CN209810143U - Low boiling point alcohol continuous esterification reaction rectification system - Google Patents
Low boiling point alcohol continuous esterification reaction rectification system Download PDFInfo
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- CN209810143U CN209810143U CN201920508986.1U CN201920508986U CN209810143U CN 209810143 U CN209810143 U CN 209810143U CN 201920508986 U CN201920508986 U CN 201920508986U CN 209810143 U CN209810143 U CN 209810143U
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Abstract
The utility model belongs to the technical field of fine chemical synthesis technology, a low boiling point alcohol continuous esterification reaction rectification system is provided. The utility model discloses in the esterification reaction in-process of low boiling point alcohol, get into the continuous gasification of alcohol at esterification tower stripping section middle part, with carboxylic acid, the abundant mass transfer heat transfer of sulfuric acid catalyst, take place esterification, and carry out the mass transfer in each rectification theoretical plate through alcohol, the heat transfer shifts out the water that the reaction generated from the top of the tower, crude ester obtains and continuously adopts at the tower cauldron, realized continuous production and dewatering in tower equipment, promote product yield and raw materials conversion rate, the cost is reduced by a wide margin. The alcohol-water mixture carried out from the top of the esterification tower is further separated by a rectifying tower, and ethanol is extracted from the top of the tower, so that the recycling of the alcohol is realized. And continuously neutralizing and centrifugally separating the crude esterified product, and finally realizing continuous post-treatment of the product by an organic phase obtained by separation through a product rectifying tower.
Description
Technical Field
The utility model belongs to the technical field of fine chemical synthesis technology, concretely relates to low boiling point alcohol continuous esterification reaction rectification system.
Background
The esterification reaction of organic matter containing carboxylic acid and organic matter containing alcohol is important reaction in organic synthesis and is the main method for synthesizing ester product, the carboxylic acid organic matter and alcohol are used for esterification reaction under the catalysis of catalyst in the reaction process, and the esterification reaction is a reversible reaction, and has balanced conversion rate, low conversion rate and incomplete reaction of raw materials, so that the industrial high-temperature distillation is generally used for removing water in reaction products and improving the conversion rate of reactants.
However, for esterification of low boiling point alcohols, such as methanol and ethanol, the alcohol raw material azeotropes with water during the distillation and water removal process, and the raw material alcohol is evaporated while removing water, so that the improvement of the conversion rate of the raw material cannot be realized.
The existing esterification process is realized in a reaction kettle in an intermittent reaction mode, and has the problems of low production efficiency, high cost and the like.
In the existing esterification process adopting concentrated sulfuric acid as a catalyst, residual concentrated sulfuric acid after reaction is neutralized by inorganic alkali such as sodium hydroxide and ammonia water, an organic phase is separated after the reaction and is rectified to obtain a product, and the reaction process usually adopts an intermittent treatment mode, so that the treatment period is long and the cost is high.
SUMMERY OF THE UTILITY MODEL
To the problem that present low boiling point alcohol esterification reaction process conversion rate is low, can't realize serialization, the utility model provides a low boiling point alcohol is esterification reaction rectification system and technology in succession, it can effectively remove the water that generates in the reaction process, has realized esterification reaction's continuous going on in the packed tower, has improved esterification reaction conversion rate and yield, has reduced formation cost and manipulation strength. And realizes the continuous production of post-treatment.
The technical scheme of the utility model:
a low boiling point alcohol continuous esterification reaction rectification system comprises a crude product ester rectifying tower, a reflux tank, a sulfuric acid catalyst elevated tank, a carboxylic acid elevated tank, a catalyst-carboxylic acid mixing tank, an alcohol elevated tank, an esterification tower, a rectifying tower, an alcohol buffer tank, an alcohol storage tank, a static reactor, a centrifugal extractor and a storage tank;
the esterification tower comprises a tower kettle, a rectification reaction section and a tower top reflux section, wherein the rectification reaction section comprises a rectification section and a stripping section, fillers are arranged in the rectification section and the stripping section, and mass transfer, heat transfer and esterification reaction are carried out on carboxylic acid, alcohol and a catalyst in the fillers;
the outlet ends of the sulfuric acid catalyst elevated tank and the carboxylic acid elevated tank are communicated with the catalyst-carboxylic acid mixing tank through pipelines, and the flow rates are controlled by flow control instruments respectively; the outlet end of the catalyst-carboxylic acid mixing tank is introduced into the middle parts of the rectifying section and the stripping section of the esterification tower through pipelines; the outlet end of the alcohol head tank is introduced into the middle part of the stripping section of the esterification tower through a pipeline; the top of the esterification tower is connected with a rectifying tower 8 through a branch of a reflux tank, and the other branch of the reflux tank refluxes to the top of the esterification tower; the top of the rectifying tower is connected with an alcohol buffer tank through a branch of a reflux tank, and the other branch of the reflux tank refluxes to the top of the rectifying tower; the alcohol buffer tank is further communicated with an alcohol storage tank through a pipeline, and the alcohol storage tank is connected with the inlet end of the alcohol head tank through a pipeline; the bottom of the esterification tower is communicated with a static reactor through a pipeline, the static reactor is further communicated with a centrifugal extractor, and the centrifugal extractor is communicated with a crude ester rectifying tower through a pipeline; the top of the crude ester rectifying tower is connected with the storage tank through a branch of the reflux tank, and the other branch of the reflux tank refluxes to the top of the crude ester rectifying tower.
The utility model has the advantages that: the utility model discloses in the esterification reaction in-process of low boiling point alcohol, get into the continuous gasification of alcohol at esterification tower stripping section middle part, with carboxylic acid, the abundant mass transfer heat transfer of sulfuric acid catalyst, take place esterification, and carry out the mass transfer in each rectification theoretical plate through alcohol, the heat transfer shifts out the water that the reaction generated from the top of the tower, crude ester obtains and continuously adopts at the tower cauldron, realized continuous production and dewatering in tower equipment, promote product yield and raw materials conversion rate, the cost is reduced by a wide margin. The alcohol-water mixture carried out from the top of the esterification tower is further separated by a rectifying tower, and ethanol is extracted from the top of the tower, so that the recycling of the alcohol is realized. And continuously neutralizing and centrifugally separating the crude esterified product, and finally realizing continuous post-treatment of the product by an organic phase obtained by separation through a product rectifying tower.
Drawings
Fig. 1 is a schematic structural diagram of the present invention.
In the figure: 1, a crude ester rectifying tower; 2, a reflux tank; 3 sulfuric acid catalyst elevated tank; 4 carboxylic acid head tank; 5 catalyst-carboxylic acid mixing tank; 6 alcohol head tank; 7, an esterification tower; 8, a rectifying tower; 9 alcohol buffer tank; 10 alcohol storage tank; 11 a static reactor; 12 centrifugal extractor; 13 storage tank.
Detailed Description
The following further describes a specific embodiment of the present invention with reference to the drawings and technical solutions.
A low boiling point alcohol continuous esterification reaction rectification system comprises a crude product ester rectification tower 1, a reflux tank 2, a sulfuric acid catalyst head tank 3, a carboxylic acid head tank 4, a catalyst-carboxylic acid mixing tank 5, an alcohol head tank 6, an esterification tower 7, a rectification tower 8, an alcohol buffer tank 9, an alcohol storage tank 10, a static reactor 11, a centrifugal extractor 12 and a storage tank 13;
the esterification tower 7 comprises a tower kettle, a rectification reaction section and a tower top reflux section, wherein the rectification reaction section comprises a rectification section and a stripping section, the rectification section and the stripping section are internally provided with fillers, and the carboxylic acid, the alcohol and the catalyst are subjected to mass transfer, heat transfer and esterification reactions in the fillers;
the sulfuric acid catalyst in the sulfuric acid catalyst elevated tank 3 and the carboxylic acid in the carboxylic acid elevated tank 4 are continuously added into a catalyst-carboxylic acid mixing tank 5 according to the proportion, are fully mixed and then enter the middle parts of a rectification section and a stripping section of an esterification tower 7; introducing the alcohol in the alcohol head tank 6 into the middle part of a stripping section of an esterification tower 7 according to the molar ratio of the alcohol to the carboxylic acid of 2:1-8: 1; the bottoms of the sulfuric acid catalyst elevated tank 3, the carboxylic acid elevated tank 4, the alcohol elevated tank 6 and the catalyst-carboxylic acid mixing tank 5 are respectively provided with a flow control instrument, and the temperature of the tower kettle of the esterification tower 7 is 65-100 ℃; the material extracted from the top of the esterification tower 7 is an alcohol-water mixture, the mixture is preheated to 40-70 ℃, then a part of alcohol is introduced into the rectifying tower 8 through the reflux tank 2 for further rectification, and the other part of alcohol flows back to the interior of the esterification tower 7 from the top of the esterification tower 7; extracting the rectified alcohol from the top of the rectifying tower 8, passing through the reflux tank 2, allowing a part of the rectified alcohol to enter an alcohol buffer tank 9 and then enter an alcohol storage tank 10, and pumping the purified alcohol into an alcohol head tank 6 for recycling; the other part of the rectified alcohol flows back to the rectifying tower 8 from the top of the rectifying tower 8 to continue reacting;
neutralizing the esterified crude product obtained from the bottom of the esterification tower 7 with ammonia water in a static reactor 11 to remove sulfuric acid in the esterified crude product, continuously separating the neutralized material in a centrifugal extractor 12, feeding the separated organic matter into a crude ester rectifying tower 1, rectifying by the crude ester rectifying tower 1, and obtaining an esterified product from the top of the tower; after the esterified product passes through the reflux tank 2, one part of the esterified product enters the storage tank 13, and the other part of the esterified product enters the crude ester rectifying tower 1 from the top of the crude ester rectifying tower 1 to continuously participate in the reaction.
The alkali liquor is ammonia water or sodium hydroxide solution.
The low boiling point alcohol is methanol or ethanol.
Claims (1)
1. A low boiling point alcohol continuous esterification reaction rectification system is characterized by comprising a crude product ester rectification tower (1), a reflux tank (2), a sulfuric acid catalyst elevated tank (3), a carboxylic acid elevated tank (4), a catalyst-carboxylic acid mixing tank (5), an alcohol elevated tank (6), an esterification tower (7), a rectification tower (8), an alcohol buffer tank (9), an alcohol storage tank (10), a static reactor (11), a centrifugal extractor (12) and a storage tank (13);
the esterification tower (7) comprises a tower kettle, a rectification reaction section and a tower top reflux section, wherein the rectification reaction section comprises a rectification section and a stripping section, fillers are arranged in the rectification section and the stripping section, and mass transfer, heat transfer and esterification reaction are carried out on carboxylic acid, alcohol and a catalyst in the fillers;
the outlet ends of the sulfuric acid catalyst elevated tank (3) and the carboxylic acid elevated tank (4) are communicated with a catalyst-carboxylic acid mixing tank (5) through pipelines, and the flow rates are respectively controlled through a flow control instrument; the outlet end of the catalyst-carboxylic acid mixing tank (5) is introduced into the middle of the rectifying section and the stripping section of the esterification tower (7) through a pipeline; the outlet end of the alcohol head tank (6) is introduced into the middle part of the stripping section of the esterification tower (7) through a pipeline; the top of the esterification tower (7) is connected with the rectifying tower (8) through a branch of the reflux tank (2), and the other branch of the reflux tank (2) refluxes to the top of the esterification tower (7); the top of the rectifying tower (8) is connected with an alcohol buffer tank (9) through a branch of the reflux tank (2), and the other branch of the reflux tank (2) refluxes to the top of the rectifying tower (8); the alcohol buffer tank (9) is further communicated with an alcohol storage tank (10) through a pipeline, and the alcohol storage tank (10) is connected with the inlet end of the alcohol head tank (6) through a pipeline; the bottom of the esterification tower (7) is communicated with a static reactor (11) through a pipeline, the static reactor (11) is further communicated with a centrifugal extractor (12), and the centrifugal extractor (12) is communicated with a crude ester rectifying tower (1) through a pipeline; the top of the crude ester rectifying tower (1) is connected with the storage tank (13) through a branch of the reflux tank (2), and the other branch of the reflux tank (2) refluxes to the top of the crude ester rectifying tower (1).
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| CN201920508986.1U CN209810143U (en) | 2019-04-16 | 2019-04-16 | Low boiling point alcohol continuous esterification reaction rectification system |
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| CN201920508986.1U CN209810143U (en) | 2019-04-16 | 2019-04-16 | Low boiling point alcohol continuous esterification reaction rectification system |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113024376A (en) * | 2021-03-12 | 2021-06-25 | 润泰化学（泰兴）有限公司 | Production process of hexadecanediester |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113024376A (en) * | 2021-03-12 | 2021-06-25 | 润泰化学（泰兴）有限公司 | Production process of hexadecanediester |
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