CN216366636U - Device for recovering sodium ethoxide from organic solution of sodium ethoxide - Google Patents
Device for recovering sodium ethoxide from organic solution of sodium ethoxide Download PDFInfo
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- CN216366636U CN216366636U CN202122886210.3U CN202122886210U CN216366636U CN 216366636 U CN216366636 U CN 216366636U CN 202122886210 U CN202122886210 U CN 202122886210U CN 216366636 U CN216366636 U CN 216366636U
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Abstract
The utility model discloses a device for recovering sodium ethoxide from an organic solution of sodium ethoxide, which is characterized in that: the system comprises a falling film evaporator, a primary scraper evaporator, a secondary scraper evaporator and a plurality of rake dryers; the top of the falling-film evaporator is connected with a sodium ethoxide organic solution feed line, the falling-film evaporator is connected with a primary scraper evaporator through a feed pump, an outlet material line at the bottom of the primary scraper evaporator is connected with a secondary scraper evaporator through a feed pump, an outlet material line at the bottom of the secondary scraper evaporator is connected with a feed inlet of a feed pump of the rake dryer, an outlet material line of the feed pump of the rake dryer is connected with feed inlets at the upper parts of a plurality of rake dryers, and a sodium ethoxide solid product is obtained at the outlet material line at the bottom of the rake dryer.
Description
Technical Field
The utility model relates to the technical field of compound recovery equipment, in particular to a device for recovering sodium ethoxide from an organic solution of sodium ethoxide.
Background
Sodium ethoxide, also known as "sodium ethoxide", is one of the typical alkoxides and has the molecular formula CH3CH2ONa. Is white or light yellow powder, is easy to absorb moisture, is decomposed when exposed to air, and gradually becomes dark after being stored for a long time. Sodium ethoxide is decomposed into sodium hydroxide and ethanol when meeting water due to extremely strong instability, and shows strong basicity. Is very easy to dissolve in polar solvent (such as ethanol), the industrial product is mostly the ethanol solution of sodium ethoxide, and the ethanol can be evaporated to dryness or the sodium ethoxide is separated out to produce the sodium ethoxide solid product. Sodium ethoxide has extremely strong chemical activity, is an intermediate and a catalyst of common chemical reactions, and is commonly used in various types of organic synthesis reactions. In industry, it is mainly used for the synthesis of pharmaceutical and agrochemical products.
The industrial preparation method of sodium ethoxide is mainly divided into a metal method and an alkaline method. The metal method is to produce sodium ethoxide by directly reacting metal sodium with absolute ethyl alcohol. The method has the advantages of simple operation, low content of free alkali, high purity and the like, but the method has the defects of easy combustion of metal sodium, high production cost, unsafe production and the like, and is rarely applied to industry at present.
The alkaline process is to produce sodium ethoxide by reacting sodium hydroxide with ethanol. The method comprises the steps of dissolving solid sodium hydroxide in ethanol and pure benzene solution (or cyclohexane and ethanol solution), heating and refluxing, and continuously reacting through a tower reactor. And distilling a ternary azeotropic mixture of benzene, ethanol and water at the tower top to remove water generated in the reaction, so that the reaction is carried out in the direction of producing sodium ethoxide. And obtaining an ethanol solution of sodium ethoxide from the tower bottom, and evaporating and drying the ethanol solution of sodium ethoxide to obtain a sodium ethoxide solid. Chinese patent CN200410035561 discloses a new process for producing sodium methoxide/ethanol by an alkaline method, wherein excessive methanol/ethanol is used for reacting with sodium hydroxide, the product sodium ethoxide is produced at the bottom of a reactor, methanol/ethanol steam evaporated at the top is dehydrated by a molecular sieve, and the dehydrated methanol/ethanol can be returned to the reactor for recycling.
The sec-butyl ester is produced by sec-butyl acetate exchange reaction by adopting sodium ethoxide as a catalyst. In the production process, the reaction raw material sec-butyl acetate contains a small amount of water, acetic acid and other impurities, so that the sec-butyl acetate and sodium ethoxide undergo a side reaction to generate sodium acetate impurities. In the process of separating sodium acetate impurities in the reaction system, part of sodium ethoxide and sodium acetate form a mixture which is discharged out of the reaction system, so that part of sodium ethoxide catalyst is lost and wasted.
SUMMERY OF THE UTILITY MODEL
The utility model aims to provide a sodium ethoxide catalyst recovery device, which can effectively recover a sodium ethoxide catalyst in an organic solution of sodium ethoxide, has the advantages of convenience in operation, simple process flow and the like, and improves economic effects.
In order to achieve the purpose, the utility model adopts the following technical scheme:
a device for recovering sodium ethoxide from an organic solution of sodium ethoxide comprises a falling film evaporator, a primary scraper evaporator, a secondary scraper evaporator and a plurality of rake dryers; the top of the falling-film evaporator is connected with a sodium ethoxide organic solution feeding line, and a material extraction line of the falling-film evaporator is connected with a feeding port of a feeding pump of the first-stage scraper evaporator; the discharge gate and the first order scraper blade evaporimeter pan feeding mouth of one-level scraper blade evaporimeter charge pump are connected, first order scraper blade evaporimeter bottom export material line and second grade scraper blade evaporimeter charge pump inlet line connection, the discharge gate and the second grade scraper blade evaporimeter pan feeding mouth of second grade scraper blade evaporimeter charge pump are connected, second grade scraper blade evaporimeter bottom export material line and the harrow does quick-witted charge pump pan feeding mouth and be connected, harrow does quick-witted charge pump export material line and the pan feeding mouth on a plurality of harrow dry quick-witted upper portions and is connected, obtains the sodium ethoxide solid product at harrow dry machine bottom export material line.
Furthermore, the drying machine comprises three drying machines, wherein one drying machine is in a feeding state when in operation, and the third drying machine is in a standby state.
Further, the falling film evaporator, the first-stage scraper evaporator and the second-stage scraper evaporator are all provided with gas phase material outlet lines, and the three gas phase material outlet lines are converged to form a gas phase solvent outlet line.
Furthermore, the falling film evaporator, the primary scraper evaporator, the secondary scraper evaporator and the rake dryer are all provided with steam heating devices.
Further, a liquid distributor is arranged at the top of the falling film evaporator.
Further, when the scraper evaporator operates, the clearance between the scraper and the cylinder is about 10 mm.
Further, the falling film evaporator is provided with a circulating line.
The raw material liquid is evaporated by the falling-film evaporator, most of the solvent is evaporated, and the condition that no crystal is separated out from the material liquid to cause the blockage of the tube array of the falling-film evaporator is ensured; part of the feed liquid circulates in the falling film evaporator and part of the feed liquid is extracted to the first-stage scraper evaporator; crystals are precipitated by the first-stage scraper evaporator, but the liquid viscosity is not too high to cause pipeline blockage; the feed liquid is evaporated by the secondary scraper evaporator and then enters the rake dryer for drying, the sodium ethoxide catalyst in the organic solution of the sodium ethoxide can be effectively recovered by adopting the novel practical device, and the novel device has the advantages of convenience in operation, simple process flow and the like, and the economic effect is improved.
Drawings
FIG. 1 is a schematic view of the structure of the apparatus of the present invention.
In the drawings are labeled: the system comprises a 1-falling film evaporator, a 2-first-stage scraper evaporator, a 3-second-stage scraper evaporator, a 4-first rake dryer, a 5-second rake dryer, a 6-third rake dryer, a 7-sodium ethoxide organic solution feeding line, an 8-gas phase solvent extraction line, a 9-first-stage scraper evaporator feeding line, a 10-second-stage scraper evaporator feeding line, an 11-rake dryer feeding line, a 12-first-stage scraper evaporator feeding pump, a 13-second-stage scraper evaporator feeding pump, a 14-rake dryer feeding pump and a 15-sodium ethoxide discharging line.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, but the technical solutions do not limit the scope of the present invention.
The utility model provides a device for recovering sodium ethoxide from an organic solution of sodium ethoxide, which comprises a falling film evaporator, a primary scraper evaporator, a secondary scraper evaporator and a plurality of rake dryers, wherein the falling film evaporator is connected with the primary scraper evaporator; the top of the falling-film evaporator is connected with a sodium ethoxide organic solution feeding line, and a material extraction line of the falling-film evaporator is connected with a feeding port of a feeding pump of the first-stage scraper evaporator; the discharge gate and the first order scraper blade evaporimeter pan feeding mouth of one-level scraper blade evaporimeter charge pump are connected, first order scraper blade evaporimeter bottom export material line and second grade scraper blade evaporimeter charge pump inlet line connection, the discharge gate and the second grade scraper blade evaporimeter pan feeding mouth of second grade scraper blade evaporimeter charge pump are connected, second grade scraper blade evaporimeter bottom export material line and the harrow does quick-witted charge pump pan feeding mouth and be connected, harrow does quick-witted charge pump export material line and the pan feeding mouth on a plurality of harrow dry quick-witted upper portions and is connected, obtains the sodium ethoxide solid product at harrow dry machine bottom export material line.
Specifically, referring to fig. 1, the raw material is transported from outside the battery limits to a sodium ethoxide organic solution feed line 7 of the falling-film evaporator 1, mixed with the circulating material at the bottom of the falling-film evaporator 1, and then enters the falling-film evaporator 1 for evaporation. The falling-film evaporator 1 is used for evaporating most of the solvent, and the solvent is evaporated to the maximum extent on the premise that the column tubes of the falling-film evaporator are not blocked due to the generation of solids. The raw material firstly enters a liquid distributor at a feed inlet in the falling film evaporator 1, the liquid distributor uniformly distributes the material on a top tube plate of the falling film evaporator 1, and the liquid on the tube plate is uniformly distributed on the inner surface of each heat exchange tube by a film distributor to form a uniform liquid film. The falling film evaporator 1 is heated by steam, and the steam flows through a shell pass; in the heat exchange tube of the falling film evaporator 1, the material flows downwards uniformly along the inner surface from the top of the heat exchange tube under the action of gravity, and is heated by shell-side steam in the flowing process of the material, so that the material is gently evaporated.
The product at the bottom of the falling film evaporator 1 is fed as a feed to the primary scraped surface evaporator 2 by a primary scraped surface evaporator feed pump 12 through a primary scraped surface evaporator feed line 9. The top of the scraper evaporator is provided with a liquid distributor. The liquid distributor pre-distributes the material on the inner surface of the top shell of the scraper evaporator, and the liquid flows downwards to enter the heating section under the action of gravity. Scrapers are evenly distributed on the heating section of the scraper evaporator, the scrapers are driven by a motor to rotate along with the rotor, and the rotating rotor provides centrifugal force for the scrapers so that the scrapers are tightly attached to the inner surface of the shell. The liquid entering the heating section is driven by the scraper to roll continuously on the inner surface of the shell, and simultaneously heated by steam on the shell side, and the material begins to evaporate.
The product at the bottom of the first-stage scraper evaporator 2 enters the second-stage scraper evaporator 3 after being boosted by the feeding pump 13 of the second-stage scraper evaporator, and the material is further concentrated by the second-stage scraper evaporator 3.
Solvent outlet lines of the falling-film evaporator 1, the first-stage scraper evaporator 2 and the second-stage scraper evaporator 3 after evaporation are mixed together to be used as a gas-phase solvent extraction line 8.
The material at the bottom of the second-stage scraper evaporator 3 is fed into the parallel-connected 3 raking drying machines for drying through a raking drying machine feeding pump 14 and a raking drying machine feeding line 11, the second raking drying machine 5 feeds the material when the first raking drying machine 4 operates, and the third raking drying machine 6 is used for standby. When the material is filled to the theoretical liquid level, the material should be switched to another rake dryer for feeding. While the material is being loaded, the steam and the motor of the rake dryer are turned on to begin evaporating the solvent. After the material is filled to the theoretical liquid level, the feeding is cut off, and the material is continuously rolled by the harrow knife in the harrow dryer, thereby enhancing the heat exchange. After drying is completed, the discharge valve at the bottom is opened, and the rotor is rotated to gather the materials in the middle to discharge the materials out of the harrow dryer.
While the foregoing is directed to the preferred embodiment of the present invention, it will be understood by those skilled in the art that various changes and modifications may be made without departing from the spirit and scope of the utility model.
Claims (7)
1. A device for recovering sodium ethoxide from an organic solution of sodium ethoxide salt is characterized in that: the system comprises a falling film evaporator, a primary scraper evaporator, a secondary scraper evaporator and a plurality of rake dryers; the top of the falling-film evaporator is connected with a sodium ethoxide organic solution feeding line, and a material extraction line of the falling-film evaporator is connected with a feeding port of a feeding pump of the first-stage scraper evaporator; the discharge gate and the first order scraper blade evaporimeter pan feeding mouth of one-level scraper blade evaporimeter charge pump are connected, first order scraper blade evaporimeter bottom export material line and second grade scraper blade evaporimeter charge pump inlet line connection, the discharge gate and the second grade scraper blade evaporimeter pan feeding mouth of second grade scraper blade evaporimeter charge pump are connected, second grade scraper blade evaporimeter bottom export material line and the harrow does quick-witted charge pump pan feeding mouth and be connected, harrow does quick-witted charge pump export material line and the pan feeding mouth on a plurality of harrow dry quick-witted upper portions and is connected, obtains the sodium ethoxide solid product at harrow dry machine bottom export material line.
2. The apparatus for recovering sodium ethoxide from an organic solution of sodium ethoxide salt according to claim 1, wherein: comprises three raking and drying machines, wherein one machine is in a feeding state when running, and the third machine is in a standby state.
3. The apparatus for recovering sodium ethoxide from an organic solution of sodium ethoxide salt according to claim 1, wherein: the falling-film evaporator, the primary scraper evaporator and the secondary scraper evaporator are all provided with gas-phase material outlet lines, and the three gas-phase material outlet lines are converged to form a gas-phase solvent outlet line.
4. The apparatus for recovering sodium ethoxide from an organic solution of sodium ethoxide salt according to claim 1, wherein: and the falling film evaporator, the primary scraper evaporator, the secondary scraper evaporator and the rake dryer are all provided with steam heating devices.
5. The apparatus for recovering sodium ethoxide from an organic solution of sodium ethoxide salt according to claim 1, wherein: and a liquid distributor is arranged at the top of the falling film evaporator.
6. The apparatus for recovering sodium ethoxide from an organic solution of sodium ethoxide salt according to claim 1, wherein: when the scraper evaporator operates, the clearance between the scraper and the cylinder is about 10 mm.
7. The apparatus for recovering sodium ethoxide from an organic solution of sodium ethoxide salt according to claim 1, wherein: the falling film evaporator is provided with a circulating line.
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CN202122886210.3U CN216366636U (en) | 2021-11-23 | 2021-11-23 | Device for recovering sodium ethoxide from organic solution of sodium ethoxide |
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CN202122886210.3U CN216366636U (en) | 2021-11-23 | 2021-11-23 | Device for recovering sodium ethoxide from organic solution of sodium ethoxide |
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