is provided with a cyclohexane feeding pipe (1601).

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