CN114917836B - Hydrogenation kettle non-pressure-relief hydrogenation device and application thereof - Google Patents
Hydrogenation kettle non-pressure-relief hydrogenation device and application thereof Download PDFInfo
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- CN114917836B CN114917836B CN202110838229.2A CN202110838229A CN114917836B CN 114917836 B CN114917836 B CN 114917836B CN 202110838229 A CN202110838229 A CN 202110838229A CN 114917836 B CN114917836 B CN 114917836B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J3/00—Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
- B01J3/04—Pressure vessels, e.g. autoclaves
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J4/00—Feed or outlet devices; Feed or outlet control devices
- B01J4/02—Feed or outlet devices; Feed or outlet control devices for feeding measured, i.e. prescribed quantities of reagents
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/32—Hydrogen storage
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Abstract
The invention provides a hydrogenation device for a hydrogenation kettle without pressure relief, which comprises a high-pressure hydrogenation kettle, a high-level feeding balance groove, a high-level groove and a low-level groove, wherein the high-level feeding balance groove and the high-level groove are arranged above the high-pressure hydrogenation kettle, and the low-level groove is arranged below the high-pressure hydrogenation kettle. The device shortens the production period, does not need to exhaust and replace the hydrogenation kettle, can put into the next batch of production immediately after the material is discharged, effectively saves time and improves the productivity; the environmental pollution is reduced, and the feeding balance groove is an empty groove, so that pressure relief is carried out almost without entrainment; the consumption of hydrogen and nitrogen is reduced; the reasonable utilization amount of hydrogen in the invention is improved by 60 percent, and the nitrogen consumption is reduced by 80 percent; in addition, the device of the invention occupies a small area.
Description
Technical Field
The invention relates to the technical field of organic chemical equipment, in particular to IPC (industrial personal computer) classification number F17C5/06, and more particularly relates to a hydrogenation device without pressure relief of a hydrogenation kettle and application thereof.
Background
The catalytic hydrogenation technology is a core technology in pharmaceutical chemical industry and other organic synthesis, and has the advantages of energy conservation, consumption reduction, environmental pollution reduction and high economic benefit.
At present, an intermittent method is commonly used in the pharmaceutical and chemical industry for hydrogenation, open fire is easy to generate when high-pressure tail gas is emptied after the hydrogenation is finished, a large amount of volatile solvents can be brought out, the running risk and environmental protection pressure of enterprises are increased, and in order to cope with the risks, the productivity is often sacrificed, and the air exhaust and pressure relief time is prolonged. In addition, after intermittent hydrogenation is finished, nitrogen replacement is needed to be carried out on the hydrogenation kettle, and hydrogen is replaced by hydrogen before hydrogenation reaction is started, so that a great amount of nitrogen and hydrogen are wasted, and the running cost of enterprises is increased.
Chinese patent CN110143883a discloses a hydrogenation reaction method, which is stable in temperature control, improves product conversion rate and purity, and reduces energy consumption and has higher degree of automation. However, the method increases time and cost and reduces productivity by replacing the hydrogenation kettle with nitrogen.
Disclosure of Invention
Aiming at the defects existing in the prior art, the invention provides a hydrogenation kettle non-pressure-relief hydrogenation device, which comprises a high-pressure hydrogenation kettle 1, a high-level feeding balance tank 2, a high-level tank 3 and a low-level tank 4, wherein the high-level feeding balance tank 2 and the high-level tank 3 are arranged above the high-pressure hydrogenation kettle 1, and the low-level tank 4 is arranged below the high-pressure hydrogenation kettle 1.
In some embodiments, the high-pressure hydrogenation kettle 1 is connected with the high-level feeding balance tank 2 through a gas-phase balance pipe, and pneumatic shut-off valves are respectively arranged at two ends of the gas-phase balance pipe.
In some embodiments, a discharging pipe is arranged at the bottom of the high-level feeding balance tank 2 and is connected with a feeding hole of the high-pressure hydrogenation kettle 1.
In some embodiments, the discharge port of the high-pressure hydrogenation kettle 1 is connected with the feed port of the elevated tank 3 through a pipeline.
In some embodiments, the outlet of the upper tank 3 is connected with the inlet of the lower tank 4 through a pipeline.
In some embodiments, the non-pressure relief device further comprises a meter.
In some embodiments, the high-level feeding balance tank 2 is provided with a liquid level sensor and a pressure remote sensor, and the gas-phase balance pipe is provided with a pressure remote sensor.
In some embodiments, the autoclave 1 is provided with a temperature, pressure, oxygen content analyzer and a gas mass flow meter remote sensor.
In some embodiments, the elevated tank 3 is provided with a pressure level remote sensor and the lower tank 4 is provided with a pressure remote sensor and a hydrogen content detection remote sensor.
In some embodiments, the high-level feeding balance tank 2 has the same volume as the high-pressure hydrogenation kettle 1, and the high-level feeding balance tank 2 is used for feeding hydrogenation raw materials under high pressure.
In some embodiments, the overhead tank 3 has the same volume as the feed volume of the hydrogenation feedstock; the elevated tank 3 is used to receive the high pressure reaction and also to reduce the overall system pressure.
In some embodiments, the volume of the lower tank 4 is the same as the volume of the upper tank 3; the low-level tank is used for decompressing the pressure of the high-level tank again and replacing nitrogen for the system to achieve the purpose of safe discharging.
The working principle of the invention is as follows: pumping the hydrogenated liquid into a normal-pressure high-position feeding balance tank 2 through a pump according to the measurement of a hydrogenated liquid mass flowmeter, and opening a pneumatic cut-off valve of a gas phase balance pipe between the high-pressure hydrogenation kettle 1 with pressure and the high-position feeding balance tank 2 to balance the pressure of the two; then, a pneumatic valve for discharging from the bottom of the high-level feeding balance tank 2 is opened, the material automatically flows into the hydrogenation kettle by utilizing the gravity of the material to react, and the high-level feeding balance tank 2 is decompressed to normal pressure for standby during the reaction. After the reaction is finished, the high-pressure hydrogenation kettle 1 presses all materials into the overhead tank 3 through pressure, and the high-pressure hydrogenation kettle 1 is emptied for standby. The liquid in the upper tank 3 is discharged downwards into the lower tank 4, and the volume and the pressure of the upper space of the upper tank 3 are calculated, and the lower tank 4 with a proper volume is selected, so that the pressure of the upper tank 3 and the lower tank 4 after the discharge is finished is less than 0.2MPa (A). And when the discharging of the upper tank 3 is finished, the discharging pneumatic valve is closed, and after the nitrogen replacement of the lower tank 4 is qualified, the hydrogenated liquid enters the next working section.
The invention further provides an application of the hydrogenation kettle non-pressure-relief hydrogenation device in preparation of amide pesticides.
The beneficial effects are that:
(1) The production period is shortened, the hydrogenation kettle does not need to be exhausted and replaced, the next batch of production can be put into the process immediately after the material is discharged, the time is effectively saved, and the productivity is improved; the production time of the 3000L hydrogenation kettle can be reduced by about 2 hours, and the ignition frequency of exhaust gas is reduced by about 80 percent;
(2) The invention reduces environmental pollution, the high-pressure exhaust gas can entrain a large amount of solvent, which is serious to environmental pollution, while the charging balance groove is an empty groove, and the pressure relief is almost carried out without entrainment;
(3) The consumption of hydrogen and nitrogen is reduced; before the device is used, hydrogen in the hydrogenation kettle is directly discharged as waste gas, then the hydrogen is replaced by nitrogen and discharged, the reasonable utilization amount of the hydrogen in the device is improved by 60%, and the nitrogen consumption is reduced by 80%;
(4) The device has small occupied area, certain enterprises use the buffer tank with huge volume to decompress and balance exhaust the tail gas in order to cope with the entrainment caused by the exhaust, and the volume of the buffer tank is more than 10 times of that of the device body in order to achieve the purpose, and the device has the volume of 3-3.5 times of that of the hydrogenation kettle and is small in volume.
(5) The invention realizes the automatic control of the process by the DCS sequential control program, and almost no manual intervention is needed.
Drawings
FIG. 1 is a schematic diagram of a hydrogenation apparatus with no pressure relief for a hydrogenation kettle according to the present invention;
in the figure, 1, a high-pressure charging kettle; 2. a high-level feeding balance groove; 3. an elevated tank; 4. a lower tank; 5. a pneumatic shut-off valve; 6. a gas phase balance pipe.
Claims (6)
1. The hydrogenation kettle non-pressure-relief hydrogenation device is characterized by comprising a high-pressure hydrogenation kettle (1), a high-level feeding balance groove (2), a high-level groove (3) and a low-level groove (4), wherein the high-level feeding balance groove (2) and the high-level groove (3) are arranged above the high-pressure hydrogenation kettle (1), and the low-level groove (4) is arranged below the high-pressure hydrogenation kettle (1); the high-level feeding balance tank (2) is provided with a liquid level sensor and a pressure remote sensor, the high-pressure hydrogenation kettle (1) is connected with the high-level feeding balance tank (2) through a gas-phase balance pipe (6), two ends of the gas-phase balance pipe are respectively provided with a pneumatic cut-off valve (5), and the gas-phase balance pipe is provided with a pressure remote sensor; the high-pressure hydrogenation kettle (1) is provided with a temperature, pressure, oxygen content analyzer and a gas mass flowmeter remote sensor; the high-level tank (3) is provided with a pressure liquid level remote sensor, the low-level tank (4) is provided with a pressure remote sensor and a hydrogen content detection remote sensor, liquid in the high-level tank (3) is discharged downwards into the low-level tank (4), the low-level tank (4) with proper volume is selected through calculating the volume and the pressure of the upper space of the high-level tank (3), so that the pressure of the high-level tank (3) after the discharging of the high-level tank (4) is finished is smaller than 0.2MPa, the volumes of the high-level feeding balance tank (2) and the high-pressure hydrogenation kettle (1) are the same, the high-level feeding balance tank (2) is used for feeding hydrogenation raw materials under high pressure, the hydrogenation raw materials are pumped into the high-pressure high-level feeding balance tank (2) through a pump according to the measurement of a hydrogenated liquid mass flowmeter, and a pneumatic cut-off valve of a gas phase balance pipe between the high-pressure hydrogenation kettle (1) and the high-level feeding balance tank (2) is opened, so that the two pressures are balanced; then, a pneumatic valve for discharging at the bottom of the high-level feeding balance tank (2) is opened, the material automatically flows into the hydrogenation kettle by utilizing the gravity of the material to react, and the high-level feeding balance tank (2) is decompressed to normal pressure for standby during the reaction.
2. The hydrogenation kettle non-pressure relief hydrogenation device according to claim 1, wherein a discharging pipe is arranged at the bottom of the high-level feeding balance tank (2), and the discharging pipe is connected with a feeding port of the high-pressure hydrogenation kettle (1).
3. The hydrogenation kettle non-pressure relief hydrogenation device according to claim 1, wherein the discharge port of the high-pressure hydrogenation kettle (1) is connected with the feed port of the elevated tank (3) through a pipeline.
4. The hydrogenation kettle non-pressure relief hydrogenation device according to claim 1, wherein the discharge port of the upper tank (3) is connected with the feed port of the lower tank (4) through a pipeline.
5. The hydrogenation kettle non-pressure relief hydrogenation device according to claim 1, wherein said non-pressure relief device further comprises an instrument.
6. Use of the hydrogenation kettle non-pressure-relief hydrogenation device according to claim 1 in the preparation of amide pesticides.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110838229.2A CN114917836B (en) | 2021-07-23 | 2021-07-23 | Hydrogenation kettle non-pressure-relief hydrogenation device and application thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202110838229.2A CN114917836B (en) | 2021-07-23 | 2021-07-23 | Hydrogenation kettle non-pressure-relief hydrogenation device and application thereof |
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| Publication Number | Publication Date |
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| CN114917836A CN114917836A (en) | 2022-08-19 |
| CN114917836B true CN114917836B (en) | 2023-07-14 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN202787469U (en) * | 2012-09-20 | 2013-03-13 | 叶晓丰 | High-low pressure balance draining device |
| CN103570557B (en) * | 2013-11-08 | 2015-10-28 | 山东沾化天九化工有限公司 | Continuous still reaction produces method and the device of 3,4 dichlorphenamide bulk powders |
| CN207016688U (en) * | 2017-06-21 | 2018-02-16 | 重庆弛源化工有限公司 | Energy-saving type BED production systems |
| CN207430244U (en) * | 2017-10-25 | 2018-06-01 | 诚达药业股份有限公司 | A kind of high pressure is fed in batches device |
| CN210434480U (en) * | 2019-07-07 | 2020-05-01 | 宿迁项王机械设备有限公司 | High-efficient hydrogenation unit of production hexamethylene diamine piperidine |
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