CN213202874U - Device for preparing high-purity trifluoromethane - Google Patents
Device for preparing high-purity trifluoromethane Download PDFInfo
- Publication number
- CN213202874U CN213202874U CN202021245515.5U CN202021245515U CN213202874U CN 213202874 U CN213202874 U CN 213202874U CN 202021245515 U CN202021245515 U CN 202021245515U CN 213202874 U CN213202874 U CN 213202874U
- Authority
- CN
- China
- Prior art keywords
- gas
- adsorption
- trifluoromethane
- condenser
- product
- 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
The utility model discloses a prepare device of high-purity trifluoromethane, including the feed gas feed system who connects gradually, adsorption system, filtration system, rectifying system and product gas fill dress system, feed gas feed system is including the raw materials steel bottle that is used for the splendid attire feed gas, adsorption system is including the adsorption tower that is used for adsorbing carbon dioxide and moisture, filtration system is including the filter that is used for filtering solid particle, rectifying system is including the first rectifying column that is used for getting rid of the light component and the second rectifying column that is used for getting rid of the heavy component, product gas fills dress system is including the product buffer tank that is used for receiving the product gas, a product steel bottle that is used for filling the gaseous membrane press of dress and is used for the splendid attire product gas. The utility model discloses a device of preparation high-purity trifluoromethane is disclosed for the first time, obtains high-purity trifluoromethane through decompression, absorption, filtration, rectification preparation, can realize the cyclic utilization of the energy.
Description
Technical Field
The utility model relates to a gas purification technique, concretely relates to prepare device of high-purity trifluoromethane.
Background
Trifluoromethane is a widely used and chemically stable fluoroalkane. In a semiconductor process, CHF3 is commonly used in a plasma etching or reactive ion etching silicon dioxide process, and CHF3 has the characteristics of high silicon dioxide etching speed, low silicon etching speed, good selectivity and large speed difference, and meets the requirements of the semiconductor process. The demand for high purity trifluoromethane as an etchant in the fabrication of 8-12 inch chips is increasing with the rapid growth of the semiconductor industry.
The volume component of industrial trifluoromethane is CHF3≥99％、H2≤100ppm、O2≤2940ppm、N2≤ 3500ppm、CO2≤2080ppm、H2O≤20ppm、CO≤153ppm、CH4≤9ppm、SF6≤8ppm、 C2F6Less than or equal to 9 ppm. The purity of the high-purity trifluoromethane used in the semiconductor industry is 99.999 percent, and how to purify the industrial trifluoromethane to obtain the high-purity trifluoromethane is a problem to be solved in the field.
Disclosure of Invention
The utility model aims at providing a prepare device of high-purity trifluoromethane prepares high-purity trifluoromethane to industrial-grade trifluoromethane purification, makes the energy can obtain abundant utilization, not only energy-conservation but also environmental protection.
In order to achieve the purpose of the utility model, the utility model adopts the technical proposal that: the utility model provides a prepare device of high-purity trifluoromethane, includes feed gas feed system, adsorption system, filtration system, rectifying system and the product gas dress system that connects gradually, feed gas feed system is including the raw material steel bottle that is used for the splendid attire feed gas, adsorption system is including the adsorption tower that is used for adsorbing carbon dioxide and moisture, filtration system is including the filter that is used for filtering solid particle, rectifying system is including the first rectifying column that is used for getting rid of light component and the second rectifying column that is used for getting rid of the heavy component that connects gradually, the product gas dress system is including the product buffer tank that is used for receiving the product gas, the membrane press that is used for filling gas and the product steel bottle that is used for the splendid attire product gas that connect gradually.
Furthermore, the raw material gas supply system comprises a plurality of raw material steel cylinders which are arranged in parallel in the raw material collection grid.
Furthermore, the adsorption system comprises two groups of adsorption towers which are arranged in parallel, and each group of adsorption tower comprises two stages of adsorption towers which are arranged in series.
Furthermore, the adsorption towers are filled with 4A molecular sieves and 5A molecular sieves, and each adsorption tower is filled with an upper layer of 4A molecular sieve and a lower layer of 5A molecular sieve to adsorb moisture and carbon dioxide in the raw material gas components.
Further, the adsorption tower is further connected with a hot nitrogen pipeline, a vacuumizing pipeline and a releasing pipeline, the hot nitrogen pipeline is connected to a hot nitrogen supply system, the vacuumizing pipeline is connected to a vacuum pump, and the vacuum pump and the releasing pipeline are connected to a tail gas receiving device.
Furthermore, the filtering system comprises two groups of filters which are arranged in parallel, and each group of filters comprises two stages of filters which are arranged in series.
Further, the precision of the filter is 1 micron.
Further, an outlet at the top end of the first rectifying tower is connected to a first condenser, a liquid phase outlet of the first condenser is connected to a first elevated tank, a bottom outlet pipeline of the first elevated tank is arranged in the first elevated tank, one of the two branches is connected with the upper reflux opening of the first rectifying tower, the other branch is connected with the middle inlet of the second rectifying tower, the top outlet of the first rectifying tower and the gas phase outlet of the first condenser are connected to a tail gas receiving device, the lower part of the first rectifying tower is connected with a first reboiler, the top end outlet of the second rectifying tower is connected with a second condenser, the liquid phase outlet of the second condenser is connected to a second elevated tank, the bottom outlet of the second elevated tank is connected to the upper reflux port of the second rectifying tower, and the lower part of the second rectifying tower is connected with a second reboiler and a residual liquid receiving device, and a top outlet of the second rectifying tower and a gas phase outlet of the second condenser are connected to the product buffer tank.
Furthermore, cold sources of the first condenser and the second condenser are refrigerating fluids, and heat sources of the first reboiler and the second reboiler are heat conduction oils.
In the above, the adsorption tower is the existing product, the core is the adsorption column, and the adsorption tower is preferably connected in parallel to form two groups, one group works, and the other group regenerates, so that the purification operation can be ensured to be uninterrupted; the adsorption column adsorbs partial impurities contained in the raw materials, the purity of high-purity trifluoromethane of a follow-up rectifying tower product is ensured, the regeneration gas in the adsorption system is high-purity hot nitrogen, and the regenerated nitrogen is recycled to the tail gas treatment system.
In the above, the filters are the existing products, the core is the filter column, and the filters are preferably connected in parallel to form two groups, so that the purification operation can be ensured to be uninterrupted, and the filters can also work simultaneously, thereby improving the filtering effect; the precision of the filter is 1 micron, particles in the raw material gas are effectively removed, and the purity of the high-purity trifluoromethane product of the subsequent rectifying tower is ensured.
In the above, the rectifying tower is a low-temperature rectifying operation, and adopts middle-lower part feeding, tower top discharging, tower bottom residual liquid recovery processing, and tower top condenser flash steam recovery to a tail gas processing system.
In the utility model, the connection is a gas pipe connection and is used for gas transmission among all parts; each part is equipped with gas access & exit, according to the utility model discloses a technical scheme, technical personnel in the field connect by oneself according to the place requirement.
Because of the application of the technical scheme, compared with the prior art, the utility model has the following advantages:
1) the device for preparing high-purity trifluoromethane disclosed by the utility model is firstly used for adsorbing raw material gas by the adsorption system to adsorb impurities such as carbon dioxide, moisture and the like in the raw material gas; the filter filters out solid particles in the adsorption tower to 1 micron; the filtered gas enters a rectifying tower; the rectifying tower is a low-temperature rectifying process, a cold source of a condenser at the tower top is provided by refrigerating fluid, light component impurities at the tower top of the first rectifying tower are discharged to a tail gas absorption system, heavy component impurities at the tower bottom of the second rectifying tower are recycled, and after the high-purity trifluoromethane is prepared by the method, the purity of the trifluoromethane reaches more than 99.999 percent;
2) the device for preparing high-purity trifluoromethane can effectively recover industrial trifluoromethane at the bottom of the rectifying tower and effectively control the production cost;
3) the utility model discloses a device for preparing high-purity trifluoromethane, two groups of adsorption towers are arranged in parallel, one group works, the other group regenerates, two groups of filters are arranged in parallel, one group works, the other group can carry out the replacement work of a filter column, and the continuity of the purification process is ensured;
4) the utility model discloses a device for preparing high-purity trifluoromethane, a gaseous product is filled through a membrane press, so that the interference of external impurities can be effectively avoided, and the purity of the product is ensured;
5) the utility model discloses a prepare high-purity trifluoromethane's device, purification efficiency is high, does not relate to chemical reagent, and especially the material of separation can be handled properly, for example cyclic utilization or collection are as other effects; and the method is easy to operate, low in cost and suitable for popularization and application.
Drawings
FIG. 1 is a schematic structural diagram of a device for preparing high-purity trifluoromethane according to the present invention.
Wherein: 11. a raw material steel cylinder; 12. collecting grids of raw materials; 21. an adsorption tower; 22. a hot nitrogen line; 23. Vacuumizing the pipeline; 24. a release line; 25. a vacuum pump; 31. a filter; 41. a first rectification column; 42. a first condenser; 43. a first elevated tank; 44. a first reboiler; 51. a second rectification column; 52. a second condenser; 53. a second elevated tank; 54. a second reboiler; 61. a product gas surge tank; 71. A film press; 81. and (5) a product steel cylinder.
Detailed Description
The invention will be further described with reference to the following drawings and examples:
in the drawings, the same components are only marked at one position, and some conventional connecting pieces such as valves are not marked, wherein a single arrow indicates the operation direction of purified gas, a double arrow indicates the operation direction of a heat source, and a triple arrow indicates the operation direction of a cold source.
Example one
Referring to fig. 1, as shown in the figure, an apparatus for preparing high-purity trifluoromethane comprises a raw material gas supply system, an adsorption system, a filtration system, a rectification system and a product gas filling system which are connected in sequence, wherein the raw material gas supply system comprises a raw material steel cylinder 11 for containing raw material gas, the adsorption system comprises an adsorption tower 21 for adsorbing carbon dioxide and moisture, the filtration system comprises a filter 31 for filtering solid particles, the rectification system comprises a first rectification tower 41 for removing light components and a second rectification tower 51 for removing heavy components which are connected in sequence, and the product gas filling system comprises a product buffer tank 61 for receiving product gas, a membrane press 71 for filling gas and a product steel cylinder 81 for containing product gas which are connected in sequence.
In the preferred embodiment of this embodiment, the raw material gas supply system includes a plurality of raw material cylinders 11 placed in parallel in a raw material storage 12.
In the preferred embodiment of the present embodiment, the adsorption system includes two groups of adsorption towers arranged in parallel, and each group of adsorption towers includes two stages of adsorption towers 21 arranged in series.
In the preferred embodiment of this example, the adsorption tower 21 is filled with 4A molecular sieves and 5A molecular sieves, and each adsorption tower is filled with an upper layer of 4A molecular sieves and a lower layer of 5A molecular sieves, and adsorbs moisture and carbon dioxide in the raw gas component.
In the preferred embodiment of the present embodiment, the adsorption tower 21 is further connected to a hot nitrogen line 22, an evacuation line 23 and a release line 24, the hot nitrogen line 22 is connected to a hot nitrogen supply system (not shown), the evacuation line 23 is connected to a vacuum pump 25, and the vacuum pump 25 and the release line 24 are connected to a tail gas receiving device (not shown).
In the preferred embodiment of this embodiment, the filtration system comprises two sets of filters arranged in parallel, each set of filters comprising two stages of filters 31 arranged in series.
In the preferred embodiment of this example, the precision of the filter 31 is 1 micron.
In the preferred embodiment of the present invention, the top outlet of the first rectifying tower 41 is connected to the first condenser 42, the liquid outlet of the first condenser 42 is connected to the first elevated tank 43, one of the outlets at the bottom of the first elevated tank 43 is connected to the upper reflux port of the first rectifying tower 41, the other is connected to the middle inlet of the second rectifying tower 51, the top outlet of the first rectifying tower 41 and the gas outlet of the first condenser 42 are connected to a tail gas receiving device (not shown in the figure), the first reboiler 44 is connected to the lower part of the first rectifying tower 41, the top outlet of the second rectifying tower 51 is connected to the second condenser 52, the liquid outlet of the second condenser 52 is connected to the second elevated tank 53, the bottom outlet of the second elevated tank 53 is connected to the upper reflux port of the second rectifying tower 51, the second rectifying tower 51 is connected to the lower part of the second rectifying tower 54 and a residual liquid receiving device (not shown in the figure), a top outlet of the second rectifying tower 51 and a gas phase outlet of the second condenser 52 are connected to a product buffer tank 61.
In the preferred embodiment of this embodiment, the cold sources of the first condenser 42 and the second condenser 52 are refrigerating fluids, and the heat sources of the first reboiler 44 and the second reboiler 54 are heat conducting oils.
The working process of the device comprises the following steps:
(1) reducing the pressure of the trifluoromethane in the raw material steel cylinders in the raw material collection lattice by a pressure reducing valve, outputting the reduced trifluoromethane, wherein the working pressure of the reduced trifluoromethane is 0.6MPa, and the reduced trifluoromethane enters one group of adsorption systems;
(2) deeply removing carbon dioxide and water in the trifluoromethane, and enabling the trifluoromethane without the carbon dioxide and the water to enter a filtering system;
(3) particles carried by the trifluoromethane through the adsorption system and particle impurities of the raw material are filtered by the filtering system, and the filtered gas enters an air inlet at the middle lower part of the first rectifying tower;
(4) the working pressure of the first rectifying tower is 0.6MPa, the working temperature of the first condenser is-65 ℃, and the working temperature of the tower bottom is 60 ℃; light component impurities H2, N2, O2 and trace CO2 at the top of the first rectifying tower are discharged to a tail gas receiving device through a discharge pipeline to be processed; the gas at the top of the tower enters a first condenser, the condensed material enters a first elevated tank, the material from the first elevated tank is divided into two parts, one part flows back to the upper tower of a first rectifying tower, and the other part flows into the middle part of a second rectifying tower to continue the rectifying operation;
(5) the working pressure of the second rectifying tower is 0.6MPa, the working temperature of the second condenser is-65 ℃, and the working temperature of the tower bottom is 60-80 ℃; heavy component impurities such as CH4, C2F6, CO, SF6 and the like at the bottom of the second rectifying tower are discharged; the gas at the tower top enters a second condenser, the condensed material enters a second elevated tank, and the material from the second elevated tank flows back to the upper tower of a second rectifying tower; the high-purity trifluoromethane which is produced from the product pipeline at the top of the tower enters a product gas buffer tank for storage;
(6) and the high-purity trifluoromethane enters a product buffer tank, and the high-purity trifluoromethane in the product tank is pressurized and filled into a product steel cylinder through a membrane press.
When one group of adsorption towers performs adsorption work, the other group of adsorption towers performs nitrogen regeneration treatment.
The utility model discloses the high-purity gas volume component of product is: CHF3≥99.999％、H2≤1ppm、O2≤1ppm、N2≤4ppm、CO2≤0.5ppm、H2O≤3ppm、CO≤0.5ppm、CH4≤0.5ppm、 SF6≤0.5ppm、C2F6≤1ppm。
Claims (9)
1. The utility model provides a prepare device of high-purity trifluoromethane, its characterized in that fills the system including the feed gas feed system, adsorption system, filtration system, rectifying system and the product gas that connect gradually, feed gas feed system is including the raw materials steel bottle that is used for the splendid attire feed gas, adsorption system is including the adsorption tower that is used for adsorbing carbon dioxide and moisture, filtration system is including the filter that is used for filtering solid particle, rectifying system is including the first rectifying column that is used for getting rid of light component and the second rectifying column that is used for getting rid of the heavy component that connect gradually, product gas fills the system and is including the product buffer tank that is used for receiving the product gas, the membrane press that is used for filling gas and the product steel bottle that is used for the product gas that connect gradually.
2. The apparatus for preparing highly pure trifluoromethane according to claim 1, wherein the raw material gas supply system comprises a plurality of raw material cylinders disposed in parallel in a raw material collection grid.
3. The apparatus for preparing highly pure trifluoromethane according to claim 1, wherein the adsorption system comprises two sets of said adsorption columns arranged in parallel, each set of said adsorption columns comprising two stages of said adsorption columns arranged in series.
4. The apparatus for preparing high-purity trifluoromethane according to claim 1, wherein the adsorption tower is filled with 4A molecular sieve and 5A molecular sieve, each adsorption tower is filled with upper 4A molecular sieve and lower 5A molecular sieve, and water and carbon dioxide in the raw gas components are adsorbed.
5. The apparatus for preparing highly pure trifluoromethane according to claim 1, wherein the adsorption column is further connected with a hot nitrogen line, an evacuation line and a release line, the hot nitrogen line is connected to a hot nitrogen supply system, the evacuation line is connected to a vacuum pump, and the vacuum pump and the release line are connected to a tail gas receiving apparatus.
6. The apparatus for preparing highly pure trifluoromethane according to claim 1, wherein said filtration system comprises two sets of said filters arranged in parallel, each set of said filters comprising two stages of said filters arranged in series.
7. The apparatus for preparing highly pure trifluoromethane according to claim 1, wherein the accuracy of the filter is 1 μm.
8. The apparatus for preparing highly pure trifluoromethane according to claim 1, wherein the top outlet of the first distillation column is connected to a first condenser, the liquid outlet of the first condenser is connected to a first elevated tank, the bottom outlet of the first elevated tank is connected in line with one of the upper reflux port of the first distillation column and the other is connected to the middle inlet of the second distillation column, the top outlet of the first distillation column and the gas outlet of the first condenser are connected to a tail gas receiver, the first distillation column is connected at the lower portion to a first reboiler, the second distillation column is connected at the top outlet to a second condenser, the liquid outlet of the second condenser is connected to a second elevated tank, the bottom outlet of the second elevated tank is connected to the upper reflux port of the second distillation column, and the second distillation column is connected at the lower portion to a second reboiler and a residual liquid receiver, and the top outlet of the second rectifying tower and the gas phase outlet of the second condenser are connected to the product buffer tank.
9. The apparatus for preparing high-purity trifluoromethane according to claim 8, wherein the cold source of the first condenser and the second condenser is refrigerating fluid, and the heat source of the first reboiler and the second reboiler is heat conducting oil.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202021245515.5U CN213202874U (en) | 2020-06-30 | 2020-06-30 | Device for preparing high-purity trifluoromethane |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202021245515.5U CN213202874U (en) | 2020-06-30 | 2020-06-30 | Device for preparing high-purity trifluoromethane |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN213202874U true CN213202874U (en) | 2021-05-14 |
Family
ID=75832481
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202021245515.5U Active CN213202874U (en) | 2020-06-30 | 2020-06-30 | Device for preparing high-purity trifluoromethane |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN213202874U (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113816826A (en) * | 2021-11-03 | 2021-12-21 | 中船重工（邯郸）派瑞特种气体有限公司 | Purification method of electronic-grade monofluoromethane |
| CN115448810A (en) * | 2022-11-11 | 2022-12-09 | 山东东岳化工有限公司 | Method and system for removing carbon dioxide and nitrous oxide in trifluoromethane |
-
2020
- 2020-06-30 CN CN202021245515.5U patent/CN213202874U/en active Active
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113816826A (en) * | 2021-11-03 | 2021-12-21 | 中船重工（邯郸）派瑞特种气体有限公司 | Purification method of electronic-grade monofluoromethane |
| CN113816826B (en) * | 2021-11-03 | 2023-05-02 | 中船(邯郸)派瑞特种气体股份有限公司 | Purification method of electronic grade monofluoromethane |
| CN115448810A (en) * | 2022-11-11 | 2022-12-09 | 山东东岳化工有限公司 | Method and system for removing carbon dioxide and nitrous oxide in trifluoromethane |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN109092010B (en) | Method for recycling waste gas in LED-MOCVD process through full-temperature-range pressure swing adsorption hydrogen extraction | |
| CN103951543B (en) | A kind of trifluoromethane purification devices and purification process | |
| CN213202874U (en) | Device for preparing high-purity trifluoromethane | |
| CN201842645U (en) | High-purity nitrogen generation system integrating membrane separation and pressure swing adsorption device | |
| CN103387211B (en) | With commercial synthesis hydrogenchloride for the method for electronic grade high-purity hydrogenchloride prepared by raw material | |
| CN206033226U (en) | Novel high -purity system oxygen system nitrogen is dual -purpose device | |
| CN109437234B (en) | Compound semiconductor epitaxy tail gas recycling device and method | |
| CN111548244A (en) | Method for recovering benzene and high-purity hydrogen in high yield from tail gas of biphenyl preparation process | |
| CN102049170B (en) | Process for producing rich oxygen by VPSA (vacuum pressure swing adsorption) air separation | |
| CN114870420A (en) | Method and device for producing high-purity electronic grade isopropanol | |
| CN211496938U (en) | Membrane separation concentration hydrogen recovery device | |
| CN107641535B (en) | Device and method for separating and purifying various gases by membrane cryogenic coupling | |
| CN211847167U (en) | Device for preparing high-purity boron trichloride | |
| CN101531342B (en) | Device and method for producing oxygen by means of pressure swing adsorption (PSA) by five beds | |
| CN211716983U (en) | Device for separating and purifying krypton and xenon | |
| CN211619943U (en) | Membrane separation nitrogen making device | |
| CN116605853A (en) | Method for preparing high-purity argon from air by adopting three-stage method | |
| CN111174530A (en) | Method and device for separating and purifying krypton and xenon | |
| CN207760043U (en) | A kind of production equipment of high-purity hydrogen peroxide | |
| CN215930316U (en) | Device for preparing high-purity carbonyl sulfide | |
| CN116177496A (en) | Purification method and device for electronic grade hydrogen bromide | |
| CN214780753U (en) | Device for preparing high-purity oxygen based on coupling separation technology | |
| CN112960650B (en) | Method and device for preparing high-purity oxygen based on coupling separation technology | |
| CN112744787B (en) | FTrPSA separation and purification method for deeply defluorinating and drying HCl gas containing high-concentration HF | |
| CN111333037B (en) | System and method for preparing high-purity hydrogen sulfide gas |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CP03 | Change of name, title or address | ||
| CP03 | Change of name, title or address |
Address after: No. 09, Yuanda Road, Shitan Industrial Park, Shizi Town, Quanjiao County, Chuzhou City, Anhui Province 239500 Patentee after: Anhui APK Electronic Material Co.,Ltd. Address before: 239500 east side of Chaoyang Road, Shitan Industrial Park, Shizi Town, Quanjiao County, Chuzhou City, Anhui Province Patentee before: ANHUI AIPEIKE ELECTRONIC MATERIALS CO.,LTD. |