CN102320623A - Purification device and purification method for electronic grade ultra-pure ammonia - Google Patents
Purification device and purification method for electronic grade ultra-pure ammonia Download PDFInfo
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- CN102320623A CN102320623A CN201110309452A CN201110309452A CN102320623A CN 102320623 A CN102320623 A CN 102320623A CN 201110309452 A CN201110309452 A CN 201110309452A CN 201110309452 A CN201110309452 A CN 201110309452A CN 102320623 A CN102320623 A CN 102320623A
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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
- C01C1/024—Purification
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Abstract
The invention discloses a purification device for electronic grade ultra-pure ammonia. The purification device comprises a liquid ammonia storage tank, a liquid ammonia pump, a carburetor, a degreaser, rectifying towers, a terminal purifier, a condenser and a product storage tank; the rectifying towers comprise a first rectifying tower and a second rectifying tower; the liquid ammonia pump is connected to the liquid ammonia storage tank and used for pumping liquid ammonia to the carburetor; the output of the carburetor is connected to the degreaser; the output of the degreaser is connected to the upper middle part of the first rectifying tower; the output of the tower top of the first rectifying tower is connected to a tower kettle of the second rectifying tower; the output of the tower top of the second rectifying tower is connected to the terminal purifier; the output of the terminal purifier is connected to the condenser; and the output of the condenser is connected to the product storage tank. In addition, the invention also provides a purification method for purifying the electronic grade ultra-pure ammonia by using the purification device. By using the device and the method, the limitation of the traditional ultra-pure ammonia refining process flow is avoided, the refining process of the ultra-pure ammonia is simplified, the energy consumption of the whole production process is greatly reduced, and the production efficiency is improved.
Description
Technical field
The present invention relates to the purifying plant and the method for purification thereof of gas, particularly a kind of purifying plant of electronic-grade ultra-pure ammonia and method of purification thereof.
Background technology
In existing ultra-pure ammonia purifying industrial device; The operational path that adopts is similar basically; The purification devices of mentioned 7N electronic-grade ultra-pure ammonia among the disclosed electronic-grade ultra-pure ammonia of utility model patent CN200920235917.4 purifying extraction element and the application for a patent for invention CN201010140687.0 for example; Be raw material all, through the vaporizer vaporization, then through the oil eliminator oil removing with industrial liquefied ammonia; Behind the molecular sieve adsorber drying and dehydrating, directly get into rectifying tower again, the purifier degree of depth dewaters and obtains the finished product the rectifying products obtained therefrom through the terminal again.In this technological process, though can obtain high purity product, its complex technical process at last; Ammonia is through repeatedly vaporization and condensation, and process such as absorption consume electric power such as need regenerate is excessive, and this is for today of energy growing tension; Be very not energy-conservation, cause the products production cost too high; And before rectifying, dry adsorption unit is set, and bring entering rectifying tower such as new granule foreign easily into, cause the fluctuation of quality product.
Summary of the invention
Problem to be solved by this invention just provides a kind of purifying plant of electronic-grade ultra-pure ammonia; Broken through the restriction of traditional ultra-pure ammonia process for refining flow process; Simplify the process for refining of ultra-pure ammonia, greatly reduced the energy consumption of whole production technology, and improved production efficiency.
In order to solve the problems of the technologies described above; The present invention adopts following technical scheme: the purifying plant of electronic-grade ultra-pure ammonia; It is characterized in that: comprise liquefied ammonia storage tank, ammonia pump, vaporizer, oil eliminator, rectifying tower, terminal purifier, condensing surface and product storage tank, said rectifying tower comprises first rectifying tower and second rectifying tower, and ammonia pump is linked in the liquefied ammonia storage tank and with liquefied ammonia and squeezes into vaporizer; Vaporizer output is connected on the oil eliminator; On oil eliminator output was connected in the first rectifying Tata, first rectifying tower was connected to the second rectifying Tata still from cat head output, and second rectifying tower is connected on the purifier of terminal from cat head output; Terminal purifier output is connected on the condensing surface, and condensing surface output is connected on the product storage tank.
Further; The cat head of said first rectifying tower is provided with first overhead condenser that is communicated with first rectifying tower; First overhead condenser output is connected to second rectifying tower, is provided with second overhead condenser that is communicated with second rectifying tower at the cat head of second rectifying tower, and second overhead condenser is exported and is connected to second rectifying tower and product storage tank; At the bottom of the tower of first rectifying tower, be provided with first tower bottom reboiler that is communicated with first rectifying tower; The output of first tower bottom reboiler is connected to first rectifying tower, at the bottom of the tower of second rectifying tower, is provided with second tower bottom reboiler that is communicated with second rectifying tower, and the output of second tower bottom reboiler is connected to second rectifying tower.
Further, the also parallelly connected output of said first tower bottom reboiler and second tower bottom reboiler is connected to the liquefied ammonia withdrawing can.
Further, said liquefied ammonia withdrawing can is connected the bottom of first tower bottom reboiler and the bottom of second tower bottom reboiler.The liquefied ammonia of residual high concentration impurities is reclaimed.
Further, said liquefied ammonia withdrawing can is also connected with the bottom of vaporizer.The liquefied ammonia of residual high concentration impurities is reclaimed.
The present invention also provides and has used the purify method of purification of electronic-grade ultra-pure ammonia of above-mentioned purifying plant in addition, it is characterized in that, may further comprise the steps:
1) through ammonia pump the liquefied ammonia in the liquefied ammonia storage tank is squeezed into the vaporizer vaporization;
2) ammonia after the vaporizer vaporization is sent into the oil eliminator oil removing; Directly send into first rectifying tower after the oil removing and carry out the separation of weight component; After the first rectifying tower cat head is through first overhead condenser, remove the light constituent impurity of incoagulability; The liquefied ammonia that contains heavy constituent impurity in first tower bottom reboiler is discharged in the liquefied ammonia withdrawing can, and the first rectifying tower cat head is sent into second rectifying tower through the liquefied ammonia of condensation and further removed weight component impurity;
3) after the second rectifying tower cat head is through second overhead condenser, remove the light constituent impurity of incoagulability; The liquefied ammonia that contains heavy constituent impurity in second tower bottom reboiler is discharged in the liquefied ammonia withdrawing can; Whether detection is qualified through the liquefied ammonia of second overhead condenser; If the qualified product storage tank of then packing into,, finally obtain the qualified ultra-pure ammonia product storage tank of packing into if defectively then send into the terminal purifier together and carry out micro-removal of impurities with the ammonia of the second rectifying Tata still.
Further, the working temperature of said vaporizer is controlled at 50 ℃～80 ℃, and WP is controlled between 1Mpa～1.5Mpa, and the boil-off rate of liquefied ammonia is at 180kg/h～230kg/h.
Further, the work liquid level is 0.5m～0.8m in the said vaporizer.
Further, the working temperature of said first rectifying tower and second rectifying tower is controlled at 20 ℃～80 ℃, and WP is controlled at 0.9Mpa～1.3Mpa.
Further, the height of said first rectifying tower and second rectifying tower is 23m～26m.
After adopting technique scheme, the present invention has following advantage: adopt two tower rectifying, remove light constituent and heavy constituent impurity respectively, fully guaranteed the purity of product ammonia; Save the dry adsorption unit before the rectifying, reduced energy consumption on the one hand, also avoided on the other hand bringing into rectifying tower such as new granule foreign, thereby made the whole technology can steady running, avoided quality product to produce fluctuation.
Description of drawings
Below in conjunction with accompanying drawing the present invention is described further:
Fig. 1 is the structural representation of an embodiment of the present invention.
Embodiment
The structural representation of an embodiment of the present invention as shown in Figure 1; The purifying plant of electronic-grade ultra-pure ammonia comprises liquefied ammonia storage tank 1, ammonia pump 2, vaporizer 3, oil eliminator 4, rectifying tower 5, terminal purifier 6, condensing surface 7 and product storage tank 8, and ammonia pump is linked in the liquefied ammonia storage tank and with liquefied ammonia and squeezes into vaporizer; Vaporizer output is connected on the oil eliminator; On oil eliminator output was connected in the first rectifying Tata, first rectifying tower was connected to the second rectifying Tata still from cat head output, and second rectifying tower is connected on the purifier of terminal from cat head output; Terminal purifier output is connected on the condensing surface, and condensing surface output is connected on the product storage tank.In the present embodiment; Said rectifying tower comprises first rectifying tower 51 and second rectifying tower 52; Oil eliminator output is connected to first rectifying tower, and the output of first rectifying tower is connected to second rectifying tower, and the output of second rectifying tower is connected to the terminal purifier; Cat head at first rectifying tower is provided with first overhead condenser 511 that is communicated with first rectifying tower; First overhead condenser output is connected to second rectifying tower, is provided with second overhead condenser, 521, the second overhead condensers that are communicated with second rectifying tower at the cat head of second rectifying tower and exports and be connected to second rectifying tower; At the bottom of the tower of first rectifying tower, be provided with first tower bottom reboiler 512 that is communicated with first rectifying tower; The output of first tower bottom reboiler is connected to first rectifying tower, at the bottom of the tower of second rectifying tower, is provided with second tower bottom reboiler, 522, the second tower bottom reboilers output that is communicated with second rectifying tower and is connected to second rectifying tower.
In addition, first tower bottom reboiler and second tower bottom reboiler also parallel connection output are connected to liquefied ammonia withdrawing can 9, and in the present embodiment, the liquefied ammonia withdrawing can is connected the bottom of first tower bottom reboiler and the bottom of second tower bottom reboiler; Simultaneously, the liquefied ammonia withdrawing can is also connected with the bottom of vaporizer.In the utility model; Getter in the purifier of terminal is according to metal or intermetallic compound and multiple gases effects such as hydrogen, oxygen, nitrogen, carbon monoxide, carbonic acid gas, steam and methane; Generate stable compound or sosoloid; Thereby remove trace impurity, in the present embodiment, the getter that preferred zirconium ferro-vanadium is processed.
The present invention also provides and has used the purify method of purification of electronic-grade ultra-pure ammonia of above-mentioned purifying plant in addition, may further comprise the steps:
1) through ammonia pump 2 liquefied ammonia in the liquefied ammonia storage tank 1 is squeezed into vaporizer 3 vaporizations;
2) ammonia after the vaporizer vaporization is sent into oil eliminator 4 oil removings; Directly send into first rectifying tower 51 after the oil removing and carry out the separation of weight component; After the first rectifying tower cat head is through first overhead condenser 511, remove the light constituent impurity of incoagulability; The liquefied ammonia that contains heavy constituent impurity in first tower bottom reboiler 512 is discharged in the liquefied ammonia withdrawing can 9, and the first rectifying tower cat head is sent into second rectifying tower 52 through the liquefied ammonia of condensation and further removed weight component impurity;
3) after the second rectifying tower cat head is through second overhead condenser 521, remove the light constituent impurity of incoagulability; The liquefied ammonia that contains heavy constituent impurity in second tower bottom reboiler 522 is discharged in the liquefied ammonia withdrawing can; Whether detection is qualified through the liquefied ammonia of second overhead condenser; If the qualified product storage tank 8 of then packing into,, finally obtain the qualified ultra-pure ammonia product storage tank of packing into through condensing surface 7 condensations if defectively then send into terminal purifier 6 together and carry out micro-removal of impurities with the ammonia of the second rectifying Tata still.
In above-mentioned steps, the working temperature of said vaporizer is controlled at 50 ℃～80 ℃, and preferred 50 ℃, 60 ℃, 70 ℃ or 80 ℃, WP is controlled between 1Mpa～1.5Mpa, generally is controlled at 1.2Mpa; The boil-off rate of liquefied ammonia is at 180kg/h～230kg/h, and this working efficiency according to purifying plant is regulated, and generally is controlled at about 210kg/h; And the work liquid level is 0.5m～0.8m in the vaporizer, can control the stable of subsequent technique like this.The working temperature of said in addition first rectifying tower and second rectifying tower is controlled at 20 ℃～80 ℃; Temperature at the bottom of from cat head to tower is variant; Preferably be controlled at 20 ℃, 40 ℃, 60 ℃ or 80 ℃, WP is controlled at 0.9Mpa～1.3Mpa, generally is controlled at 1.0Mpa; Also having the height of first rectifying tower and second rectifying tower is 23m～26m, about preferred 24m.The liquefied ammonia of the residual high concentration impurities of vaporizer and rectifying tower reboiler bottom is recycled in the liquefied ammonia withdrawing can in the whole process.
Traditional ammonia purifying technique thinks that the oxygen impurities composition in the ultra-pure ammonia product is too high, and moisture is difficult to be removed to the ppb order of magnitude; Be because rectifying is difficult to reach the isolating limit requirement of ppb level; Ignored the mutual chemical reaction combination of composition in the ammonia in fact, in industrial ammonia, carbonic acid gas and water that trace exists; Show that through theoretical research the carbon dioxide content in ammonia is at 0～0.5 mol ratio (CO
2/ NH
3) time, the ammoniacal liquor carbonization process can take place, 2NH
3+ CO
2→ NH
2COONH
4, NH
2COONH
4+ 2H
2O+CO
2→ 2NH
4HCO
3, therefore, in rectifying, except considering impurity composition conventional in the ammonia, also should add above-mentioned NH during design
2COONH
4And NH
4HCO
3The separate design of two kinds of components has so just been avoided the product moisture wherein and the problem of oxygen element impurity index exceeding standard after rectifying is come out.So adopt two-tower rectification in the present invention, fully guaranteed the purity of product ammonia.
Claims (10)
1. the purifying plant of electronic-grade ultra-pure ammonia; It is characterized in that: comprise liquefied ammonia storage tank (1), ammonia pump (2), vaporizer (3), oil eliminator (4), rectifying tower (5), terminal purifier (6), condensing surface (7) and product storage tank (8); Said rectifying tower comprises first rectifying tower (51) and second rectifying tower (52); Ammonia pump is linked in the liquefied ammonia storage tank and with liquefied ammonia and squeezes into vaporizer, and vaporizer output is connected on the oil eliminator, on oil eliminator output is connected in the first rectifying Tata; First rectifying tower is connected to the second rectifying Tata still from cat head output; Second rectifying tower is connected on the purifier of terminal from cat head output, and purifier output in terminal is connected on the condensing surface, and condensing surface output is connected on the product storage tank.
2. the purifying plant of electronic-grade ultra-pure ammonia according to claim 1; It is characterized in that: the cat head of said first rectifying tower is provided with first overhead condenser (511) that is communicated with first rectifying tower; The output of first overhead condenser is connected to second rectifying tower; Cat head at second rectifying tower is provided with second overhead condenser (521) that is communicated with second rectifying tower; The output of second overhead condenser is connected to second rectifying tower and product storage tank, at the bottom of the tower of first rectifying tower, is provided with first tower bottom reboiler (512) that is communicated with first rectifying tower, and the output of first tower bottom reboiler is connected to first rectifying tower; At the bottom of the tower of second rectifying tower, be provided with second tower bottom reboiler (522) that is communicated with second rectifying tower, the output of second tower bottom reboiler is connected to second rectifying tower.
3. the purifying plant of electronic-grade ultra-pure ammonia according to claim 2 is characterized in that: said first tower bottom reboiler and second tower bottom reboiler also parallel connection output are connected to liquefied ammonia withdrawing can (9).
4. the purifying plant of electronic-grade ultra-pure ammonia according to claim 3 is characterized in that: said liquefied ammonia withdrawing can is connected the bottom of first tower bottom reboiler and the bottom of second tower bottom reboiler.
5. according to the purifying plant of claim 3 or 4 described electronic-grade ultra-pure ammonia, it is characterized in that: said liquefied ammonia withdrawing can is also connected with the bottom of vaporizer.
6. use the purify method of purification of electronic-grade ultra-pure ammonia of the described purifying plant of claim 1, it is characterized in that, may further comprise the steps:
1) through ammonia pump (2) liquefied ammonia in the liquefied ammonia storage tank (1) is squeezed into vaporizer (3) vaporization;
2) ammonia after the vaporizer vaporization is sent into oil eliminator (4) oil removing; Directly send into first rectifying tower (51) after the oil removing and carry out the separation of weight component; After the first rectifying tower cat head is through first overhead condenser (511), remove the light constituent impurity of incoagulability; The liquefied ammonia that contains heavy constituent impurity in first tower bottom reboiler (512) is discharged in the liquefied ammonia withdrawing can, and the cat head of the first rectifying Tata still is sent into second rectifying tower (52) through the liquefied ammonia of condensation and further removed weight component impurity;
3) after the second rectifying tower cat head is through second overhead condenser (521), remove the light constituent impurity of incoagulability; The liquefied ammonia that contains heavy constituent impurity in second tower bottom reboiler (522) is discharged in the liquefied ammonia withdrawing can (9); Whether detection is qualified through the liquefied ammonia of second overhead condenser; If the qualified product storage tank (8) of then packing into; If defectively then send into terminal purifier (6) together and carry out micro-removal of impurities, finally obtain the qualified ultra-pure ammonia product storage tank of packing into through condensing surface (7) condensation with the ammonia of the second rectifying Tata still.
7. the purifying plant of electronic-grade ultra-pure ammonia according to claim 6 is characterized in that: the working temperature of said vaporizer is controlled at 50 ℃～80 ℃, and WP is controlled between 1Mpa～1.5Mpa; The boil-off rate of liquefied ammonia is at 180kg/h～230kg/h.
8. according to the purifying plant of claim 6 or 7 described electronic-grade ultra-pure ammonia, it is characterized in that: the work liquid level is 0.5m～0.8m in the said vaporizer.
9. the purifying plant of electronic-grade ultra-pure ammonia according to claim 6 is characterized in that: the working temperature of said first rectifying tower and second rectifying tower is controlled at 20 ℃～80 ℃, and WP is controlled at 0.9Mpa～1.3Mpa.
10. according to the purifying plant of claim 6 or 9 described electronic-grade ultra-pure ammonia, it is characterized in that: the height of said first rectifying tower and second rectifying tower is 23m～26m.
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Cited By (7)
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| CN103466656A (en) * | 2012-06-06 | 2013-12-25 | 华东理工大学 | Membrane absorption method for preparation of ultra-clean high-purity ammonia water |
| CN106315620A (en) * | 2016-10-20 | 2017-01-11 | 福建久策气体集团有限公司 | Ultra-pure ammonia purification device and purification method thereof |
| CN107777703A (en) * | 2016-08-25 | 2018-03-09 | 四川天采科技有限责任公司 | A kind of purification method of the full temperature journey sorption extraction deep dehydration removal of impurities of ultra-pure ammonia |
| CN109231238A (en) * | 2018-08-30 | 2019-01-18 | 海宁市英德赛电子有限公司 | A kind of high-purity ammon continuous process system and its production technology |
| CN109481982A (en) * | 2018-10-18 | 2019-03-19 | 海宁市英德赛电子有限公司 | A kind of the rectifying Preparation equipment and technique of 6N4 high-purity ammon |
| CN111960436A (en) * | 2020-09-03 | 2020-11-20 | 福建省宜品生物科技有限公司 | Ultrapure ammonia production device and production method |
| CN113603113A (en) * | 2021-09-17 | 2021-11-05 | 浙江建业微电子材料有限公司 | Production device and production method suitable for electronic-grade ammonia gas and ammonia water |
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| CN111960436A (en) * | 2020-09-03 | 2020-11-20 | 福建省宜品生物科技有限公司 | Ultrapure ammonia production device and production method |
| CN113603113A (en) * | 2021-09-17 | 2021-11-05 | 浙江建业微电子材料有限公司 | Production device and production method suitable for electronic-grade ammonia gas and ammonia water |
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Application publication date: 20120118 |