CN218422814U - Production system of ethyl benzoate - Google Patents
Production system of ethyl benzoate Download PDFInfo
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- CN218422814U CN218422814U CN202222888301.5U CN202222888301U CN218422814U CN 218422814 U CN218422814 U CN 218422814U CN 202222888301 U CN202222888301 U CN 202222888301U CN 218422814 U CN218422814 U CN 218422814U
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Abstract
The utility model discloses a production system of ethyl benzoate, which comprises a reaction kettle, wherein the top of the reaction kettle is provided with an exhaust port, the lower part or the bottom of the reaction kettle is provided with an ethanol inlet and a nitrogen inlet, and the top of the inner cavity of the reaction kettle is provided with at least one spray head; the sprayer is connected with the benzoyl chloride storage tank, the ethanol inlet is connected with the vaporization tank, the vaporization tank is connected with the ethanol storage tank, the exhaust port is connected with the gas absorption tank, the gas absorption tank is connected with the nitrogen buffer tank through the nitrogen compressor, and the gas outlet of the nitrogen buffer tank is connected with the nitrogen inlet of the reaction kettle. Production system novel structure, with ethanol with gaseous form let in reation kettle in succession, benzoyl chloride spouts reation kettle in succession with the form of spraying, two raw materialss reverse contact in reation kettle, contact more fully, very big reduction reaction time, reduced impurity and generated, improved raw materials conversion.
Description
Technical Field
The utility model relates to a production system of ethyl benzoate, concretely relates to adopt continuous feeding mode, need not catalyst and solvent and participate in production system of ethyl benzoate of reaction belongs to ethyl benzoate production system technical field.
Background
The ethyl benzoate is an organic compound with a molecular formula of C 9 H 10 O 2 The product is colorless transparent liquid, is miscible with ethanol, diethyl ether, petroleum ether, propylene glycol, chloroform, mineral oil and most nonvolatile oil, is insoluble in glycerol, and is naturally present in fructus Persicae, fructus Ananadis Comosi, currant, and black tea. The ethyl benzoate has wide application range, is used for preparing essence, is also used as a solvent of cellulose ester, cellulose ether, resin and the like, is used as a solvent and a perfume auxiliary agent, is a common organic synthesis intermediate, is also used for organic synthesis, has the fragrance of wintergreen oil and cushaw oil, is smooth and sweet in flavor. Can be used for preparing artificial cananga oil and evening primrose oil. Can be used in small amount for edible essence, tobacco and edible berry essence, and can also be used as solvent for cellulose ester, cellulose ether and resins.
At present, the common preparation method of ethyl benzoate in industry is as follows: benzoic acid and ethanol are esterified under the catalysis of sulfuric acid to generate the compound with the following reaction formula. The reaction device adopted by the method is a common reaction kettle, raw materials are added into the kettle at one time for reaction, the wastewater amount is large, the pollution is serious, and in addition, because the method usually uses strong acid such as sulfuric acid, the corrosion of equipment can be serious.
In addition, the method is a liquid-liquid reaction, continuous stirring is needed to ensure that the raw materials are fully contacted, the reaction time needs eight hours to finish the reaction, the production efficiency is seriously influenced, impurities are increased, and the reaction conversion rate is reduced.
SUMMERY OF THE UTILITY MODEL
The utility model provides a not enough to prior art exists, the utility model provides a production system of ethyl benzoate, this production system improve the feeding mode of raw materials, have avoided the joining of catalyst and solvent, and the reaction is more quick, has easy and simple to handle, reduces reaction time, saves the advantage of cost to the conversion rate and the yield of product are also higher.
The utility model discloses specific technical scheme as follows:
a production system of ethyl benzoate comprises a reaction kettle, wherein an exhaust port is formed in the top of the reaction kettle, an ethanol inlet and a nitrogen inlet are formed in the lower part or the bottom of the reaction kettle, and at least one spray head is arranged at the top of an inner cavity of the reaction kettle; the sprayer is connected with the benzoyl chloride storage tank, the ethanol inlet is connected with the vaporization tank, the vaporization tank is connected with the ethanol storage tank, the exhaust port is connected with the gas absorption tank, the gas absorption tank is connected with the nitrogen buffer tank through the nitrogen compressor, and the gas outlet of the nitrogen buffer tank is connected with the nitrogen inlet of the reaction kettle.
Further, the bottom of the reaction kettle is also provided with a discharge port, the discharge port is connected with a feed inlet of the reaction liquid storage tank, the discharge port of the reaction liquid storage tank is connected with the distillation tank, the upper part of the distillation tank is provided with an ethanol outlet, the ethanol outlet is connected with an ethanol recovery tank, the bottom of the distillation tank is provided with a product outlet, and the product outlet is connected with a product storage tank.
Furthermore, the spray heads are used for spraying the benzoyl chloride into the reaction kettle from the top of the reaction kettle in a spray mode, and the number of the spray heads can be one or two or more. Specifically, the amount of benzoyl chloride added may be adjusted.
Further, the ethanol storage tank is connected with the vaporization tank through a pipeline, and a first infusion metering pump is arranged on the pipeline and used for accurately pumping ethanol into the vaporization tank according to a specified amount.
Further, the benzoyl chloride storage tank is connected with the spray head through a pipeline, and a second infusion metering pump is arranged on the pipeline and used for pumping benzoyl chloride into the reaction kettle according to a specified flow.
Furthermore, the reaction liquid storage tank is connected with the distillation retort through a pipeline, and a third infusion metering pump is arranged on the pipeline and used for pumping the reaction liquid into the distillation retort for processing.
Further, a condenser is arranged at the top of the reaction kettle.
Further, the reaction kettle is also connected with a vacuum pump to vacuumize the reaction kettle.
Furthermore, water is filled in the gas absorption tank, the gas discharged from the gas outlet is a mixer of hydrogen chloride and nitrogen, the mixer flows through the gas absorption tank firstly to absorb the hydrogen chloride therein to be converted into hydrochloric acid, and then the residual nitrogen enters the nitrogen buffer tank through the nitrogen compressor to realize the circulation of the nitrogen.
Furthermore, a pressure gauge and a flow meter are arranged on the nitrogen buffer tank.
The utility model has the advantages of as follows:
1. the utility model discloses production system novel structure, let in reation kettle with ethanol in succession with gaseous form, benzoyl chloride spouts reation kettle in succession with the form of spraying, and two raw materialss reverse contact in reation kettle, the contact is more abundant, very big reduction reaction time, reduced impurity and generated, improved the raw materials conversion rate.
2. The utility model discloses with nitrogen gas at reation kettle inner loop, nitrogen gas can take the hydrogen chloride who generates out of reation kettle, has promoted the reaction and has gone on forward, has guaranteed thoroughly going on of reaction, and product conversion rate is high with the yield. The discharged nitrogen is absorbed by the gas absorption tank and can be sold outside, thereby avoiding the environment pollution caused by the discharge of HCl and being more environment-friendly.
3. The utility model discloses reaction system need not the participation of solvent, catalyst, has both saved the cost, has simplified the operation again, is suitable for large-scale industrial production.
Drawings
FIG. 1 is a schematic diagram of a system for producing ethyl benzoate.
In the figure, 1, an ethanol storage tank; 2. a benzoyl chloride storage tank; 3. a reaction kettle; 4. a first infusion metering pump; 5. a second infusion metering pump; 6. a reaction liquid storage tank; 7. a vaporization tank; 8. a distillation tank; 9. an ethanol recovery tank; 10. a product storage tank; 11. a third infusion metering pump; 12. a spray head; 13. a gas absorption tank; 14. a nitrogen compressor; 15. and (6) a nitrogen buffer tank.
Detailed Description
The invention will be further described with reference to the following drawings and specific examples, which are given by way of illustration only and are not intended to limit the scope of protection.
Example 1
Fig. 1 is the utility model discloses ethyl benzoate's production system's structural schematic, production system includes reation kettle, and reation kettle is inside to be a cavity, and the top of the inside cavity of reation kettle is equipped with at least one shower nozzle, the shower nozzle passes through the pipeline and links to each other with benzoyl chloride storage tank, and reation kettle's top still is equipped with the gas vent, and reation kettle's lower part or bottom still are equipped with nitrogen gas import, the gas vent links to each other with the gas absorption jar, and the gas absorption jar passes through nitrogen compressor and links to each other with nitrogen gas buffer tank, and nitrogen gas buffer tank's gas outlet links to each other with reation kettle's nitrogen gas import. An ethanol inlet is arranged at the lower part or the bottom of the reaction kettle and is connected with a vaporization tank, and the vaporization tank is connected with an ethanol storage tank. The bottom of reation kettle is equipped with the discharge gate, the discharge gate links to each other with the feed inlet of reaction liquid storage tank, and the discharge gate of reaction liquid storage tank links to each other with the retort, and the upper portion of retort is equipped with the ethanol export, the ethanol export links to each other with the ethanol recovery jar, and the bottom of retort is equipped with the product export, the product export links to each other with the product storage tank.
Furthermore, a first infusion metering pump is arranged on a pipeline connecting the ethanol storage tank and the vaporization tank and used for accurately pumping ethanol into the vaporization tank according to a specified amount, and a second infusion metering pump is arranged on a pipeline connecting the benzoyl chloride storage tank and the spray head and used for pumping the benzoyl chloride into the reaction kettle according to a specified flow rate. And a third infusion metering pump is arranged on a pipeline connecting the reaction liquid storage tank and the distillation retort and is used for pumping the reaction liquid into the distillation retort for treatment.
Furthermore, a condenser is arranged at the top of the reaction kettle, and the reaction kettle is connected with a vacuum pump.
Further, the gas absorption tank is filled with water for absorbing hydrogen chloride in the gas and converting the hydrogen chloride into hydrochloric acid. The gas after passing through the gas absorption tank is nitrogen, and enters the nitrogen buffer tank after being compressed by the nitrogen compressor, the nitrogen buffer tank is provided with a pressure gauge and a flowmeter, the outflow of the nitrogen is controlled by the flowmeter, and the nitrogen is then introduced into the reaction kettle. The gas absorption tank, nitrogen compressor, and nitrogen buffer tank may be collectively referred to as a nitrogen recycle system.
The working process of the production system is as follows: pumping ethanol into a vaporization tank by a first infusion metering pump, closing a valve after pumping a certain amount of ethanol, simultaneously starting a vacuum pump of a reaction kettle to keep the vacuum degree in the reaction kettle at 0.01-0.1 MPa, and starting a nitrogen circulating system to ensure that the nitrogen introduction speed is 0.1m 3 /h～0.4m 3 And h, opening a condenser at the top of the reaction kettle, ensuring that the temperature of the reaction kettle is 30-70 ℃, feeding gaseous ethanol into the reaction kettle from the lower part or the bottom of the reaction kettle from a vaporization tank, opening a second infusion metering pump at the moment, pumping benzoyl chloride into a spray head, spraying the benzoyl chloride into the reaction kettle in a spray manner from the spray head, starting reaction after reactants are mixed, bubbling nitrogen in the reaction kettle, fully taking away hydrogen chloride formed by the reaction, and stopping introducing the nitrogen until the alcoholysis dechlorination and dehydrogenation reactions are finished. The gas discharged from the reaction vessel was absorbed with water in a gas absorption tank, thereby converting the hydrogen chloride gas into hydrochloric acid. After the reaction is finished, the obtained reaction liquid enters a reaction liquid storage tank, is pumped into a distillation kettle by a third infusion metering pump, and excessive ethanol is distilled out of the distillation kettleAnd the condensed liquid enters an ethanol recovery tank, and the residual liquid is a product and enters a product storage tank.
Furthermore, the flow rate of the gaseous ethanol is controlled to be 90-100 kg/h, the conveying speed of the benzoyl chloride is controlled to be 270-290 kg/h, and the molar ratio of the ethanol to the benzoyl chloride is 1:0.9 to 1.1.
Example 2
The ethyl benzoate is produced by adopting the production system, and the steps are as follows:
940.2kg of benzoyl chloride and 318.2kg of ethanol are respectively pumped into a benzoyl chloride storage tank and an ethanol storage tank, and N is used after feeding is finished 2 The two reservoirs were evacuated.
The nitrogen circulation system of the reaction kettle is started to carry out nitrogen circulation, and the introduction speed of the nitrogen is 0.2m 3 And h, simultaneously starting a vacuum pump, vacuumizing the reaction kettle, and keeping the vacuum degree between 0.08 and 0.1MPa. Opening a condenser at the top of the reaction kettle, introducing ethanol into a vaporization tank, introducing the ethanol into the bottom of the reaction kettle after the ethanol is vaporized by the vaporization tank, controlling the flow rate of gaseous ethanol to be 95kg/h, then opening a discharge valve of a benzoyl chloride storage tank, spraying benzoyl chloride into the reaction kettle from a spray head at the top of the reaction kettle by using a metering pump, controlling the conveying speed of the benzoyl chloride to be 280kg/h, reacting the benzoyl chloride and the gaseous ethanol through countercurrent contact, keeping the temperature of the reaction kettle at 60 ℃, continuing to react in the reaction kettle for 4h after the feeding of the benzoyl chloride and the ethanol is finished, then, not allowing obvious acidic gas to escape, continuing to introduce nitrogen for 0.5h, stopping introducing nitrogen after the reaction is finished, and obtaining 956.8kg of ethyl benzoate with the conversion rate of raw materials of 95%.
Claims (9)
1. A production system of ethyl benzoate is characterized in that: the device comprises a reaction kettle, wherein an exhaust port is arranged at the top of the reaction kettle, an ethanol inlet and a nitrogen inlet are arranged at the lower part or the bottom of the reaction kettle, and at least one spray head is arranged at the top of an inner cavity of the reaction kettle; the device comprises a spray head, a benzoyl chloride storage tank, an ethanol inlet, a vaporization tank, an exhaust port, a nitrogen buffer tank, a nitrogen compressor, a reaction kettle and a gas absorption tank, wherein the spray head is connected with the benzoyl chloride storage tank, the ethanol inlet is connected with the vaporization tank, the vaporization tank is connected with the ethanol storage tank, the exhaust port is connected with the gas absorption tank, the gas absorption tank is connected with the nitrogen buffer tank through the nitrogen compressor, and the gas outlet of the nitrogen buffer tank is connected with the nitrogen inlet of the reaction kettle.
2. The production system of claim 1, wherein: the bottom of the reaction kettle is also provided with a discharge port, the discharge port is connected with a feed inlet of the reaction liquid storage tank, the discharge port of the reaction liquid storage tank is connected with a distillation tank, the upper part of the distillation tank is provided with an ethanol outlet, the ethanol outlet is connected with an ethanol recovery tank, the bottom of the distillation tank is provided with a product outlet, and the product outlet is connected with a product storage tank.
3. The production system according to claim 1 or 2, wherein: the ethanol storage tank is connected with the vaporization tank through a pipeline, and a first infusion metering pump is arranged on the pipeline.
4. The production system according to claim 1 or 2, wherein: the benzoyl chloride storage tank is connected with the spray head through a pipeline, and a second infusion metering pump is arranged on the pipeline.
5. The production system according to claim 1 or 2, wherein: the reaction liquid storage tank is connected with the distillation tank through a pipeline, and a third infusion metering pump is arranged on the pipeline.
6. The production system of claim 1, wherein: the top of the reaction kettle is also provided with a condenser.
7. The production system of claim 1, 2 or 6, wherein: the reaction kettle is connected with a vacuum pump.
8. The production system of claim 1, 2 or 6, wherein: the gas absorption tank is filled with water.
9. The production system of claim 1, 2 or 6, wherein: and a pressure gauge and a flowmeter are arranged on the nitrogen buffer tank.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202222888301.5U CN218422814U (en) | 2022-11-01 | 2022-11-01 | Production system of ethyl benzoate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202222888301.5U CN218422814U (en) | 2022-11-01 | 2022-11-01 | Production system of ethyl benzoate |
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| Publication Number | Publication Date |
|---|---|
| CN218422814U true CN218422814U (en) | 2023-02-03 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN202222888301.5U Active CN218422814U (en) | 2022-11-01 | 2022-11-01 | Production system of ethyl benzoate |
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| CN (1) | CN218422814U (en) |
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- 2022-11-01 CN CN202222888301.5U patent/CN218422814U/en active Active
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