CN100531846C - Recovery cyclic utilization method and apparatus for recovering discharged alkaline air in process of production of silane with magnesium silicide method - Google Patents
Recovery cyclic utilization method and apparatus for recovering discharged alkaline air in process of production of silane with magnesium silicide method Download PDFInfo
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- CN100531846C CN100531846C CNB2008100246792A CN200810024679A CN100531846C CN 100531846 C CN100531846 C CN 100531846C CN B2008100246792 A CNB2008100246792 A CN B2008100246792A CN 200810024679 A CN200810024679 A CN 200810024679A CN 100531846 C CN100531846 C CN 100531846C
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Abstract
The invention discloses a recovery and recycling method of the discharged ammonia during the silane production process by the process of magnesium silicide method, the process includes the steps that: the generated residues during the silane production process by the process of magnesium silicide method are discharged into an ammonia recovery tank; when the temperature and the pressure of the residues in the ammonia recovery tank increase, the ammonia escapes from the residues to reach a pressure at 0.1MPa, the ammonia enters a condenser after the dust filtration and the silane removal; the condenser is refrigerated to liquefy the ammonia; and then the liquid ammonia is arranged in a liquid ammonia storage tank for recycling. At the same time, the invention also discloses a device to implement the method of the invention. The method of the invention adopts the low-temperature technology for recovering the gaseous ammonia to be converted into the liquid ammonia to carry out the recycling, which can not only save the consumption of the liquid ammonia, but can also protect the atmospheric environment. The device of the invention has simple structure, low manufacturing cost and convenient installation.
Description
Technical field
The present invention relates to the recovery method of ammonia in a kind of Chemical Manufacture, is the recycle and reuse method and the special equipment of the ammonia that discharges in a kind of magnesium silicide method explained hereafter silane process specifically.
Technical background
The ammonia recovery technology is used for circulation cooling injection column plate technology, isobaric composite absorption column plate technology, low resistance film jet tray technology being arranged during chemical fertilizer industry produces more, is applied to the recovery of carbonization ammonia, isobaric recovery tower, copper respectively and washes regeneration ammonia recovery tower, ammonia still.China's utility model patent " gas and synthetic ammonia purge ammonia recovery unit " (patent No. 200620122545) discloses establishing and method of this type of ammonia recovery.
Magnesium silicide method is produced silane, use liquid ammonia to make medium, and the water content of ammonia is very low, and after silane extracted usually, in the residue discharge process such as greening magnesium, ammonia also discharged to atmosphere thereupon, severe contamination environment, wasted resource.Above-mentioned disclosed prior art can not be used for the recovery of magnesium silicide method ammonia that technical process is discharged.
Summary of the invention
Technical problem to be solved by this invention is to fill up the blank of prior art, and the recycle and reuse method of the ammonia that discharges in a kind of magnesium silicide method explained hereafter silane process is provided.This method adopts cryogenic technique that the gaseous ammonia that reclaims is changed into liquid ammonia and recycles, has both saved the consumption of liquefied ammonia, has protected atmospheric environment again.Simultaneously, the present invention also provides a kind of special equipment of implementing this method.
The basic principle of the inventive method: because the silane reaction stove is made medium with liquefied ammonia, the ammonia that end reaction generates and the liquefied ammonia of use are blended in the residue that magnesium chloride is a main component.Therefore, the residue of discharging at first enters the ammonia recycling can, and ammonia slowly releases along with the rising of temperature in jar, and when the jar internal pressure reached certain pressure, ammonia entered refrigeration compressing apparatus, and refrigerant compression is a liquefied ammonia.Owing to contain silane dust and residual silane in the ammonia of production of silane discharging, so before to the ammonia refrigerant compression, will take control techniques.
The recycle and reuse method of the ammonia that discharges in the magnesium silicide method explained hereafter silane process of the present invention, its processing step is:
1, opens silane reaction stove residue outlet exhaust-valve, the residue that produces in the magnesium silicide method explained hereafter silane process is entered the ammonia recycling can; When residue all enters the ammonia recycling can, close residue outlet exhaust-valve;
2, the residue temperature rises in the ammonia recycling can, and ammonia is overflowed from the slag body, the increased pressure in the ammonia recycling can, and pressure arrives 0.1MPa (gauge pressure), opens the ammonia recycling can top valve of giving vent to anger, and ammonia dedusting after filtration, removes that silane is laggard goes into condenser; Again with residual residue discharging in the ammonia recycling can;
3, start refrigeration compressor, make condenser temperature be lower than-33.5 ℃, make ammonia liquefaction;
4, open the condensator outlet valve, liquefied ammonia flows into liquid ammonia storage tank, and is standby;
When 5, producing silane, be stored in liquefied ammonia in the liquid ammonia storage tank and enter the silane reaction stove and recycle.
The recycle and reuse equipment of the ammonia that discharges in the magnesium silicide method explained hereafter silane process of the present invention, constitute by ammonia recycling can, condenser, refrigeration compressor and liquid ammonia storage tank, it is characterized in that: the slag inlet on ammonia recycling can top connects silane reaction stove residue outlet exhaust-valve, ammonia recycling can top is provided with at least one gas outlet, each gas outlet is connected with the condenser air inlet by each corresponding dust filter unit, refrigeration compressor freezes to condenser, and ammonia recycling can bottom is provided with the residue floss hole; The outlet of condenser liquefied ammonia connects liquid ammonia storage tank, and the outlet of liquid ammonia storage tank connects the silane reaction stove.
Described dust filter unit is a hollow pipe, and two ends add flange and connect, and interior dress contains the silicate rock wool of the acetamide aqueous solution.
Described ammonia recycling can is provided with assisted heating device.
The inventive method adopts cryogenic technique recovery gaseous ammonia to change into liquid ammonia and recycles, has promptly saved the consumption of liquefied ammonia, has protected atmospheric environment.Present device, simple in structure, cheap for manufacturing cost, easy for installation.
Description of drawings
Fig. 1 is the inventive method flow process and device structure schematic block diagram;
Fig. 2 is an ammonia recycling can structural representation;
Fig. 3 is ammonia recycling can and dust precipitator structure vertical view;
The specific embodiment
Below in conjunction with accompanying drawing the present invention is described in further details.
Embodiment: as shown in Figure 1, 2, 3, the recycle and reuse equipment of the ammonia that discharges in the magnesium silicide method explained hereafter silane process of the present invention, constitute by ammonia recycling can 2, condenser 5, refrigeration compressor 6 and liquid ammonia storage tank 8, it is characterized in that: the slag inlet on ammonia recycling can top connects silane reaction stove residue outlet exhaust-valve 1, the monnolithic case of ammonia recycling can is circular pot type structure, and the gaseous ammonia of reacting furnace discharging enters (pressure that relies on the silane producer) from the top of tank body.Ammonia recycling can top is provided with four valves 3 of giving vent to anger, each air outlet valve door is connected with the condenser air inlet by each corresponding dust filter unit 4, therefore four dust filter units are parallel setting, ammonia recycling can bottom is provided with heating tube as assisted heating device 10, and its bottom is provided with residue floss hole 11.Dust filter unit 4 adopts φ 10～15 stainless steels or carbon steel seamless pipe to do body, and two ends add flange and connect, the silicate rock wool of the interior dress acetamide aqueous solution.Adopt industrial silicon hydrochlorate rock wool, soaked 24 hours, use washed with de-ionized water 3～4 times, immerse in the acetamide saturated solution, soak and dry the body of packing into after 3～4 hours naturally with 1%HCl watery hydrochloric acid.It not only can Chalk-dust filtering, also can absorb a small amount of silane of coming with gaseous ammonia simultaneously.Filter is arranged to parallel way, and a part is used, and a part is changed in addition.This does not need to open tank body and operates.Refrigeration compressor is used for the condenser refrigeration, and the outlet of condenser liquefied ammonia connects liquid ammonia storage tank, and the outlet of liquid ammonia storage tank connects the silane reaction stove.
As shown in Figure 1, the recycle and reuse method of the ammonia that discharges in the magnesium silicide method explained hereafter silane process of the present invention, its processing step is:
1. open silane reaction stove residue outlet exhaust-valve 1, the residue that produces in the magnesium silicide method explained hereafter silane process is all entered ammonia recycling can 2, close residue outlet exhaust-valve 1 then.
2. the residue temperature rises (in case of necessity in the ammonia recycling can, can heat the residue in the ammonia recycling can with the assisted heating device heating), increased pressure, ammonia is overflowed from the slag body, arrive 0.1MPa (gauge pressure), open the recycling can valve 3 of giving vent to anger, ammonia through dust filter unit 4 dedustings, remove that silane is laggard goes into condenser 5.Again residual residue in the ammonia recycling can is discharged through residue floss hole 11.
3. start refrigeration compressor 6, make condenser 5 temperature be lower than-33.5 ℃, make ammonia liquefaction.Liquefied ammonia reaches a certain amount of back or the recycling can internal pressure is lower than 0.02MPa (gauge pressure) in the condenser, closes the recycling can valve 3 of giving vent to anger.
4. open condensator outlet valve 7, liquefied ammonia flows into liquid ammonia storage tank 8.
5. open liquid ammonia storage tank outlet valve 9, liquefied ammonia enters the silane reaction stove and recycles.
Claims (4)
1, the recycle and reuse method of the ammonia that discharges in a kind of magnesium silicide method explained hereafter silane process, its processing step is:
A, the residue that produces in the magnesium silicide method explained hereafter silane process is entered the ammonia recycling can;
B, the residue temperature rises in the ammonia recycling can, and ammonia is overflowed from the slag body, and ammonia recycling can internal pressure increases, and arrives 0.1MPa, sends ammonia dedusting after filtration, after removing silane into condenser; Again with residual residue discharging in the ammonia recycling can;
C, start refrigeration machine, make condenser temperature be lower than-33.5 ℃, make ammonia liquefaction;
D, with the liquefied ammonia liquid ammonia storage tank of packing into, standby;
E, when producing silane, be stored in liquefied ammonia in the liquid ammonia storage tank and send into the silane reaction stove and recycle.
2, the recycle and reuse equipment of the ammonia that discharges in a kind of magnesium silicide method explained hereafter silane process, comprise ammonia recycling can, condenser, refrigeration compressor and liquid ammonia storage tank, it is characterized in that: the slag inlet on ammonia recycling can top connects silane reaction stove residue outlet exhaust-valve, ammonia recycling can top is provided with at least one gas outlet, each gas outlet is connected with the condenser air inlet by each corresponding dust filter unit, refrigeration compressor freezes to condenser, and ammonia recycling can bottom is provided with the residue floss hole; The outlet of condenser liquefied ammonia connects liquid ammonia storage tank, and the outlet of liquid ammonia storage tank connects the silane reaction stove.
3, according to the recycle and reuse equipment of the ammonia that discharges in the described magnesium silicide method explained hereafter of the claim 2 silane process, it is characterized in that: described dust filter unit is a hollow pipe, and two ends add flange and connect, and interior dress contains the silicate rock wool of the acetamide aqueous solution.
4, according to the recycle and reuse equipment of the ammonia that discharges in the described magnesium silicide method explained hereafter of the claim 2 silane process, it is characterized in that: described ammonia recycling can is provided with assisted heating device.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2008100246792A CN100531846C (en) | 2008-04-01 | 2008-04-01 | Recovery cyclic utilization method and apparatus for recovering discharged alkaline air in process of production of silane with magnesium silicide method |
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| CNB2008100246792A CN100531846C (en) | 2008-04-01 | 2008-04-01 | Recovery cyclic utilization method and apparatus for recovering discharged alkaline air in process of production of silane with magnesium silicide method |
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| CN100531846C true CN100531846C (en) | 2009-08-26 |
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| CNB2008100246792A Expired - Fee Related CN100531846C (en) | 2008-04-01 | 2008-04-01 | Recovery cyclic utilization method and apparatus for recovering discharged alkaline air in process of production of silane with magnesium silicide method |
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101798085B (en) * | 2010-04-21 | 2012-10-17 | 江苏扬农化工集团有限公司 | Process for preparing silane by magnesium silicide method |
| CN101817541B (en) * | 2010-04-21 | 2012-03-21 | 江苏扬农化工集团有限公司 | Method and device for separating magnesium chloride hexammoniate during silane production by the magnesium silicide method |
| CN101928012B (en) * | 2010-09-13 | 2012-01-11 | 化学工业第二设计院宁波工程有限公司 | Energy utilization method in low-temperature liquid ammonia recovery process |
| CN103073026B (en) * | 2013-02-07 | 2015-07-01 | 上海兄弟微电子技术有限公司 | Ammonia gas recovery system |
| CN106512661A (en) * | 2016-10-28 | 2017-03-22 | 浙江海富海洋生物科技有限公司 | Method and device for circulating ammonia gas in hydroxyapatite preparation process |
| CN109759412B (en) * | 2019-02-28 | 2020-11-06 | 北京真空电子科技有限公司 | Recovery device |
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