CN103675119A - Experiment device for recycling ammonia in LED (light emitting diode) mixed waste gas by compression refrigeration method and verifying method of experiment device - Google Patents
Experiment device for recycling ammonia in LED (light emitting diode) mixed waste gas by compression refrigeration method and verifying method of experiment device Download PDFInfo
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- CN103675119A CN103675119A CN201310577187.7A CN201310577187A CN103675119A CN 103675119 A CN103675119 A CN 103675119A CN 201310577187 A CN201310577187 A CN 201310577187A CN 103675119 A CN103675119 A CN 103675119A
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Abstract
The invention discloses an experiment device for recycling ammonia in LED (light emitting diode) mixed waste gas by a compression refrigeration method and a verifying method of the experiment device. The verifying method is mainly used for verifying that GaN is deposited by the ammonia and a trimethyl gallium gas phase of a semiconductor light emitting diode (LED); the mixed gas of ammonia, nitrogen and hydrogen is discharged in a production process, and a little of ammonia in the mixed gas is recycled by the compression refrigeration method technology; the correctness of chemically technical software measurement during technical design is verified; the possible deflection in a design and actual implementation process is prevented; the design precision is improved; the investment loss is reduced.
Description
Technical field
The present invention relates to process waste gas technical field in LED production, be particularly related to a kind of for verifying that vapour deposition becomes GaN with trimethyl gallium at ammonia at semiconductor light-emitting-diode (being called for short LED), in production run, discharge ammonia, nitrogen, hydrogen gas mixture, by compression freezing technique, reclaim a small amount of ammonia in mixed gas, in Process Planning, verify the correctness of metallization processes software measuring and calculating, prevent the deviation that may produce in design and actual implementation process, improve design accuracy, reduce the method for investment loss.
Background technology
Ultra-pure ammonia is mainly asked starting material (can be described as is the grain of four major trades) as light emitting diode (LED), flat-panel monitor (FPD), semiconductor and crystal silicon solar batteries sheet (four major trades).
And because the decision of technique has 99% ammonia, along with nitrogen, hydrogen, discharge in light emitting diode (LED) is produced, need to effectively be reclaimed by retracting device, not so can serious environment pollution.
The method reclaiming at present by: 1, will discharge ammonia and neutralize with sulfuric acid, the later waste liquid of neutralization enters sewage treatment plant and processes; 2, will discharge ammonia and absorb into ammoniacal liquor with film-falling absorption tower water, ammoniacal liquor is undersold; 3, packed tower is absorbed as ammoniacal liquor by discharge ammonia, and ammoniacal liquor is undersold; 4, use compressor compresses mixed gas, then by ammonia condensation wherein, be that liquefied ammonia is recovered as industrial liquid ammonia with cryogenic refrigeration, nitrogen, hydrogen qualified discharge.
In above-mentioned several method, compress freezing and have again economic worth.But (LED) composition of discharging waste gas scale, various gases is all different, need detailed scientific software design.And Software for Design and reality there will be deviation unavoidably, once there is deviation, will cause and reclaim taking a bath and incuring loss through delay recycle program of waste gas.
Summary of the invention
Goal of the invention of the present invention is in order to overcome the shortcoming of above-mentioned background technology, a kind of experimental provision and verification method thereof that freezing reclaims ammonia in LED mix waste gas that compress is provided, thereby by this method, obtain the data of testing under various pressure, temperature, flow in compression freezing removal process for mixed gas, for bigger device provides the design data of science.Can verify well the authenticity of chemistry calculation software data and revise.Method is novel, reduced investment, experiment is fast, data science is true.
Technical scheme of the present invention is: a kind of experimental provision that compresses ammonia in freezing recovery LED mix waste gas, it comprises: hybrid standard gas cylinder, decompression pressure regulator valve group, tensimeter, cryogenic freezing liquid container, cryogenic freezing liquid, the rotating freeze pipe group of Luo, gas-liquid separator, thermometer, gas meter, pressure regulating valve, gas chromatograph, waste gas neutralization bucket, described hybrid standard gas cylinder is connected with decompression pressure regulator valve group I, decompression pressure regulator valve group I is connected with the rotating freeze pipe group of Luo, the rotating freeze pipe group of Luo is connected with gas-liquid separator, gas-liquid separator is connected with decompression pressure regulator valve group II, the outlet of decompression pressure regulator valve group II is provided with two pipelines, wherein a pipeline is connected with gas chromatograph injection port, between gas chromatograph and decompression pressure regulator valve group II, be provided with pressure regulating valve II, gas chromatograph is connected with waste gas neutralization bucket by gas chromatograph exhausting pipeline, another pipeline is connected with gas meter, between gas meter and decompression pressure regulator valve group II, be provided with pressure regulating valve I, gas meter is connected with waste gas neutralization bucket by exhausting pipeline, described cryogenic freezing liquid container can bear subzero 100 ℃ of low temperature cool-bags and fill cryogenic freezing liquid, the rotating freeze pipe group of described Luo and gas-liquid separator are placed in cryogenic freezing liquid container, thermometer is also installed in cryogenic freezing liquid container.
In the rotating freeze pipe group of described Luo and gas-liquid separator connection procedure, be provided with tensimeter, the pressure limit that can accurately show is minimum 0MPa, maximum 5MPa; The rotating freeze pipe group of described Luo is made by the high pressure stainless steel pipes that can bear 5MPa, the corrosion of resistance to ammonia; The pressure limit that described decompression pressure regulator valve group regulates is minimum 1MPa, maximum 5MPa.
Compress the methods of experiments that freezing reclaims ammonia in LED mix waste gas, the method comprises following step:
(1) mix the composition of source of the gas: the mixed gas bottle being formed by nitrogen 60%～75%, hydrogen 25%～20%, ammonia 15%～5% of a 40L of configuration, pressure is 5.0MPa, substitutes the mixed gas source of the gas after similar LED production discharging waste gas and compression;
(2) composition of refrigerated source: be mixed into low-temperature refrigerant by ethanol and dry ice, can regulate arbitrarily between-72 ℃～-0 ℃, to substitute deep freeze refrigerator and refrigerated source;
(3) composition of subcooling condenser: be made into Luo by 1/4th stainless-steel seamless pipes rotating, be arranged in a low-temperature (low temperature) vessel, threading is mixed into low-temperature refrigerant by ethanol and dry ice, the condenser that formation is comprised of refrigerant, the rotating stainless-steel tube of Luo, can between-72 ℃～-0 ℃, regulate arbitrarily temperature, for the ammonia of condensation mixed gas, investigate the condensation ratio of ammonia under various temperature conditions;
(4) composition of gas-liquid separator: by the stainless steel pipes of DN25, form a duct-type gas-liquid separator, / 2nd places, middle part are the entrance of gas-liquid mixture after condensation, top is the floss hole of uncondensed gas, bottom is between the storage of ammonia after condensation, for separating of combination gas through condensed liquefied ammonia and solidifying gas nitrogen and hydrogen;
(5) detection of emptying gas component: the not solidifying gas after separation, from separation vessel is discharged, leads to gas chromatograph, and the ratio of the nitrogen in test Exhaust Gas, hydrogen, ammonia, to confirm the various data of Exhaust Gas under various process conditions;
(6) collection of emptying gas absorbs: the not solidifying gas after separation, from separation vessel is discharged, discharges water and adds a small amount of dilute sulfuric acid via a Plastic Drum, and PH, in 6, guarantees can neutralization reaction become ammonium sulfate after emptying waste gas enters, free from environmental pollution.
The composition of described mixing source of the gas is to be undertaken by the method for gravimetric method preparation gas, after preparing, adopts molar volume of gas to calculate the volumetric concentration of each component by gravimetric method again.
The composition mixing gas cylinder of described mixing source of the gas, with pressure-regulating valve, can be 0.1MPa in pressure minimum, is to the maximum between 5.0MPa and regulates, and with the large-scale compressor pressure of simulation, regulates.
The detection of described emptying gas component is to form with a gas chromatography instrument being comprised of the gas chromatographic column of 3 meters of thermal conductivity detector (TCD), two six-way valves, two diameters 1/8th, length.
Last in described gas chromatographic column is pre-column, and the preseparation chromatography post that filler is comprised of 5A molecular sieve can be effectively separated by nitrogen, hydrogen; Latter one in gas chromatographic column is ammonia separating column, and filler is the chromatogram pillar of being filled by porapad-Q, can ammonia is separated.
The detection of described emptying gas component, can carry out nitrogen, hydrogen, ammonia in mixed gas separation and accurately detect from 0.1%～100%.
Utilize this methods of experiments, can be by the mixed gas being formed by nitrogen 60%～75%, hydrogen 25%～20%, ammonia 15%～5%, pressure between 0.1MPa～5.0MPa regulates, refrigerant condensation between-72 ℃～-0 ℃, accurate detection through nitrogen, hydrogen, ammonia from 0.1%～100% gas chromatography, measures the various parameters such as compressor pressure scope, refrigerating machine chilling temperature scope, Ammonia recovery rate.
The invention has the beneficial effects as follows: by the inventive method, use compression freezing technique to reclaim a small amount of ammonia in mixed gas, in Process Planning, verify the correctness of metallization processes software measuring and calculating, prevent the deviation that may produce in design and actual implementation process, improve design accuracy, reduce investment loss, thereby obtain the data of testing under various pressure, temperature, flow in compression freezing removal process for mixed gas, for bigger device provides the design data of science; Can verify well the authenticity of chemistry calculation software data and revise, method be novel, reduced investment, experiment is fast, data science is true.
Accompanying drawing explanation
Fig. 1 is the structural drawing of system of the present invention;
Wherein: 1, hybrid standard gas cylinder, 2, decompression pressure regulator valve group I, 3, tensimeter, 4, cryogenic freezing liquid container, 5, cryogenic freezing liquid, 6, the rotating freeze pipe group of Luo, 7, gas-liquid separator, 8, thermometer, 9, decompression pressure regulator valve group II, 10, gas meter, 11, pressure regulating valve I, 12, pressure regulating valve II, 13, gas chromatograph, 14, exhausting pipeline, 15, gas chromatograph exhausting pipeline, 16, waste gas neutralization bucket.
Embodiment
The present embodiment is a kind of experimental provision and verification method thereof that freezing is recycled ammonia in LED discharging waste gas that compress, and it comprises: hybrid standard gas cylinder (1), decompression pressure regulator valve group, tensimeter (3), cryogenic freezing liquid container (4), cryogenic freezing liquid (5), the rotating freeze pipe group of Luo (6), gas-liquid separator (7), thermometer (8), gas meter (10), pressure regulating valve, gas chromatograph (13), waste gas neutralization bucket (16).
As shown in Figure 1, described hybrid standard gas cylinder (1) is by nitrogen, hydrogen, ammonia carries out mixed configuration in proportion, replace compression gas cylinder for experiment, top pressure 20MPa, hybrid standard gas cylinder (1) is connected with decompression pressure regulator valve group I (2), decompression pressure regulator valve group I (2) is connected with the rotating freeze pipe group of Luo (6), the rotating freeze pipe group of Luo (6) is connected with gas-liquid separator (7), gas-liquid separator (7) is connected with decompression pressure regulator valve group II (9), decompression pressure regulator valve group II (9) outlet is provided with two pipelines, wherein a pipeline is connected with gas chromatograph (13) injection port, between gas chromatograph (13) and decompression pressure regulator valve group II (9), be provided with pressure regulating valve II (12), gas chromatograph (13) is connected with waste gas neutralization bucket (16) by gas chromatograph exhausting pipeline (15), another pipeline is connected with gas meter (10), between gas meter (10) and decompression pressure regulator valve group II (9), be provided with pressure regulating valve I (11), gas meter (10) is connected with waste gas neutralization bucket (16) by exhausting pipeline (14), described cryogenic freezing liquid container (4) can bear subzero 100 ℃ of low temperature cool-bags and fill cryogenic freezing liquid (5), the rotating freeze pipe group of described Luo (6) is placed in cryogenic freezing liquid container (4) with gas-liquid separator (7), thermometer (8) is also installed in cryogenic freezing liquid container (4), in the rotating freeze pipe group of described Luo (6) and gas-liquid separator (7) connection procedure, be provided with tensimeter (3), the pressure limit that can accurately show is minimum 0MPa, maximum 5MPa.
Compress the methods of experiments that freezing reclaims ammonia in LED mix waste gas, the method comprises following step:
(1) mix the composition of source of the gas: the mixed gas bottle being formed by nitrogen 60%～75%, hydrogen 25%～20%, ammonia 15%～5% of a 40L of configuration, pressure is 5.0MPa, substitutes the mixed gas source of the gas after similar LED production discharging waste gas and compression;
(2) composition of refrigerated source: be mixed into low-temperature refrigerant by ethanol and dry ice, can regulate arbitrarily between-72 ℃～-0 ℃, to substitute deep freeze refrigerator and refrigerated source;
(3) composition of subcooling condenser: be made into Luo by 1/4th stainless-steel seamless pipes rotating, be arranged in a low-temperature (low temperature) vessel, threading is mixed into low-temperature refrigerant by ethanol and dry ice, the condenser that formation is comprised of refrigerant, the rotating stainless-steel tube of Luo, can between-72 ℃～-0 ℃, regulate arbitrarily temperature, for the ammonia of condensation mixed gas, investigate the condensation ratio of ammonia under various temperature conditions;
(4) composition of gas-liquid separator: by the stainless steel pipes of DN25, form a duct-type gas-liquid separator, / 2nd places, middle part are the entrance of gas-liquid mixture after condensation, top is the floss hole of uncondensed gas, bottom is between the storage of ammonia after condensation, for separating of combination gas through condensed liquefied ammonia and solidifying gas nitrogen and hydrogen;
(5) detection of emptying gas component: the not solidifying gas after separation, from separation vessel is discharged, leads to gas chromatograph, and the ratio of the nitrogen in test Exhaust Gas, hydrogen, ammonia, to confirm the various data of Exhaust Gas under various process conditions;
(6) collection of emptying gas absorbs: the not solidifying gas after separation, from separation vessel is discharged, discharges water and adds a small amount of dilute sulfuric acid via a Plastic Drum, and PH, in 6, guarantees can neutralization reaction become ammonium sulfate after emptying waste gas enters, free from environmental pollution.
Claims (7)
1. one kind is compressed the experimental provision that freezing reclaims ammonia in LED mix waste gas, it comprises: hybrid standard gas cylinder, decompression pressure regulator valve group, tensimeter, cryogenic freezing liquid container, cryogenic freezing liquid, the rotating freeze pipe group of Luo, gas-liquid separator, thermometer, gas meter, pressure regulating valve, gas chromatograph, waste gas neutralization bucket, it is characterized in that described hybrid standard gas cylinder is connected with decompression pressure regulator valve group I, decompression pressure regulator valve group I is connected with the rotating freeze pipe group of Luo, the rotating freeze pipe group of Luo is connected with gas-liquid separator, gas-liquid separator is connected with decompression pressure regulator valve group II, the outlet of decompression pressure regulator valve group II is provided with two pipelines, wherein a pipeline is connected with gas chromatograph injection port, between gas chromatograph and decompression pressure regulator valve group II, be provided with pressure regulating valve II, gas chromatograph is connected with waste gas neutralization bucket by gas chromatograph exhausting pipeline, another pipeline is connected with gas meter, between gas meter and decompression pressure regulator valve group II, be provided with pressure regulating valve I, gas meter is connected with waste gas neutralization bucket by exhausting pipeline, described cryogenic freezing liquid container can bear subzero 100 ℃ of low temperature cool-bags and fill cryogenic freezing liquid, the rotating freeze pipe group of described Luo and gas-liquid separator are placed in cryogenic freezing liquid container, thermometer is also installed in cryogenic freezing liquid container.
2. compress the methods of experiments that freezing reclaims ammonia in LED mix waste gas, it is characterized in that: the method comprises following step:
(1) mix the composition of source of the gas: the mixed gas bottle being formed by nitrogen 60%～75%, hydrogen 25%～20%, ammonia 15%～5% of a 40L of configuration, pressure is 5.0MPa, substitutes the mixed gas source of the gas after similar LED production discharging waste gas and compression;
(2) composition of refrigerated source: be mixed into low-temperature refrigerant by ethanol and dry ice, can regulate arbitrarily between-72 ℃～-0 ℃, to substitute deep freeze refrigerator and refrigerated source;
(3) composition of subcooling condenser: be made into Luo by 1/4th stainless-steel seamless pipes rotating, be arranged in a low-temperature (low temperature) vessel, threading is mixed into low-temperature refrigerant by ethanol and dry ice, the condenser that formation is comprised of refrigerant, the rotating stainless-steel tube of Luo, can between-72 ℃～-0 ℃, regulate arbitrarily temperature, for the ammonia of condensation mixed gas, investigate the condensation ratio of ammonia under various temperature conditions;
(4) composition of gas-liquid separator: by the stainless steel pipes of DN25, form a duct-type gas-liquid separator, / 2nd places, middle part are the entrance of gas-liquid mixture after condensation, top is the floss hole of uncondensed gas, bottom is between the storage of ammonia after condensation, for separating of combination gas through condensed liquefied ammonia and solidifying gas nitrogen and hydrogen;
(5) detection of emptying gas component: the not solidifying gas after separation, from separation vessel is discharged, leads to gas chromatograph, and the ratio of the nitrogen in test Exhaust Gas, hydrogen, ammonia, to confirm the various data of Exhaust Gas under various process conditions;
(6) collection of emptying gas absorbs: the not solidifying gas after separation, from separation vessel is discharged, discharges water and adds a small amount of dilute sulfuric acid via a Plastic Drum, and PH, in 6, guarantees can neutralization reaction become ammonium sulfate after emptying waste gas enters, free from environmental pollution.
3. a kind of methods of experiments that freezing reclaims ammonia in LED mix waste gas of compressing according to claim 2, the composition that it is characterized in that described mixing source of the gas is to be undertaken by the method for gravimetric method preparation gas, after preparing by gravimetric method, adopt molar volume of gas to calculate again the volumetric concentration of each component.
4. a kind of methods of experiments that freezing reclaims ammonia in LED mix waste gas of compressing according to claim 2, the composition mixing gas cylinder that it is characterized in that described mixing source of the gas, with pressure-regulating valve, can be 0.1MPa in pressure minimum, be to the maximum between 5.0MPa and regulate, with the large-scale compressor pressure of simulation, regulate.
5. a kind of methods of experiments that freezing reclaims ammonia in LED mix waste gas of compressing according to claim 2, it is characterized in that the detection of described emptying gas component, is to form with a gas chromatography instrument being comprised of the gas chromatographic column of 3 meters of thermal conductivity detector (TCD), two six-way valves, two diameters 1/8th, length.
6. a kind ofly according to claim 5 compress the methods of experiments that freezing reclaims ammonia in LED mix waste gas, it is characterized in that last in described gas chromatographic column is pre-column, the preseparation chromatography post that filler is comprised of 5A molecular sieve, can be effectively separated by nitrogen, hydrogen; Latter one in gas chromatographic column is ammonia separating column, and filler is the chromatogram pillar of being filled by porapad-Q, can ammonia is separated.
7. a kind of methods of experiments that freezing reclaims ammonia in LED mix waste gas of compressing according to claim 2, it is characterized in that the detection of described emptying gas component, nitrogen, hydrogen, ammonia in mixed gas can be carried out to separation and accurately detect from 0.1%～100%.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108265279A (en) * | 2016-12-30 | 2018-07-10 | 苏州纳维科技有限公司 | Metal Ga efficient utilization devices and method |
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| JPS5418499A (en) * | 1977-07-12 | 1979-02-10 | Toyo Engineering Corp | Condensation and separation of ammonia |
| CN102679688A (en) * | 2012-05-25 | 2012-09-19 | 贵州开磷（集团）有限责任公司 | Technology for recycling ammonia from synthesis ammonia tail gas |
| CN102963910A (en) * | 2012-11-26 | 2013-03-13 | 苏州金宏气体股份有限公司 | Method for recovering and reutilizing waste ammonia gas in LED (light-emitting diode) manufacturing through compression method |
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- 2013-11-15 CN CN201310577187.7A patent/CN103675119A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5418499A (en) * | 1977-07-12 | 1979-02-10 | Toyo Engineering Corp | Condensation and separation of ammonia |
| CN102679688A (en) * | 2012-05-25 | 2012-09-19 | 贵州开磷（集团）有限责任公司 | Technology for recycling ammonia from synthesis ammonia tail gas |
| CN102963910A (en) * | 2012-11-26 | 2013-03-13 | 苏州金宏气体股份有限公司 | Method for recovering and reutilizing waste ammonia gas in LED (light-emitting diode) manufacturing through compression method |
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| Title |
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| 吴江红 等: "超高纯氨杂质分析", 《低温与特气》 * |
| 方华 等: "氦离子色谱仪在超高纯氨分析中的应用", 《低温与特气》 * |
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| 汤剑波 等: "MOCVD 尾气中氨气吸附回收的探讨与研究", 《低温与特气》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108265279A (en) * | 2016-12-30 | 2018-07-10 | 苏州纳维科技有限公司 | Metal Ga efficient utilization devices and method |
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Application publication date: 20140326 |