CN102502701A - Production process and preparation method of ultrapure ammonia - Google Patents
Production process and preparation method of ultrapure ammonia Download PDFInfo
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- CN102502701A CN102502701A CN2011103403161A CN201110340316A CN102502701A CN 102502701 A CN102502701 A CN 102502701A CN 2011103403161 A CN2011103403161 A CN 2011103403161A CN 201110340316 A CN201110340316 A CN 201110340316A CN 102502701 A CN102502701 A CN 102502701A
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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 the special gas production field,, exactly be a kind of ultra-pure ammonia production technique and preparation method thereof.
Background technology
Ultra-pure ammonia is to adopt sophisticated equipment and technology industrial liquefied ammonia to be carried out deep processing and make ammonia purity reach the high product innovation more than the 6N (99.9999%), is one of main raw material of photovoltaic and LED product.Owing to China starts late to the research of ultra-pure ammonia and reason, the basic dependence on import of domestic electronic-grade ultra-pure ammonia such as technological level is lower.
The main technique flow process of producing ultra-pure ammonia at present is: with industrial liquefied ammonia is raw material, after filtering oil removing, removing metallic impurity, gets into vaporizer, and the vaporization back gets into one-level purifier (oil removing and dewater), and condensation is after rectifying tower is removed H
2, O
2, N
2, CO, CO
2, CH
4Deng impurity, get into the terminal purification devices at last,, the degree of depth can obtain the ultra-pure ammonia product of purity more than 99.9999% after dewatering.
The defective 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 objective of the invention is to existing defective, provide that a kind of energy consumption is lower, the ultra-pure ammonia production technique of the purity of ammonia.
Above-mentioned purpose realizes through following scheme:
A kind of ultra-pure ammonia production technique is characterized in that:
Raw material ammonia gets into rectifying tower through the pump pressurization, and the rectifying tower control pressure is at 1.3-1.5Pa, and rectification temperature is controlled at about 60 ℃; Remove impurity such as light constituent and portion water; When ammonia purity >=99.995%, water Han Liang ≦ 100ppm, light constituent total content reclaim cold during less than 10ppb; Get into the oil removing water eliminator after reclaiming cold; Controlled temperature in 1.2-1.3 Pa scope, when ammonia purity >=99.9995%, gets into the terminal purification devices at 50-55 ℃, pressure during water Han Liang ≦ 100ppb; Temperature in the gear at 40-50 ℃, pressure in 1.0-1.2 Pa scope, through the degree of depth dewater and impurity after gas ammonia after condensation, get into product ammonia jar and can obtain the ultra-pure ammonia product.
Described a kind of ultra-pure ammonia production technique is characterized in that: raw material ammonia is a 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 each step of production technique is produced reclaims and gets into 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 more than 7N (99.99999%).
(4), safety performance is good, level of automation is high.
(5), existing ultra-pure ammonia technical process is optimized, the cancellation vaporizer is transformed the one-level purifier, adopts the novel de-oiling water eliminator, makes full use of system capacity.
Description of drawings:
Fig. 1 is a process flow sheet of the present invention.
Wherein, the 1st, raw material ammonia jar, the 2nd, ammonia pump, the 3rd, low-temperature fractionating tower, the 4th, oil removing water eliminator, the 5th, terminal purification devices, the 6th, condensing surface, the 7th, product ammonia jar, the 8th, useless ammonia storage tank.
Embodiment
Embodiment 1:
A kind of ultra-pure ammonia production technique is characterized in that:
Raw material ammonia gets into rectifying tower through the pump pressurization, and the rectifying tower control pressure is at 1.3-1.5Pa, and rectification temperature is controlled at about 60 ℃; Remove impurity such as light constituent and portion water; When ammonia purity >=99.995%, water Han Liang ≦ 100ppm, light constituent total content reclaim cold during less than 10ppb; Get into the oil removing water eliminator after reclaiming cold; Controlled temperature in 1.2-1.3 Pa scope, when ammonia purity >=99.9995%, gets into the terminal purification devices at 50-55 ℃, pressure during water Han Liang ≦ 100ppb; Temperature in the gear at 40-50 ℃, pressure in 1.0-1.2 Pa scope, through the degree of depth dewater and impurity after gas ammonia after condensation, get into product ammonia jar and can obtain the ultra-pure ammonia product.
Described a kind of ultra-pure ammonia production technique is characterized in that: raw material ammonia is a 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 each step of production technique is produced reclaims and gets into waste liquid recovery storage tank.
Embodiment 2:
Referring to Fig. 1; In this technology; Be connected with valve with 304 stainless steel pipes between raw material ammonia jar (1), ammonia pump (2), rectifying tower (3), each equipment of oil removing water eliminator (4), be connected with valve with 316L stainless steel (inwall electropolishing processing) pipeline between terminal purification devices (5), condensing surface (6), each equipment of product ammonia jar (7).System adopts DCS to control automatically.Behind rectifying tower (3), the light constituent total content is less than 10ppb; Oil removing water eliminator (4) back water-content is less than 100ppb; Terminal purification devices (5) back water-content is less than 1ppb, and ammonia content is greater than 7N.
Technical process of the present invention: the liquefied ammonia in the raw material ammonia jar (1) gets into rectifying tower (3) through pump (2) pressurization; Get into oil removing water eliminator (4) after removing light constituent and portion water; Further remove and get into terminal purification devices (5) behind most of water, the gas ammonia of removing behind the impurity gets into product ammonia jar after condensation.The waste liquid that each technology controlling and process point produces gets into waste liquid and reclaims storage tank (8).
Raw material ammonia is a 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, about 60 ℃ of rectification temperatures; Oil removing water eliminator outlet ammonia purity >=99.9995%, water Han Liang ≦ 100ppb; Terminal purifier outlet ammonia purity >=99.99999%, water Han Liang ≦ 1ppb, the light constituent total content is less than 10ppb.
Claims (3)
1. ultra-pure ammonia production technique is characterized in that:
Raw material ammonia gets into rectifying tower through the pump pressurization, and the rectifying tower control pressure is at 1.3-1.5Pa, and rectification temperature is controlled at about 60 ℃; Remove impurity such as light constituent and portion water; When ammonia purity >=99.995%, water Han Liang ≦ 100ppm, light constituent total content reclaim cold during less than 10ppb; Get into the oil removing water eliminator after reclaiming cold; Controlled temperature in 1.2-1.3 Pa scope, when ammonia purity >=99.9995%, gets into the terminal purification devices at 50-55 ℃, pressure during water Han Liang ≦ 100ppb; Temperature in the gear at 40-50 ℃, pressure in 1.0-1.2 Pa scope, through the degree of depth dewater and impurity after gas ammonia after condensation, get into product ammonia jar and can obtain the 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 a 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 each step of production technique is produced reclaims and gets into 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 |
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| 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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| CN102502701A true CN102502701A (en) | 2012-06-20 |
| CN102502701B 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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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN102963909A (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 ammonia water method |
| CN103880039A (en) * | 2012-12-19 | 2014-06-25 | 海安海太铸造有限公司 | Ammonia purifying and deoiling device |
| 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 |
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 |
-
2011
- 2011-11-02 CN CN201110340316.1A patent/CN102502701B/en not_active Expired - Fee Related
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 |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN102963909A (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 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 |
| 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 |
| CN103880039A (en) * | 2012-12-19 | 2014-06-25 | 海安海太铸造有限公司 | Ammonia purifying and deoiling device |
| 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 |
| 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 |
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| Publication number | Publication date |
|---|---|
| CN102502701B (en) | 2014-07-30 |
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