CN215139772U - Inert atmosphere circulation purification device for chemical reaction kettle - Google Patents
Inert atmosphere circulation purification device for chemical reaction kettle Download PDFInfo
- Publication number
- CN215139772U CN215139772U CN202120485110.7U CN202120485110U CN215139772U CN 215139772 U CN215139772 U CN 215139772U CN 202120485110 U CN202120485110 U CN 202120485110U CN 215139772 U CN215139772 U CN 215139772U
- Authority
- CN
- China
- Prior art keywords
- gas
- storage tank
- reaction kettle
- water
- oxygen
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Images
Landscapes
- Separation Of Gases By Adsorption (AREA)
Abstract
An inert atmosphere circulating purification device for a chemical reaction kettle is characterized in that an exhaust port of a reaction kettle (1) is connected with a cold trap (2); after organic impurities are removed by cold trap adsorption, the gas enters a normal pressure gas storage tank (3); the gas in the normal pressure gas storage tank (3) is circularly purified by the purification system (6) until the required water oxygen index is met; then, qualified high-purity inert gas is pressed into a high-pressure gas storage tank (5) by a compressor (4); and finally, introducing the air inlet of the reaction kettle again to realize circulating air supply. The device is provided with an independent gas purification system, can be selectively started, and greatly prolongs the service life of the water and oxygen adsorption column. In addition, the defect that gas can be insufficiently adsorbed by a purification system through single pass can be avoided through repeated circulation purification, so that higher purity of the inert gas is ensured.
Description
Technical Field
The utility model relates to a device that chemical industry reation kettle inert atmosphere circulation purified, in particular to organic chemical industry reaction unit who is very sensitive, need high-purity inert atmosphere protection to water and oxygen belongs to the chemical industry equipment field.
Background
In the chemical industry field, especially in the fine chemical production, many reactions need to be carried out in a high-purity inert atmosphere without water and oxygen, so that the safety of the reaction is ensured, and side reactions caused by water and oxygen are reduced. For example, some catalysts lose effectiveness when meeting water and oxygen, some high-activity reagents have explosion risks when meeting water and oxygen, and some materials in high-temperature reaction can generate obvious oxidation side reactions when meeting oxygen. Therefore, these sensitive chemical reactions must be protected by purging with a high purity inert gas (usually high purity nitrogen or high purity argon) (CN 208532663U). However, high purity inert gases are expensive and direct venting can result in significant waste. Therefore, the recycling of the inert gas is inevitably an environmentally friendly development trend.
At present, the literature has reported equipment for recycling inert gases. However, some of the apparatuses were not subjected to gas purification and were directly recycled (CN 204768607U). There are also some patent documents reporting nitrogen gas recycling devices (CN 206008678U) with water washing tanks (to remove water-soluble impurities) and molecular sieve adsorption tanks (to remove organic impurities and water vapor), but oxygen removal devices in the recycling process are not considered. In fact, the inert gas is inevitably permeated and polluted by the external air in the continuous circulating process, so that the oxygen content of water in the inert gas is increased, and the adverse effect is brought to a reaction system.
SUMMERY OF THE UTILITY MODEL
To the not enough of prior art, the utility model provides a circulation purifier of high-purity inert atmosphere is applicable to the meticulous organic chemical industry reaction that is very sensitive, needs high-purity inert atmosphere protection to water and oxygen.
The utility model discloses a scheme contains inert gas circulation system and gas purification system two parts, and gas circulation system includes cold trap, ordinary pressure gas holder, gas compressor and high-pressure gas holder, and gas purification system then includes circulating fan, aqueous vapor adsorption column, oxygen adsorption column, and gas purification system links to each other with the ordinary pressure gas holder.
In the practical application process, the inert gas discharged from the reaction kettle is firstly removed of organic vapor and other organic impurities through the cold trap, and then discharged into the normal-pressure gas storage tank. The normal pressure gas storage tank has larger volume and can realize sufficient pressure buffering. The normal pressure gas storage tank body is provided with a pressure sensor, a water vapor sensor and an oxygen sensor and is connected with a PLC automatic control system. When water or oxygen exceeds the standard, the PLC controls and starts the gas purification system. And under the condition that the water oxygen index is qualified, when the pressure sensor detects that the pressure of the tank body is higher than a certain set value, the PLC system controls to start the gas compressor, and the inert gas in the normal-pressure gas storage tank is pressed into the high-pressure gas storage tank. The high-pressure gas storage tank is further connected with a gas inlet of the reaction kettle and used for purging the reaction kettle with inert gas. Through the process, the recycling of the inert gas is finally realized.
When the gas purification system works, the circulating fan guides the gas in the normal-pressure gas storage tank to sequentially pass through the efficient water adsorption column and the efficient oxygen adsorption column, so that a small amount of water vapor and oxygen in the gas are removed, and the gas returns to the normal-pressure gas storage tank again. The gas purification system continuously and circularly works until the water oxygen index of the inert gas in the normal-pressure gas storage tank is qualified.
The water adsorption column is filled with a water gas adsorption material, and the water gas adsorption material is preferably a 3A molecular sieve.
The oxygen adsorption column is filled with an oxygen adsorption material, and the oxygen adsorption material is preferably a copper catalyst.
When the water adsorption column and the oxygen adsorption column in the gas purification system are saturated in adsorption, the water adsorption column and the oxygen adsorption column can be regenerated and utilized in a vacuum heating and/or hydrogen reduction mode, so that replacement can be reduced, and cost is reduced.
In the gas purification system, the water adsorption column and the oxygen adsorption column can be combined into a comprehensive water-oxygen adsorption column, and only the water-gas adsorption material and the oxygen adsorption material are mixed and filled. An active carbon adsorption column can be added in front of the water oxygen adsorption column for adsorbing a small amount of residual organic impurities and protecting the water oxygen adsorption material from being damaged.
The connection order of each equipment can change each other among the gas purification system, as long as do not influence the function, its simple transform form all is in the utility model discloses a protection range.
The utility model provides a cold trap can fully cool off organic solvent and other organic impurities that contain in the reation kettle institute combustion gas, guarantees that aqueous vapor and oxygen sensor are not damaged or influence the precision by organic impurities, also can protect the water adsorption column and the oxygen adsorption column among the clean system to avoid organic impurities to destroy.
The utility model discloses a set up gas compressor and high-pressure gas holder for the endless inert gas can be used for the pressurization operation, and it is more convenient to use.
The utility model discloses the biggest characteristics lie in, through setting up independent gas purification system, can selectively purify the operation, only just start clean system when water oxygen content exceeds standard promptly, can prolong the life of water, oxygen adsorption column greatly. On the other hand, the purification system can perform repeated and repeated cyclic purification operation, so that the defect that gas can be insufficiently adsorbed when passing through the purification system once is avoided, and higher purity of the inert gas can be ensured.
The device for the circulation purification of the inert atmosphere can be connected with a plurality of reaction kettles, plays a role in centralized purification and cyclic utilization, and has good compatibility and expandability.
The device for the circulation purification of the inert atmosphere is suitable for fine organic chemical reactions which are very sensitive to water and oxygen and need high-purity inert atmosphere protection, such as reactions using water-oxygen sensitive catalysts (such as low-valent iron, cobalt, nickel, copper, palladium, platinum and ruthenium catalysts), reactions using water-oxygen sensitive reagents (such as active metals, alkyl metal reagents and aryl metal reagents) and organic chemical reactions above 200 ℃ (such as heterocyclic ring-closing reactions at high temperature).
Drawings
Fig. 1 is the structure schematic diagram of the inert atmosphere circulation purification device for the chemical reaction kettle.
Reference numerals: the method comprises the following steps of 1-a reaction kettle, 2-a cold trap, 3-a normal pressure gas storage tank, 4-a gas compressor, 5-a high pressure gas storage tank, 6-a gas purification system, 7-a circulating fan, 8-a water adsorption column, 9-an oxygen adsorption column, 10-a water gas sensor, 11-an oxygen sensor, 12-a pressure sensor, 13-a high purity inert gas supplement port, 14-a gas discharge port, 15-a high purity inert gas branch and 16-a PLC control system.
Detailed Description
The present invention will be further explained with reference to the drawings and examples.
The embodiment of the utility model provides a device for the cyclic purification of the inert atmosphere of a chemical reaction kettle, as shown in figure 1, an exhaust port of the reaction kettle 1 is connected with a cold trap 2; after organic impurities are removed by adsorption of a cold trap 2, the gas enters a normal-pressure gas storage tank 3; the gas in the normal pressure gas storage tank 3 is circularly purified by a purification system 6 until the required water oxygen index is met; then, qualified high-purity inert gas is pressed into a high-pressure gas storage tank 5 by a gas compressor 4; finally, the high-pressure gas storage tank 5 is connected with the gas inlet of the reaction kettle 1 to realize circulating gas supply.
The gas purification system 6 comprises a circulating fan 7, a water adsorption column 8 and an oxygen adsorption column 9. When the gas purification system 6 works, gas with higher water oxygen content in the normal-pressure gas storage tank 3 is guided by the circulating fan 7, sequentially passes through the water adsorption column 8 and the oxygen adsorption column 9, and returns to the normal-pressure gas storage tank 3 again. The gas purification system 6 performs a plurality of times of circulating purification operations until the water oxygen content reaches the standard.
A water vapor sensor 10, an oxygen sensor 11, a pressure sensor 12, a high-purity inert gas supplement port 13 and a gas discharge port 14 are arranged on a tank body of the normal-pressure gas storage tank 3; the above-mentioned equipment and corresponding control valves are connected with a PLC control system 16. When the system detects that the water content or oxygen content value is higher, the PLC controls the gas purification system 6 to be automatically started until the index is qualified. Under the condition that the water oxygen index is qualified, when the system detects that the gas pressure is higher than a certain set value, the PLC controls the gas compressor 4 to be automatically started, and gas is pressed into the high-pressure gas storage tank 5 until the pressure is lower than the set value. When the system detects that the gas pressure is lower than a certain set value, the PLC controls to automatically open the high-purity inert gas supplementing port 13 to supplement the inert gas. When the pressure exceeds the safe range, the PLC controls the gas discharge port 14 to be opened, and the redundant gas is discharged through the gas discharge port 14.
The reaction kettle is provided with a high-purity inert gas branch 15 on the gas inlet pipeline, and when the gas pressure of the high-pressure gas storage tank 5 in the circulating system is insufficient, inert gas can be supplemented through the high-purity inert gas branch 15.
In this embodiment, the water vapor adsorbing material used in the water adsorbing column 8 is 3A molecular sieve, and the oxygen adsorbing material used in the oxygen adsorbing column 9 is copper catalyst.
Claims (5)
1. The utility model provides an inert atmosphere circulation purifier for chemical industry reation kettle which characterized in that:
the device for circularly purifying the inert atmosphere of the chemical reaction kettle comprises a cold trap (2), a normal-pressure gas storage tank (3), a gas compressor (4), a high-pressure gas storage tank (5) and a gas purification system (6) which operates independently, wherein the cold trap, the normal-pressure gas storage tank, the gas compressor, the high-pressure gas storage tank and the gas purification system are sequentially connected in series; the inlet and outlet pipelines of the gas purification system (6) are connected with the normal-pressure gas storage tank (3);
the gas purification system (6) comprises a circulating fan (7), a water adsorption column (8) and an oxygen adsorption column (9).
2. The inert atmosphere circulation purification device for the chemical reaction kettle as claimed in claim 1, wherein a water gas sensor (10), an oxygen sensor (11) and a pressure sensor (12) are arranged on the tank body of the normal pressure gas storage tank (3).
3. The inert atmosphere circulation purification device for the chemical reaction kettle as claimed in claim 2, wherein the water gas sensor (10), the oxygen sensor (11), the pressure sensor (12), the gas compressor (4), the circulating fan (7) and the control circuit of the corresponding auxiliary valve are connected with a PLC control system (16).
4. The inert atmosphere circulation purification device for the chemical reaction kettle according to any one of claims 1 to 3, characterized in that a high purity inert gas supplement port (13) and a gas discharge port (14) are arranged on the tank body of the normal pressure gas storage tank (3), and a high purity inert gas branch (15) is arranged on the gas inlet pipeline of the reaction kettle.
5. The inert atmosphere circulation purification device for the chemical reaction kettle according to any one of claims 1 to 3, wherein the water vapor adsorbing material filled in the water adsorbing column (8) is a 3A molecular sieve, and the oxygen adsorbing material filled in the oxygen adsorbing column (9) is a copper catalyst.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202120485110.7U CN215139772U (en) | 2021-03-05 | 2021-03-05 | Inert atmosphere circulation purification device for chemical reaction kettle |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202120485110.7U CN215139772U (en) | 2021-03-05 | 2021-03-05 | Inert atmosphere circulation purification device for chemical reaction kettle |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN215139772U true CN215139772U (en) | 2021-12-14 |
Family
ID=79413955
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202120485110.7U Active CN215139772U (en) | 2021-03-05 | 2021-03-05 | Inert atmosphere circulation purification device for chemical reaction kettle |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN215139772U (en) |
-
2021
- 2021-03-05 CN CN202120485110.7U patent/CN215139772U/en active Active
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| KR101388266B1 (en) | Method and apparatus for separating blast furnace gas | |
| KR20120125334A (en) | Inert gas recovery system and method | |
| JP2013538880A (en) | Integrated biogas purification system to remove water, siloxane, sulfur, oxygen, chloride and volatile organic compounds | |
| CA1125478A (en) | Self-regenerating method and system of removing oxygen and water impurities from hydrogen gas | |
| CA3033841C (en) | Method for recovering hydrogen from biomass pyrolysis gas | |
| CN110559800A (en) | Intermediate-temperature hydrogen storage alloy preparation and pressure swing adsorption purification method | |
| CN112408325B (en) | System and method for continuously extracting hydrogen from tail gas and recycling tail gas | |
| JP2016084272A (en) | Method for producing hydrogen gas and apparatus for producing hydrogen gas | |
| JPWO2018116982A1 (en) | Hydrogen production apparatus and hydrogen production method | |
| CN110595221A (en) | Tail gas recycling device and process for galvanizing continuous annealing furnace | |
| KR102035870B1 (en) | Purifying method and purifying apparatus for argon gas | |
| CN215139772U (en) | Inert atmosphere circulation purification device for chemical reaction kettle | |
| CN111646432A (en) | Hydrogen purification system | |
| JP2003267725A (en) | Method of manufacturing ammonia, its apparatus and flue gas denitrification using the manufactured ammonia | |
| CA2651797C (en) | Method for treatment of drain in hydrogen production and hydrogen production system | |
| JP3815445B2 (en) | Hydrogen gas purification apparatus and purification method | |
| CN201815242U (en) | Organic waste gas catalytic oxidation purification treatment system device | |
| CN214612673U (en) | Waste argon recycling device of cold rolling annealing furnace protective gas supply system | |
| CN212549026U (en) | Purification system of self-supplying regeneration gas | |
| CN211261816U (en) | Tail gas recovery processing and recycling device of galvanizing continuous annealing furnace | |
| JP2010012464A (en) | Method for separating sulfur from gas containing sulfur | |
| CN112358899A (en) | System and method for preparing liquefied natural gas from biogas | |
| US20040187683A1 (en) | Gas recovery system to improve the efficiency of abatementand/or implement reuse/reclamation | |
| JP4217785B2 (en) | Gas regeneration type discharge NOx treatment method and apparatus | |
| CN215559020U (en) | Pressure swing adsorption nitrogen making system combined with nitrogen purifier |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| GR01 | Patent grant | ||
| GR01 | Patent grant |