CN217025827U - Ethyl cyanoacetate byproduct purification device - Google Patents
Ethyl cyanoacetate byproduct purification device Download PDFInfo
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- CN217025827U CN217025827U CN202220240101.6U CN202220240101U CN217025827U CN 217025827 U CN217025827 U CN 217025827U CN 202220240101 U CN202220240101 U CN 202220240101U CN 217025827 U CN217025827 U CN 217025827U
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Abstract
The utility model provides a purifying device for ethyl cyanoacetate byproducts, which comprises a first distillation tower, a first condenser, a second distillation tower and a second condenser which are sequentially communicated, wherein the first distillation tower is also communicated with an alkali liquor storage tank, and a conveying pump is arranged between the first condenser and the second distillation tower. The utility model provides a purifying device for ethyl cyanoacetate by-products, aiming at reducing the acidity of purified crude alcohol and avoiding damaging the cyanoacetic acid in the crude alcohol.
Description
Technical Field
The utility model belongs to the technical field of ethanol recovery, and particularly relates to a device for purifying ethyl cyanoacetate by-products.
Background
Ethyl cyanoacetate is an important pharmaceutical intermediate, and is widely used for synthesizing compounds such as esters, amides, acids and the like. The production process mainly adopts cyanoacetic acid and ethanol to carry out esterification reaction under the catalysis of sulfuric acid to generate ethyl cyanoacetate and water. In the esterification process, the water generated in the reaction needs to be continuously removed to ensure the smooth proceeding of the esterification reaction. During the distillation of water, a large amount of ethanol is also distilled out, and a byproduct, namely crude alcohol, is generated, wherein the main component of the crude alcohol is a mixture of water and ethanol. The crude alcohol as a by-product has a water content of about 30%, an ethanol content of about 70%, and a high acidity.
Because the crude alcohol contains acidic substances, if the purification treatment is directly carried out by adopting a molecular sieve pervaporation membrane, silicate in the molecular sieve is easily corroded, and the service life of the molecular sieve is influenced. If the neutralization reaction is carried out by adding alkali liquor to the crude alcohol, the alkali liquor will destroy the cyanoacetic acid component contained in the crude alcohol and will increase the water content in the crude alcohol.
SUMMERY OF THE UTILITY MODEL
The utility model aims to provide a device for purifying ethyl cyanoacetate byproducts, which aims to reduce the acidity of purified crude alcohol and avoid damaging the cyanoacetic acid component in the crude alcohol.
In order to achieve the purpose, the utility model adopts the technical scheme that: the utility model provides an ethyl cyanoacetate byproduct purification device, including first distillation column, first condenser, second distillation column and the second condenser that communicates in proper order, first distillation column still communicates with the alkali lye storage tank, be equipped with the delivery pump between first condenser and the second distillation column.
In one possible implementation, a first buffer tank is arranged between the first condenser and the second distillation column.
In a possible implementation manner, the ethyl cyanoacetate byproduct purification device further comprises an ethanol storage tank communicated with the discharge end of the second condenser, and an esterification tank communicated with the feed inlet of the first distillation tower, wherein a discharge outlet of the ethanol storage tank is communicated with the feed inlet of the esterification tank.
In a possible implementation manner, a second buffer tank is arranged between the second condenser and the ethanol storage tank.
In a possible implementation manner, the air outlet of the second buffer tank is connected with an absorption tank.
In one possible implementation, the discharge ports of the first distillation column and the second distillation column are respectively communicated with a treatment tank, and the treatment tanks are used for treating residues discharged from the first distillation column and the second distillation column.
In a possible implementation manner, a pH detector is arranged between the first condenser and the second distillation tower.
In a possible implementation manner, an atomization assembly is arranged in the first distillation tower, and the atomization assembly is communicated with the alkali liquor storage tank.
In one possible implementation, a separation packing is arranged in the second distillation column, and the separation packing is used for adsorbing moisture.
In a possible implementation manner, a jacket is arranged outside the esterification tank, the jacket is provided with an inlet and an outlet, and the jacket is used for accommodating a heating medium.
The purification device for the ethyl cyanoacetate byproduct provided by the utility model has the beneficial effects that: compared with the prior art, the ethyl cyanoacetate byproduct purification device has the advantages that the crude alcohol after the esterification reaction is introduced into the first distillation tower, the liquid alkali in the alkali liquor storage tank is introduced into the first distillation tower to react with the acidic substances in the crude alcohol, and the liquid alkali is used for adjusting the pH value of the crude alcohol and reducing the acidity of the crude alcohol. Simultaneously, evaporating water and ethanol in the crude alcohol at high temperature in a first distillation tower to primarily reduce the water content in the ethanol, leaving residues and high-boiling-point substances after acid substances in the crude alcohol react with liquid caustic soda at the bottom of the first distillation tower, and introducing the vaporized ethanol and water into a first condenser for condensation and liquefaction. And the liquefied mixture of water and ethanol enters a second distillation tank for further distillation to reduce the water content of the ethanol, high-boiling-point substances in the mixture are retained at the bottom of the second distillation tank, and then the separated ethanol is introduced into a second condenser for condensation and liquefaction. The method firstly decomposes the acidic substances in the crude alcohol to reduce the acidity of the crude alcohol, then removes residues in the crude alcohol by twice distillation, simultaneously distills out water in the ethanol, reduces the water content of the ethanol, improves the purity of the ethanol, avoids destroying cyanoacetic acid in the crude alcohol, and realizes the recycling of the ethanol.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the drawings needed for the embodiments or the prior art descriptions will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings without creative efforts.
Fig. 1 is a schematic structural diagram of an apparatus for purifying ethyl cyanoacetate by-product according to an embodiment of the present invention.
In the figure: 1. an esterification tank; 101. a jacket; 2. a first distillation column; 201. an atomizing assembly; 3. a first condenser; 4. a pH detector; 5. a first buffer tank; 6. a delivery pump; 7. a second distillation column; 8. a second condenser; 9. a second buffer tank; 10. an ethanol storage tank; 11. a treatment tank; 12 an absorption tank.
Detailed Description
In order to make the technical problems, technical solutions and advantageous effects to be solved by the present invention more clearly apparent, the present invention is further described in detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the utility model and do not limit the utility model.
Referring to fig. 1, a purification apparatus for ethyl cyanoacetate byproduct according to the present invention will now be described. The ethyl cyanoacetate byproduct purification device comprises a first distillation tower 2, a first condenser 3, a second distillation tower 7 and a second condenser 8 which are sequentially communicated, wherein the first distillation tower 2 is also communicated with an alkali liquor storage tank, and a delivery pump 6 is arranged between the first condenser 3 and the second distillation tower 7.
Compared with the prior art, the ethyl cyanoacetate byproduct purification device provided by the utility model has the advantages that crude alcohol after esterification reaction is introduced into the first distillation tower 2, liquid alkali in the alkali liquor storage tank is introduced into the first distillation tower 2 to react with acidic substances in the crude alcohol, and the liquid alkali is used for adjusting the pH value of the crude alcohol and reducing the acidity of the crude alcohol. Meanwhile, water and ethanol in the crude alcohol are evaporated at high temperature in the first distillation tower 2, the water content in the ethanol is initially reduced, residues and high-boiling point substances after the acid substances in the crude alcohol react with the liquid caustic soda are left at the bottom of the first distillation tower 2, and the vaporized ethanol and water are introduced into a first condenser 3 for condensation and liquefaction. And the liquefied mixture of water and ethanol enters a second distillation tank for further distillation to reduce the water content of the ethanol, high-boiling-point substances in the mixture are reserved at the bottom of the second distillation tank, and then the separated ethanol is introduced into a second condenser 8 for condensation and liquefaction. The method comprises the steps of decomposing acidic substances in the crude alcohol, reducing the acidity of the crude alcohol, removing residues in the crude alcohol by twice distillation, distilling water in the ethanol, reducing the water content of the ethanol, improving the purity of the ethanol, avoiding damaging cyanoacetic acid in the crude alcohol, and recycling the ethanol.
The water content of the crude alcohol after completion of the distillation in the first distillation column 2 was 10 to 15%, and the water content of the crude alcohol after completion of the distillation in the second distillation column 7 was 2 to 5%.
In particular, the delivery pump 6 is a material-beating pump.
In some embodiments, referring to fig. 1, a first buffer tank 5 is disposed between the first condenser 3 and the second distillation column 7.
In this embodiment, the mixture of water and ethanol condensed and liquefied by the condenser enters the first buffer tank 5 for temporary storage, and the first buffer tank 5 can prevent the transfer pump 6 from idling, so that the service life of the transfer pump 6 is prolonged.
In some embodiments, referring to fig. 1, the apparatus for purifying ethyl cyanoacetate by-product further includes an ethanol storage tank 10 communicated with the discharge end of the second condenser 8, and an esterification tank 1 communicated with the feed inlet of the first distillation column 2, wherein the discharge port of the ethanol storage tank 10 is communicated with the feed inlet of the esterification tank 1.
The crude alcohol is distilled twice to obtain purified alcohol, the alcohol is liquefied under the action of a second condenser 8, and the purified alcohol enters an alcohol storage tank 10 for temporary storage. Ethanol in the ethanol storage tank 10 is introduced into the esterification tank 1 to be used as a raw material to react with cyanoacetic acid to produce ethyl cyanoacetate, so that the cyclic utilization of the ethanol is realized, and the production cost is reduced. The scheme in this embodiment can directly let in ethanol in esterification tank 1, has improved production efficiency, and the crude alcohol in esterification tank 1 also can directly let in first distillation tower 2 and carry out the distillation reaction, has reduced intermediate link, and whole system compact structure occupies a small space, has realized continuous production.
In some embodiments, referring to fig. 1, a second buffer tank 9 is disposed between the second condenser 8 and the ethanol storage tank 10.
The ethanol liquefied by the second condenser 8 enters the second buffer tank 9 for temporary storage, so that the phenomenon that the uncondensed ethanol vapor is over-high in pressure and directly enters the ethanol storage tank 10 to easily damage the ethanol storage tank 10 is avoided.
In some embodiments, referring to fig. 1, the outlet of the second buffer tank 9 is connected to an absorption tank 12.
The uncondensed ethanol enters the second buffer tank 9 along with the liquid ethanol, and the ethanol vapor is introduced into the absorption tank 12 for absorption. The absorption tank 12 can regulate the pressure in the system and simultaneously avoid environmental pollution caused by direct discharge of primary steam.
In some embodiments, referring to fig. 1, the discharge ports of the first distillation column 2 and the second distillation column 7 are respectively communicated with a treatment tank 11, and the treatment tank 11 is used for treating the residue discharged from the first distillation column 2 and the second distillation column 7.
Introducing the high boiling point residues in the first distillation tower 2 and the second distillation tower 7 into a treatment tank 11 respectively, adding an acidic substance into the treatment tank 11 to make the residues in the treatment tank 11 acidic, and then performing negative pressure dehydration and desalination treatment on the acidic residues in the treatment tank 11. The structure in the embodiment is mainly to treat the high boiling point substances in the first distillation tower 2 and the second distillation tower 7, and the treated substances can be recycled in the esterification tank 1, so that the raw materials are saved.
In some embodiments, referring to fig. 1, a PH detector 4 is disposed between the first condenser 3 and the second distillation column 7.
The pH detector 4 detects the pH of the hydrous ethanol liquefied by the first condenser 3, and the pH value of the hydrous ethanol detected by the pH detector 4 is 7-8, so that the neutralized crude alcohol in the first distillation tower 2 is ensured to be neutral.
In some embodiments, referring to fig. 1, an atomizing assembly 201 is disposed in the first distillation tower 2, and the atomizing assembly 201 is connected to the lye storage tank.
The liquid caustic soda in the lye storage tank sprays the liquid caustic soda into the first distillation tower 2 through the atomizing assembly 201, and the atomized liquid caustic soda can fully react with the acidic substances in the crude alcohol, so that the contact area between the atomized liquid caustic soda and the acidic substances is increased, and the reaction efficiency is improved.
In some embodiments, referring to fig. 1, the second distillation column 7 is provided with a separation packing for adsorbing moisture.
The separation filler can absorb the water in the hydrous ethanol, further reduce the water content in the ethanol and improve the purity of the ethanol.
Optionally, the separation filler is a ceramic corrugated filler, and the ceramic corrugated filler has large flux, good physical property, good corrosion resistance and good high temperature resistance.
In some embodiments, referring to fig. 1, the esterification tank 1 is externally provided with a jacket 101, the jacket 101 has an inlet and an outlet, and the jacket 101 is used for accommodating a heating medium.
Heating medium gets into in the jacket 101 from the feeding, produces the heat exchange to the material in the jar 1 of esterifying to flow out of jacket 101 by the export, heating medium continuously gets into in the jacket 101, can effectively heat the material in the jar 1 of esterifying, and efficiency is higher.
Optionally, the heating medium is high temperature steam.
Optionally, a stirring component is further disposed in the esterification tank 1, and is used for accelerating the reaction between the crude alcohol and the liquid caustic soda.
Optionally, a first temperature detection assembly is arranged in the first distillation tower 2, and the temperature of the tower kettle of the first distillation tower 2 is controlled to be 120 ℃, the temperature in the tower is controlled to be 90-100 ℃, the temperature of the tower top is controlled to be 80-90 ℃, the content of the alcohol extracted from the tower top is controlled to be 85-90%, and the moisture is controlled to be 10-15%.
Optionally, a second temperature detection component is arranged in the second distillation tower 7, and the temperature of the tower kettle of the second distillation tower 7 is controlled to be 110-.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the utility model, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (9)
1. The device for purifying the ethyl cyanoacetate byproduct is characterized by comprising a first distillation tower, a first condenser, a second distillation tower and a second condenser which are sequentially communicated, wherein the first distillation tower is also communicated with an alkali liquor storage tank, and a delivery pump is arranged between the first condenser and the second distillation tower;
still include with the ethanol storage tank of the discharge end intercommunication of second condenser, and with the jar of esterifying of the feed inlet intercommunication of first distillation column, the discharge gate of ethanol storage tank with the feed inlet intercommunication of jar of esterifying.
2. The apparatus of claim 1, wherein a first buffer tank is disposed between the first condenser and the second distillation column.
3. The apparatus of claim 1, wherein a second buffer tank is disposed between the second condenser and the ethanol storage tank.
4. The apparatus for purifying ethyl cyanoacetate by-product as set forth in claim 3, wherein the second buffer tank is connected to the absorption tank at its outlet.
5. The apparatus for purifying ethyl cyanoacetate byproduct as defined in claim 1, wherein the discharge ports of the first distillation column and the second distillation column are respectively connected to a treatment tank for treating the residue discharged from the first distillation column and the second distillation column.
6. The apparatus of claim 1, wherein a PH detector is disposed between the first condenser and the second distillation column.
7. The apparatus of claim 1, wherein the first distillation tower is provided with an atomization assembly, and the atomization assembly is communicated with the lye storage tank.
8. The apparatus for purifying ethyl cyanoacetate byproduct as set forth in claim 1, wherein a separation packing for adsorbing moisture is provided in the second distillation column.
9. The apparatus for purifying ethyl cyanoacetate byproduct as claimed in claim 1, wherein the esterification tank is externally provided with a jacket having an inlet and an outlet, the jacket being adapted to receive a heating medium.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202220240101.6U CN217025827U (en) | 2022-01-28 | 2022-01-28 | Ethyl cyanoacetate byproduct purification device |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202220240101.6U CN217025827U (en) | 2022-01-28 | 2022-01-28 | Ethyl cyanoacetate byproduct purification device |
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| Publication Number | Publication Date |
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| CN217025827U true CN217025827U (en) | 2022-07-22 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN202220240101.6U Active CN217025827U (en) | 2022-01-28 | 2022-01-28 | Ethyl cyanoacetate byproduct purification device |
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