CN111389169A - Device and method for recovering high-purity ammonia from compound semiconductor tail gas - Google Patents
Device and method for recovering high-purity ammonia from compound semiconductor tail gas Download PDFInfo
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- CN111389169A CN111389169A CN202010124823.0A CN202010124823A CN111389169A CN 111389169 A CN111389169 A CN 111389169A CN 202010124823 A CN202010124823 A CN 202010124823A CN 111389169 A CN111389169 A CN 111389169A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/002—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by condensation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D5/00—Condensation of vapours; Recovering volatile solvents by condensation
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
- C01C1/00—Ammonia; Compounds thereof
- C01C1/02—Preparation, purification or separation of ammonia
- C01C1/12—Separation of ammonia from gases and vapours
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Abstract
The invention relates to a device and a method for recovering high-purity ammonia from compound semiconductor tail gas, belonging to the technical field of environment and resource utilization.
Description
Technical Field
The invention belongs to the technical field of environment and resource utilization, and particularly relates to a device and a method for recovering high-purity ammonia from compound semiconductor tail gas.
Background
In the production process of the compound semiconductor, a large amount of mixed gas of nitrogen, hydrogen and ultrapure ammonia (the concentration of the mixed gas is 30-80% of nitrogen, 10-40% of hydrogen and 10-30% of ultrapure ammonia in general) is required to be used, and the mixed gas is directly discharged after passing through the production process, so that precious gas resources are wasted, and the environment is polluted. With the deep implementation of energy conservation, environmental protection and circular economy in the world, industrial projects with certain economic value but certain environmental pollution are often limited in the application process. The emission of ammonia gas directly pollutes the environment, and the production of compound semiconductors is strictly limited. Therefore, the current solution is to use a water washing method to dissolve ammonia gas in water, so that expensive high-purity and ultra-pure ammonia gas is changed into cheap ammonia water.
At present, no mature technology and method for recovering high-purity ammonia from compound semiconductor tail gas exist at home and abroad.
Disclosure of Invention
In order to make up for the defects of the prior art, the invention provides a device and a method for recovering high-purity ammonia from compound semiconductor tail gas. The device and the method can realize safe emission of tail gas after high-purity ammonia is recovered (the device and the method meet the national environmental protection emission standard).
The invention has the following inventive concept: the method for liquefying and recycling ammonia gas by pressurizing and low-temperature reboiling degasification ammonia has the obvious characteristics that the purity and the recovery rate of the recycled ammonia are high, and the harmful substances in the discharged gas meet the national environmental protection standard.
The invention adopts the following technical scheme: a device for recovering high-purity ammonia from compound semiconductor tail gas comprises a tail gas buffer tank, a multistage compressor, a low-temperature reboiling ammonia removal liquefaction device, a valve, a pipeline pipe fitting and a control system which are sequentially connected;
the low-temperature reboiling and degassing ammonia liquefaction device comprises a turbine expander, a main heat exchanger, a condensing tower, a reboiling and degassing tower and a liquid ammonia storage kettle, wherein a secondary heat exchanger is arranged in the liquid ammonia storage kettle, and the bottom of the reboiling and degassing tower is connected with the liquid ammonia storage kettle;
the liquid ammonia storage kettle is connected with a high-purity ammonia outlet through a main heat exchanger;
the outlet of the multistage compressor is sequentially connected with the main heat exchanger, the turboexpander, the condensing tower and the non-condensable gas outlet through a pipeline A; the outlet of the multistage compressor is connected with the secondary heat exchanger through a pipeline B;
and a condensing tower is connected above the reboiling degassing tower, and the condensing tower is connected with a non-condensable gas outlet through a main heat exchanger.
Furthermore, the tail gas buffer tank adopts any one device of a resistance-free centralized discharge pipeline, a gas storage tank or a gas bag; the multistage compressor is an oil-free multistage compressor.
Furthermore, the reboiled degasser uses a metal grid to separate the upper part and the lower part, and metal fillers are respectively filled in the upper part and the lower part.
In the whole system, all the temperature, pressure, flow and instruments, valves and the like are controlled by a control system.
The tail gas from the raw gas compressor exchanges heat with non-condensable gas discharged from the upper part of the reboiling degassing tower and reheated liquid ammonia through a main heat exchanger, then is cooled through a turbine expander, and then enters a condensing tower on the upper part of the reboiling degassing tower through a throttle valve, part of ammonia gas is liquefied and is introduced into the reboiling degassing tower along with the non-condensable gas from the middle of two sections of fillers, a condensing tower is arranged on the upper part of the reboiling degassing tower, a non-condensable gas discharge port is arranged at the top of the condensing tower and is connected with the main heat exchanger, the ammonia gas in the tail gas entering the reboiling degassing tower is liquefied into liquid ammonia when passing through the condensing tower, and flows to a liquid ammonia storage kettle at the bottom of the reboiling degassing tower under the action of gravity. The non-condensable gas (nitrogen, hydrogen and a trace amount of ammonia) is discharged from a discharge port at the top of the reboiling degasification tower through the condensation tower, fully exchanges heat with raw material tail gas from a multi-stage compressor and then is discharged into the atmosphere.
And a part of the raw material tail gas entering the main heat exchanger enters a secondary heat exchanger of the liquid ammonia storage kettle after passing through the regulating valve, so that part of the liquid ammonia is boiled and vaporized again, and non-condensable gas in the liquid ammonia is stripped out, so that the purity of the liquid ammonia is improved. High-purity liquid ammonia is output from the liquid ammonia storage kettle by the shield pump, and is output to a boundary area after heat exchange with raw material tail gas by the main heat exchanger.
The invention also requests a method for recovering high-purity ammonia from the compound semiconductor tail gas, and ammonia gas in the tail gas is separated and purified into liquid ammonia by utilizing the processes of pressurization and low-temperature reboiling, degassing and liquefaction. The method specifically comprises the following steps:
s1, concentrating tail gas generated in the production process of a compound semiconductor into a tail gas buffer tank, and pressurizing the tail gas to 0.6-2.0 Mpa by a multistage compressor;
s2, cooling the pressurized tail gas to-50 to-100 ℃ after passing through a turbo expander and a main heat exchanger;
s3, liquefying ammonia gas by the tail gas treated in the step S2 through a low-temperature reboiling degassing tower to obtain liquid ammonia with the concentration of 99.999%;
s4, a part of raw material tail gas passes through a secondary heat exchanger in the liquid ammonia storage kettle, the secondary heat exchanger is designed in the liquid ammonia storage kettle device, part of liquid ammonia in the liquid ammonia storage kettle can be vaporized and flows to the upper part of the reboiling degassing tower, the vaporized ammonia in the filler is dissolved in descending liquid ammonia, hydrogen and nitrogen in the ammonia are exchanged, undissolved ammonia is condensed to flow downwards to the liquid ammonia storage kettle when passing through the top condensing tower, the liquid ammonia is further purified, and non-condensable gas is discharged from the top.
Further, the non-condensable hydrogen, nitrogen and trace ammonia in the low-temperature reboiling tower device in the step S3 are discharged from the top of the reboiling degassing tower after passing through the main exchanger.
The device and the method provided by the invention have the following characteristics:
1. the recovery rate of ammonia is high, generally can reach more than 99.9 percent, and the recovery rate of economic operation is 98 percent.
2. The recovery purity of the ammonia gas is high, and reaches over 99.999 percent under the condition of economic recovery rate.
3. The content of ammonia in the discharged non-condensable gas is lower than 2 percent, and the discharged non-condensable gas can be directly discharged.
4. The invention has good comprehensive utilization effect, can obtain liquid ammonia and qualified exhaust gas in a set of device for the first time, recycles resources to the maximum extent, recycles expensive liquid ammonia, and saves production and operation cost.
5. In recent years, strict requirements on environmental protection are provided in China, the exhaust gas of the invention completely meets the national environmental protection requirements, and the influence of industrial production on the environment is reduced.
The invention has the beneficial effects that:
the method can recover a large amount of expensive liquid ammonia which is exhausted once in the traditional process and is recycled into the production process again by a separation and purification method, greatly reduces the production cost of L ED and compound semiconductors, improves the production yield of devices, has the remarkable characteristics of high recovery efficiency, high purity of the recovered liquid ammonia, good purification depth and low recovery cost, simultaneously realizes the purposes of energy conservation and emission reduction, energy conservation and environmental protection and comprehensive utilization of resources, promotes the development of the field, and has incomparable technical advantages and wide application prospect.
Drawings
FIG. 1 is a flow chart of the purification process for recovering liquid ammonia from tail gas according to the present invention.
FIG. 2 is a schematic diagram of the structure of the low-temperature reboiled ammonia separation unit of the present invention.
The system comprises a tail gas buffer tank 1, a multistage compressor 2, a low-temperature reboiling degassing ammonia liquefaction device 3, a turboexpander 5, a main heat exchanger 6, a condensing tower 7, a reboiling degassing tower 8, a secondary heat exchanger 9, a liquid ammonia storage kettle 10, a raw gas inlet 11, non-condensable gas high-level emptying 12, a liquid ammonia outlet 13, a non-condensable gas outlet 14, a high-purity ammonia outlet 15 and raw gas from a compression process.
Detailed Description
The invention is described in detail below with reference to the figures and the specific embodiments, without limiting the scope of the invention.
Example 1
This example is a recovery and purification process carried out under the tail gas index shown in Table 1.
TABLE 1 Properties of the exhaust gas
| Composition of | H2 | N2 | NH3 | O2 | SiH4 | Mo source |
| The content is V% | 20.0 | 60 | 20 | ≤50ppm | Micro-scale | Micro-scale |
The operating conditions are as follows:
flow rate: 2000Nm3/h
Pressure: atmospheric pressure
Temperature: 40-50 deg.C
The operation method comprises the following steps:
s1, concentrating tail gas generated in the production process of a compound semiconductor into a tail gas buffer tank 1, and pressurizing the tail gas to 1.7Mpa by a multistage compressor 2;
s2, the pressurized tail gas enters a turbine expander 4 after exchanging heat with a main heat exchanger 5, and the temperature of the tail gas is reduced to-70 ℃ to-90 ℃;
s3, the tail gas passing through the upper temperature and the lower temperature enters a condensing tower 6 of a low-temperature reboiling degassing ammonia liquefying device 3 through throttling, a temperature area lower than-90 ℃ is formed in the condensing tower 6, then the tail gas (gas-liquid mixture) enters from the middle part of a reboiling degassing tower 7, liquid ammonia descends into a liquid ammonia storage kettle 9 under the action of gravity, non-condensable gas and part of ammonia gas upwards flow through the condensing tower 6, the non-liquefied ammonia gas is condensed, and the non-condensable nitrogen gas, hydrogen gas and trace ammonia gas are discharged from the top of the reboiling degassing tower 7.
S4, a part of raw material tail gas passes through a secondary heat exchanger 8 in a liquid ammonia storage kettle 9, the secondary heat exchanger 8 is designed in a device of the liquid ammonia storage kettle 9, part of liquid ammonia in the liquid ammonia storage kettle 9 can be vaporized and flows to the upper part of a reboiling degassing tower 7, the vaporized ammonia in the filler is dissolved in descending liquid ammonia, hydrogen and nitrogen in the ammonia are exchanged, undissolved ammonia is condensed when passing through a top condensing tower 6 and flows downwards to the liquid ammonia storage kettle 9, the liquid ammonia is further purified, 99.999% of liquid ammonia is obtained, and non-condensable gas is discharged from the top.
The recovered gas state is shown in Table 2.
Table 2: state of recovered gas
The above description is only for the purpose of creating a preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art can substitute or change the technical solution and the inventive concept of the present invention within the technical scope of the present invention.
Claims (5)
1. The device for recovering high-purity ammonia from compound semiconductor tail gas is characterized by comprising a tail gas buffer tank (1), a multistage compressor (2), a low-temperature reboiling ammonia removal liquefaction device (3), a valve, a pipeline pipe fitting and a control system which are sequentially connected;
the low-temperature reboiling degassing ammonia liquefaction device (3) comprises a turbine expander (4), a main heat exchanger (5), a condensing tower (6), a reboiling degassing tower (7) and a liquid ammonia storage kettle (9), wherein a secondary heat exchanger (8) is arranged in the liquid ammonia storage kettle (9), and the bottom of the reboiling degassing tower (7) is connected with the liquid ammonia storage kettle (9);
the liquid ammonia storage kettle (9) is connected with a high-purity ammonia outlet through the main heat exchanger (5);
the outlet of the multi-stage compressor (2) is sequentially connected with the main heat exchanger (5), the turboexpander (4), the condensing tower (6) and the non-condensable gas outlet through a pipeline A; the outlet of the multi-stage compressor (2) is connected with a secondary heat exchanger (8) through a pipeline B;
a condensing tower (6) is connected above the reboiling degassing tower (7), and the condensing tower (6) is connected with a non-condensable gas outlet through a main heat exchanger (5).
2. The apparatus for recovering high-purity ammonia from compound semiconductor exhaust gas according to claim 1, wherein the exhaust gas buffer tank (1) is one of a resistance-free centralized discharge pipeline, a gas storage tank and a gas bag; the multi-stage compressor (2) is an oil-free multi-stage compressor.
3. The apparatus for recovering high-purity ammonia from compound semiconductor off-gas according to claim 1, wherein the reboiled degasser (7) comprises a metal grid separating upper and lower portions, and metal packings packed therein.
4. A method for recovering high-purity ammonia from compound semiconductor tail gas is characterized by comprising the following steps:
s1, concentrating tail gas generated in the production process of a compound semiconductor into a tail gas buffer tank (1), and pressurizing the tail gas to 0.6-2.0 Mpa by a multistage compressor (2);
s2, cooling the pressurized tail gas to-50 to-100 ℃ after passing through a turbo expander (4) and a main heat exchanger (5);
s3, liquefying ammonia gas by the tail gas treated in the step S2 through a reboiling degassing tower (7) to obtain liquid ammonia;
s4, passing part of raw material tail gas through a secondary heat exchanger (8) in a liquid ammonia storage kettle (9), vaporizing part of liquid ammonia in the tower kettle to flow to the upper part of a reboiling degassing tower (7), dissolving the vaporized ammonia in the filler into descending liquid ammonia, exchanging hydrogen and nitrogen in the ammonia, condensing undissolved ammonia when passing through a top condensing tower (6) and flowing downwards to the liquid ammonia storage kettle (9), further purifying the liquid ammonia, and discharging non-condensable gas from the top.
5. The method according to claim 4, wherein the noncondensable hydrogen, nitrogen and trace ammonia in the reboiled degasser (7) in step S3 are discharged from the top of the reboiled degasser (7) after passing through the main exchanger (5).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010124823.0A CN111389169A (en) | 2020-02-27 | 2020-02-27 | Device and method for recovering high-purity ammonia from compound semiconductor tail gas |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202010124823.0A CN111389169A (en) | 2020-02-27 | 2020-02-27 | Device and method for recovering high-purity ammonia from compound semiconductor tail gas |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| AU2934002A (en) * | 2001-04-06 | 2002-10-10 | Rohm And Haas Company | Improved process for ammonia recovery |
| EP1291339A2 (en) * | 2001-09-05 | 2003-03-12 | Basf Aktiengesellschaft | Continuous process for the synthesis of monoethanolamine, diethanolamine and triethanolamine |
| CN102502634A (en) * | 2011-11-17 | 2012-06-20 | 中国五环工程有限公司 | Technological method for preparing food-grade CO2 based on high-concentration carbon dioxide exhaust gas |
| CN104556148A (en) * | 2014-12-29 | 2015-04-29 | 安徽淮化股份有限公司 | Synthesis ammonia conversion condensate recycling treatment method and device thereof |
| CN206837532U (en) * | 2017-05-17 | 2018-01-05 | 万和昌 | The distillation system of ammonia |
| CN109437234A (en) * | 2018-11-15 | 2019-03-08 | 大连中鼎化学有限公司 | A kind of compound semiconductor epitaxial tail gas recycling device and method |
-
2020
- 2020-02-27 CN CN202010124823.0A patent/CN111389169A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| AU2934002A (en) * | 2001-04-06 | 2002-10-10 | Rohm And Haas Company | Improved process for ammonia recovery |
| EP1291339A2 (en) * | 2001-09-05 | 2003-03-12 | Basf Aktiengesellschaft | Continuous process for the synthesis of monoethanolamine, diethanolamine and triethanolamine |
| CN102502634A (en) * | 2011-11-17 | 2012-06-20 | 中国五环工程有限公司 | Technological method for preparing food-grade CO2 based on high-concentration carbon dioxide exhaust gas |
| CN104556148A (en) * | 2014-12-29 | 2015-04-29 | 安徽淮化股份有限公司 | Synthesis ammonia conversion condensate recycling treatment method and device thereof |
| CN206837532U (en) * | 2017-05-17 | 2018-01-05 | 万和昌 | The distillation system of ammonia |
| CN109437234A (en) * | 2018-11-15 | 2019-03-08 | 大连中鼎化学有限公司 | A kind of compound semiconductor epitaxial tail gas recycling device and method |
Non-Patent Citations (1)
| Title |
|---|
| 西安交通大学计光华: "《透平膨胀机》", 28 February 1982, 机械工业出版社 * |
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Application publication date: 20200710 |