CN102502701B - Production process and preparation method of ultrapure ammonia - Google Patents
Production process and preparation method of ultrapure ammonia Download PDFInfo
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- CN102502701B CN102502701B CN201110340316.1A CN201110340316A CN102502701B CN 102502701 B CN102502701 B CN 102502701B CN 201110340316 A CN201110340316 A CN 201110340316A CN 102502701 B CN102502701 B CN 102502701B
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- ammonia
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- water
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
Abstract
The invention relates to a production process of ultrapure ammonia, which includes that raw material ammonia is pumped into a rectification column, enters a deoiling and dewatering device after impurities such as light components, part of water and the like are removed and cold energy is recovered, and enters a terminal purifying device after most of water is removed, and gaseous ammonia with water and impurities deep removed is condensed and enters an ammonia product cylinder so as to obtain the ultrapure ammonia product. The production process is simple in procedure and economical in investment and system energy is optimized, energy consumption can be reduced by 40%, and purity of the ammonia product can be stably kept more than 7N (99.99999%) for a long time.
Description
Technical field
The present invention relates to special gas production field,, be exactly a kind of ultra-pure ammonia production technique and preparation method thereof.
Background technology
Ultra-pure ammonia is to adopt sophisticated equipment and technology to carry out deep processing and make ammonia purity reach 6N(99.9999% industrial liquid ammonia) above high-tech product is one of main raw material of photovoltaic and LED product.Because China starts late to the research of ultra-pure ammonia and reason, the basic dependence on import of domestic electronic grade ultrapure ammonia such as technology level is lower.
The technical process of producing at present ultra-pure ammonia is: taking industrial liquid ammonia as raw material, through filtering oil removing, except entering vaporizer after metallic impurity, enter one-level purifier (oil removing and dewater) after vaporization, after condensation, remove H through rectifying tower
2, O
2, N
2, CO, CO
2, CH
4deng impurity, finally enter terminal purification devices, after dewatering, the degree of depth can obtain the more than 99.9999% ultra-pure ammonia product of purity.
The defect that existing procedure exists:
(1) flow process is longer, and capacity usage ratio is low, and power consumption is higher.
(2) purity of product ammonia can not be steady in a long-term more than 7N.
Summary of the invention
The object of the invention is for Existing Defects, provide that a kind of energy consumption is lower, the ultra-pure ammonia production technique of the purity of ammonia.
Above-mentioned purpose realizes by following scheme:
A kind of ultra-pure ammonia production technique, is characterized in that:
Raw material ammonia enters rectifying tower through pump pressurization, rectifying tower control pressure is at 1.3-1.5Pa, rectification temperature is controlled at 60 DEG C of left and right, remove the impurity such as light constituent and part water, when ammonia purity >=99.995%, water Han Liang≤100ppm, light constituent total content reclaims cold while being less than 10ppb, after reclaiming cold, enter oil removing water eliminator, control temperature at 50-55 DEG C, pressure is within the scope of 1.2-1.3 Pa, when ammonia purity >=99.9995%, when water Han Liang≤100ppb, enter terminal purification devices, temperature in control device is at 40-50 DEG C, pressure is within the scope of 1.0-1.2 Pa, through the degree of depth dewater and impurity after gas ammonia after condensation, enter product ammonia tank and can obtain ultra-pure ammonia product.
Described a kind of ultra-pure ammonia production technique, is characterized in that: raw material ammonia is general industry level liquefied ammonia, ammonia purity >=99.6% ， Shui≤0.2-0.3% ， You≤10mg/kg.
Described a kind of ultra-pure ammonia production technique, is characterized in that: the waste liquid that the each step of production technique produces reclaims and enters waste liquid recovery storage tank.
Beneficial effect of the present invention is:
(1), technical process is simple, reduced investment.
(2), system capacity optimization, energy consumption can reduce by 40%.
(3), the purity of product ammonia can be steady in a long-term at 7N(99.99999%) more than.
(4), safety performance is good, level of automation is high.
(5), existing ultra-pure ammonia technical process is optimized, cancel vaporizer, transformation one-level purifier, adopts novel de-oiling water eliminator, makes full use of system capacity.
brief description of the drawings:
Fig. 1 is process flow sheet of the present invention.
Wherein, the 1st, raw material ammonia tank, the 2nd, ammonia pump, the 3rd, low-temperature fractionating tower, the 4th, oil removing water eliminator, the 5th, terminal purification devices, the 6th, condenser, the 7th, product ammonia tank, the 8th, useless ammonia storage tank.
Embodiment
Embodiment 1:
A kind of ultra-pure ammonia production technique, is characterized in that:
Raw material ammonia enters rectifying tower through pump pressurization, rectifying tower control pressure is at 1.3-1.5Pa, rectification temperature is controlled at 60 DEG C of left and right, remove the impurity such as light constituent and part water, when ammonia purity >=99.995%, water Han Liang≤100ppm, light constituent total content reclaims cold while being less than 10ppb, after reclaiming cold, enter oil removing water eliminator, control temperature at 50-55 DEG C, pressure is within the scope of 1.2-1.3 Pa, when ammonia purity >=99.9995%, when water Han Liang≤100ppb, enter terminal purification devices, temperature in control device is at 40-50 DEG C, pressure is within the scope of 1.0-1.2 Pa, through the degree of depth dewater and impurity after gas ammonia after condensation, enter product ammonia tank and can obtain ultra-pure ammonia product.
Described a kind of ultra-pure ammonia production technique, is characterized in that: raw material ammonia is general industry level liquefied ammonia, ammonia purity >=99.6% ， Shui≤0.2-0.3% ， You≤10mg/kg.
Described a kind of ultra-pure ammonia production technique, is characterized in that: the waste liquid that the each step of production technique produces reclaims and enters waste liquid recovery storage tank.
Embodiment 2:
Referring to Fig. 1, in this technique, between raw material ammonia tank (1), ammonia pump (2), rectifying tower (3), the each equipment of oil removing water eliminator (4), be connected with valve with 304 stainless steel pipes, between terminal purification devices (5), condenser (6), the each equipment of product ammonia tank (7), be connected with valve with 316L stainless steel (inwall electropolishing processing) pipeline.System adopts DCS automatically to control.After rectifying tower (3), light constituent total content is less than 10ppb; After oil removing water eliminator (4), water-content is less than 100ppb; After terminal purification devices (5), water-content is less than 1ppb, and ammonia content is greater than 7N.
Technical process of the present invention: the liquefied ammonia in raw material ammonia tank (1) enters rectifying tower (3) through pump (2) pressurization, after removing light constituent and part water, enter oil removing water eliminator (4), after further removing most of water, enter terminal purification devices (5), the gas ammonia of removing after impurity enters product ammonia tank after condensation.The waste liquid that each technology controlling and process point produces enters waste liquid and reclaims storage tank (8).
Raw material ammonia is general industry level liquefied ammonia, ammonia purity >=99.6% ， Shui≤0.2-0.3% ， You≤10mg/kg; Rectifying tower outlet ammonia purity >=99.995%, water Han Liang≤100ppm, light constituent total content is less than 10ppb, 60 DEG C of left and right of rectification temperature; Oil removing water eliminator outlet ammonia purity >=99.9995%, water Han Liang≤100ppb; Terminal purifier outlet ammonia purity >=99.99999%, water Han Liang≤1ppb, light constituent total content is less than 10ppb.
Claims (3)
1. a ultra-pure ammonia production technique, is characterized in that:
Raw material ammonia enters rectifying tower through pump pressurization, rectifying tower control pressure is at 1.3-1.5Pa, rectification temperature is controlled at 60 DEG C, remove light constituent and part water impurity, when ammonia purity >=99.995%, water Han Liang≤100ppm, light constituent total content reclaims cold while being less than 10ppb, after reclaiming cold, enter oil removing water eliminator, control temperature at 50-55 DEG C, pressure is within the scope of 1.2-1.3 Pa, when ammonia purity >=99.9995%, when water Han Liang≤100ppb, enter terminal purification devices, temperature in control device is at 40-50 DEG C, pressure is within the scope of 1.0-1.2 Pa, through the degree of depth dewater and impurity after gas ammonia after condensation, enter product ammonia tank and can obtain ultra-pure ammonia product.
2. a kind of ultra-pure ammonia production technique according to claim 1, is characterized in that: raw material ammonia is general industry level liquefied ammonia, ammonia purity >=99.6% ， Shui≤0.2-0.3% ， You≤10mg/kg.
3. a kind of ultra-pure ammonia production technique according to claim 1, is characterized in that: the waste liquid that the each step of production technique produces reclaims and enters waste liquid recovery storage tank.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110340316.1A CN102502701B (en) | 2011-11-02 | 2011-11-02 | Production process and preparation method of ultrapure ammonia |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110340316.1A CN102502701B (en) | 2011-11-02 | 2011-11-02 | Production process and preparation method of ultrapure ammonia |
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| Publication Number | Publication Date |
|---|---|
| CN102502701A CN102502701A (en) | 2012-06-20 |
| CN102502701B true CN102502701B (en) | 2014-07-30 |
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| CN201110340316.1A Expired - Fee Related CN102502701B (en) | 2011-11-02 | 2011-11-02 | Production process and preparation method of ultrapure ammonia |
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102963909B (en) * | 2012-11-26 | 2014-08-06 | 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 ammonia water method |
| CN102963910B (en) * | 2012-11-26 | 2014-08-06 | 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 |
| CN103880039A (en) * | 2012-12-19 | 2014-06-25 | 海安海太铸造有限公司 | Ammonia purifying and deoiling device |
| CN106315620B (en) * | 2016-10-20 | 2019-03-12 | 福建久策气体集团有限公司 | A kind of ultra-pure ammonia purification device and its purification method |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN201520643U (en) * | 2009-09-28 | 2010-07-07 | 苏州市金宏气体有限公司 | Device for purifying and extracting electronic-grade ultra-pure ammonia |
| CN101817540A (en) * | 2010-04-06 | 2010-09-01 | 苏州金宏气体股份有限公司 | Purification method of 7N electronic grade hyperpure ammonia |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN201520643U (en) * | 2009-09-28 | 2010-07-07 | 苏州市金宏气体有限公司 | Device for purifying and extracting electronic-grade ultra-pure ammonia |
| CN101817540A (en) * | 2010-04-06 | 2010-09-01 | 苏州金宏气体股份有限公司 | Purification method of 7N electronic grade hyperpure ammonia |
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| CN102502701A (en) | 2012-06-20 |
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Granted publication date: 20140730 Termination date: 20201102 |