CN202030539U - Device for producing 7N electronic grade hyperpure ammonia through rectification separation - Google Patents
Device for producing 7N electronic grade hyperpure ammonia through rectification separation Download PDFInfo
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- CN202030539U CN202030539U CN2011200666550U CN201120066655U CN202030539U CN 202030539 U CN202030539 U CN 202030539U CN 2011200666550 U CN2011200666550 U CN 2011200666550U CN 201120066655 U CN201120066655 U CN 201120066655U CN 202030539 U CN202030539 U CN 202030539U
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Abstract
The utility model relates to a device for producing 7N electronic grade hyperpure ammonia through rectification separation. The main body of the device consists of three rectifying towers and two vaporizers with tower bottoms. Moreover, the device is also provided with two industrial liquid ammonia feeding tanks used alternatively, two air source heaters for completing heating, two finished product tanks used alternatively and an industrial liquid ammonia recycling tank; moreover, the device is also provided with three recycling condensers and three tower top condensers as well as a finished product condenser; in addition, three ammonia filters are also arranged behind the three rectifying towers. Materials can be automatically fed by using gas phase balance and liquid level differences; moreover, the purity of the hyperpure ammonia produced through three times of rectification can be 99.99999 percent by using the special design concept of integrating designing the rectifying towers with the vaporizers and using the two tower bottoms to complete the vaporization of the three rectifying towers.
Description
Technical field
The utility model relates to a kind of rectifying separation device, is specifically related to a kind of employing technical grade liquefied ammonia, with rectifying separation can continuous production 6.4N electronic-grade ultra-pure ammonia device.
Background technology
Ultra-pure ammonia is an important electron gas in the semi-conductor industry, in production process of semiconductor, and ammonia (NH
3) same silane (SiH
4) generation silicon nitride film together reacts; On MOCVD equipment, ammonia acts on the sapphire with trimethyl-gallium and forms gallium nitride light-emitting diode, i.e. LED by vapour growth.
Along with development of science and technology increases for the demand of electronic product, novel energy-conserving illuminating device, clean energy day by day with society, also more and more higher for the purity requirement of ultra-pure ammonia.For example, when producing the LED device of high brightness, because the geometrical shape of device is constantly dwindled and the brightness requirement of LED improves constantly, the pollutant load in the raw material ammonia is very important for the quality of product.Therefore, purification technique, the equipment for ammonia is the focus of research always.
Because semiconductor technology evolves such as developed country's photoelectron speed is violent, greatly promoted gas companies improves purity to ammonia research.At present, the many LED of China produce the used import ammonia of user, basically be U.S.'s Praxair, APCI, French liquid air, German woods moral and The foreign chicken products such as Japanese clear and electrician, the ultra-pure ammonia preparation method that they adopted all adopts basically raw material ammonia is removed part oil through active carbon adsorber, remove portion water by molecular sieve adsorber absorption again, remove partial oxygen through the reductor adsorber again, pass through the simple rectifying of one-level or secondary again, obtain the ultra-pure ammonia product through the terminal purifier again.
The shortcoming of this type of device is: activated carbon, molecular sieve and terminal purifier need manipulation of regeneration in the adsorber, have large quantity of exhaust gas to discharge in the regenerative process, have formed secondary pollution; The terminal purifier can produce side reaction in purge process, influence the purity of the finished product; Owing to can't utilize again by ammonia, the waste gas after multiple tracks absorption and the desorb, have a strong impact on environment and product yield; Technical process is oversize, and equipment is many, investment is many.
Summary of the invention
Shortcoming at above-mentioned existence, the purpose of this utility model is: but ingenious, the safe and reliable continuous production of a kind of design, environmental protection, energy-conservation are proposed, collection vaporizer, rectifying tower are one, need not adsorption unit, terminal purification devices, produce the device of 7N electronic-grade ultra-pure ammonia merely by rectifying separation.
The technical solution of the utility model is: an industrial raw material liquid ammonia storage tank, the raw materials ammonia feed pot of two parallel connections, on industrial raw material liquid ammonia storage tank discharging pipeline, be provided with to the reinforced ammonia pump of the raw materials ammonia feed pot of two parallel connections, the raw materials ammonia feed pot of two parallel connections is communicated with one-level rectifying vaporization integration apparatus by a carrier pipe road, the outlet pipe of one-level rectifying vaporization integration apparatus is by the ammonia strainer and then be communicated with two-stage rectification vaporization integration apparatus, the outlet pipe of two-stage rectification vaporization integration apparatus is communicated with degree of depth purification rectifying tower by another ammonia strainer, one-level rectifying vaporization integration apparatus, the bottom of two-stage rectification vaporization integration apparatus is connected to the heating system of gasification usefulness respectively, one-level rectifying vaporization integration apparatus, the top of two-stage rectification vaporization integration apparatus and degree of depth purification rectifying tower is connected to the condensing reflux blowdown system, and degree of depth purification rectifying tower is communicated with finished product by the 3rd ammonia strainer and accepts charging system.
Described ammonia strainer is the tubular type accurate filter, and the filter core in this tubular type accurate filter is made with K-49 type beta glass fibre film, can filter the particle less than 0.01um.
The mouth of pipe that gas-liquid equilibrium can be formed at the top of the gas phase mouth of the raw materials ammonia feed pot of described two parallel connections and one-level rectifying vaporization integration apparatus is communicated with, and the mouth of pipe that the prime rectifying that the liquid phase mouth pipeline of the raw materials ammonia feed pot of two parallel connections and its position are hanged down 100CM is at least vaporized on the integration apparatus is communicated with.
Described heating system comprises two air source water heaters, two hot water circulating pumps, and the hot water entrance of two air source water heaters is communicated with the hot water entrance of one-level rectifying vaporization integration apparatus and two-stage rectification vaporization integration apparatus respectively and constitutes the pipeline circulation in conjunction with two hot water circulating pumps.
Described condensing reflux blowdown system comprises three overhead condensers that are communicated with the cat head gas phase mouth of one-level rectifying vaporization integration apparatus, two-stage rectification vaporization integration apparatus and degree of depth purification rectifying tower respectively, the liquid phase mouth of three overhead condensers is communicated with three cat head header tanks respectively, and the lower part outlet of three cat head header tanks is communicated to the trim the top of column mouth of one-level rectifying vaporization integration apparatus, two-stage rectification vaporization integration apparatus and degree of depth purification rectifying tower respectively.
This device also is provided with recovery system, this recovery system comprises three recovery condensers, the gas phase mouth of three recovery condensers is communicated with the emptying mouth of pipe of above-mentioned three overhead condensers respectively, the liquid phase mouth of three recovery condensers all is communicated to a withdrawing can, and this withdrawing can also is communicated with the raffinate row mouth of one-level rectifying vaporization integration apparatus and two-stage rectification vaporization integration apparatus.
Described finished product is accepted charging system and is comprised the finished product condenser, the gas phase mouth of finished product condenser is communicated with in the outlet of the ammonia strainer that the outlet with degree of depth purification rectifying tower links to each other, the finished product receiving tank that is connected with finished product condenser liquid phase mouth, finished product receiving tank bottom liquid phase mouth is connected to filling pump, and the filling pump pipeline connection has finished product to fill steel cylinder.
The beneficial effects of the utility model are: the raw materials ammonia feed pot of two parallel connections can alternately be one-level rectifying vaporization integration apparatus feed by valve control, has guaranteed the continuity of feed.Raw materials ammonia feed pot and one-level rectifying vaporization integration apparatus gas-liquid equilibrium also utilize the two liquid level difference to feed in raw material, and not only eliminated use mechanical pump fault defective how but also saved cost.The vaporizer circulating hot water adopts air source water heater to produce, and can save a large amount of energy costs.By three grades of rectifying separation, the component emptying of will mixing is reclaimed, and the bottom product discharging is reclaimed, and devices such as super strainer filtration have improved the purity of ammonia.The ultra-pure ammonia that the device that uses a kind of rectifying separation of the utility model to produce 7N electronic-grade ultra-pure ammonia is produced, single assorted component is reduced in the 10ppb, and moisture is less than 50ppb.Reach advanced world standards.By vaporizer, rectifying tower are combined, two-stage rectification vaporization integration apparatus and degree of depth purification rectifying tower share a tower still, make device structure more reasonable.But ingenious, the safe and reliable continuous production of the utility model design, environmental protection, energy-conservation.
Description of drawings
Fig. 1 is the utility model structural representation;
Among the figure: 1, industrial raw material liquid ammonia storage tank, 2, ammonia pump, 3, the first raw materials ammonia feed pot, 4, the second raw materials ammonia feed pot, 5, one-level rectifying vaporization integration apparatus, 6, two-stage rectification vaporization integration apparatus, 7, degree of depth purification rectifying tower, 8～10, overhead condenser, 11～13, reclaim condenser, 14～16, ammonia strainer, 17～19, the cat head header tank, 20, the finished product condenser, 21～22, hot water heater, 25～26, hot water circulating pump, 23～24, the finished product receiving tank, 27, the finished product filling pump; 28～29, finished product fills steel cylinder, and 30, industrial liquefied ammonia withdrawing can.
Embodiment
As can be seen from Figure 1, a kind of rectifying separation is produced the device of 7N electronic-grade ultra-pure ammonia, and main body includes one-level rectifying vaporization integration apparatus 5, two-stage rectification vaporization integration apparatus 6 and degree of depth purification rectifying tower 7 and constitutes.Industrial raw material liquid ammonia storage tank 1 send raw materials ammonia by ammonia pump 2 to the first raw materials ammonia feed pot 3 and the second raw materials ammonia feed pot defeated 4 of parallel connection, the raw materials ammonia feed pot of two parallel connections can alternately be one-level rectifying vaporization integration apparatus feed by valve control, has guaranteed the continuity of feed.
The upper gaseous phase mouth pipeline of the first raw materials ammonia feed pot 3 in parallel and the second raw materials ammonia feed pot defeated 4 is communicated with the mouth of pipe that gas-liquid equilibrium can be formed at the top of one-level rectifying vaporization integration apparatus 5, mouth of pipe on the one-level rectifying vaporization integration apparatus 5 of the low at least 100CM in the liquid phase mouth pipeline of the raw materials ammonia feed pot of two parallel connections and its position is communicated with, formation liquid level difference charging system.
Degree of depth purification rectifying tower 7 tower bottomss are managed mutually with two-stage rectification vaporization integration apparatus 6 and are connected, and finish the discharging of degree of depth purification rectifying tower 7 tower bottomss.Degree of depth purification rectifying tower 7 links to each other with overhead condenser 10 gas phase pipes, and overhead condenser 10 liquid phase mouths link to each other with cat head header tank 19 tops, and cat head header tank 19 bottoms are connected with degree of depth purification rectifying tower 7 cats head, forms the rectifying tower return-flow system.The overhead condenser 10 emptying mouths of pipe are connected with recovery condenser 11 gas phase mouths, reclaim condenser 11 liquid phase mouths and are connected with industrial liquefied ammonia withdrawing can 30 upper orifice, reach the purpose that reclaims industrial liquefied ammonia.
Going out ammonia outlet in degree of depth purification rectifying tower 7 towers is connected with ammonia strainer 16,16 outlets of ammonia strainer are connected with finished product condenser 20 upper gaseous phase mouths, finished product condenser 20 bottom liquid phase mouths are connected with the upper orifice of finished product receiving tank 23 with finished product receiving tank 24, form the finished product receiving system.
Finished product receiving tank 23 is connected with finished product filling pump 27 with finished product receiving tank 24 bottom liquid phase mouths, and finished product filling pump 27 and finished product fill steel cylinder 28 and fill steel cylinder 29 with finished product and be connected, and form the finished product charging system.
When reality is used, when having one to fill it up with raw materials ammonia in the raw materials ammonia feed pot of two parallel connections, open one of them and gas-liquid equilibrium pipe valve and liquid phase pipe valve that one-level rectifying vaporization integration apparatus 5 links to each other, it is reinforced to utilize liquid level difference to finish automatically.Open hot water heater 21 and be connected valve, just finish the liquefied ammonia vaporization with one-level rectifying vaporization integration apparatus 5 hot water entrances.After opening overhead condenser 8 water coolants turnover valve, rectifying tower and vaporizer 5 are with regard to works better.When overhead condenser 8 emptying are opened, open and reclaim condenser 13 cooling water intakeoutfall, finished the work that industrial liquefied ammonia is reclaimed in emptying.Open the one-level rectifying vaporization integration apparatus 5 bottom products row pipe valve that mouthful is connected, reach the purpose of the industrial liquefied ammonia of recovery tower still with industrial liquefied ammonia withdrawing can 30 upper orifice.
After one-level rectifying vaporization integration apparatus 5 first products are purified normal operation, open one-level rectifying vaporization integration apparatus 5 middle and upper part first product ammonia outlet valves, first product ammonia vapour enters ammonia strainer 14 and the two-stage rectification vaporization integration apparatus 6 middle and upper parts enforcement degree of depth is purified reinforced.Open hot water heater 22 and be connected valve, just finish the liquefied ammonia vaporization with two-stage rectification vaporization integration apparatus 6 hot water entrances.After opening overhead condenser 9 water coolants turnover valve, two-stage rectification vaporization integration apparatus 6 is with regard to works better.When overhead condenser 9 emptying are opened, open backlash and receive condenser 12 cooling water intakeoutfall, finished the work that industrial liquefied ammonia is reclaimed in 6 emptying of two-stage rectification vaporization integration apparatus.Open the two-stage rectification vaporization integration apparatus 6 bottom products row pipe valve that mouthful is connected, reach the purpose of the industrial liquefied ammonia of recovery tower still with industrial liquefied ammonia withdrawing can 30 upper orifice.
After the 6 normal operations of two-stage rectification vaporization integration apparatus, open two-stage rectification vaporization integration apparatus 6 tower stills and degree of depth purification rectifying tower 7 tower still gas phase pipe valves, open two-stage rectification vaporization integration apparatus 6 and degree of depth purification rectifying tower 7 tower bottomss pipe valve mutually, finish the two-stage rectification integration apparatus 6 of vaporizing and circulate mutually with the gas-liquid of degree of depth purification rectifying tower 7.After opening overhead condenser 10 water coolants turnover valve, degree of depth purification rectifying tower 7 is with regard to works better.When overhead condenser 10 emptying are opened, open and reclaim condenser 11 cooling water intakeoutfall, finished the work that industrial liquefied ammonia is reclaimed in 7 emptying of degree of depth purification rectifying tower.After degree of depth purification rectifying tower 7 works better, open degree of depth purification rectifying tower 7 middle and upper part ammonia outlet valves, finished product ammonia vapour enters ammonia strainer 16 and finished product condenser 20, enters finished product receiving tank 23 and finished product receiving tank 24 simultaneously.Just finished product is filled bottle 28 and finished product and fill bottles 29 and fill when opening finished product filling pump 27, finish whole process of production.
Claims (6)
1. a rectifying separation is produced the device of 7N electronic-grade ultra-pure ammonia, it is characterized in that comprising an industrial raw material liquid ammonia storage tank, the raw materials ammonia feed pot of two parallel connections, on industrial raw material liquid ammonia storage tank discharging pipeline, be provided with to the reinforced ammonia pump of the raw materials ammonia feed pot of two parallel connections, the raw materials ammonia feed pot of two parallel connections is communicated with one-level rectifying vaporization integration apparatus by a carrier pipe road, the outlet pipe of one-level rectifying vaporization integration apparatus is by the ammonia strainer and then be communicated with two-stage rectification vaporization integration apparatus, the outlet pipe of two-stage rectification vaporization integration apparatus is communicated with degree of depth purification rectifying tower by another ammonia strainer, one-level rectifying vaporization integration apparatus, the bottom of two-stage rectification vaporization integration apparatus is connected to the heating system of gasification usefulness respectively, one-level rectifying vaporization integration apparatus, the top of two-stage rectification vaporization integration apparatus and degree of depth purification rectifying tower is connected to the condensing reflux blowdown system, and degree of depth purification rectifying tower is communicated with finished product by the 3rd ammonia strainer and accepts charging system.
2. rectifying separation according to claim 1 is produced the device of 7N electronic-grade ultra-pure ammonia, the mouth of pipe that gas-liquid equilibrium can be formed at the top of gas phase mouth and one-level rectifying vaporization integration apparatus that it is characterized in that the raw materials ammonia feed pot of described two parallel connections is communicated with, and the mouth of pipe that the prime rectifying that the liquid phase mouth pipeline of the raw materials ammonia feed pot of two parallel connections and its position are hanged down 100CM is at least vaporized on the integration apparatus is communicated with.
3. rectifying separation according to claim 1 is produced the device of 7N electronic-grade ultra-pure ammonia, it is characterized in that described heating system comprises two air source water heaters, two hot water circulating pumps, the hot water entrance of two air source water heaters is communicated with the hot water entrance of one-level rectifying vaporization integration apparatus and two-stage rectification vaporization integration apparatus respectively and constitutes the pipeline circulation in conjunction with two hot water circulating pumps.
4. rectifying separation according to claim 1 is produced the device of 7N electronic-grade ultra-pure ammonia, it is characterized in that described condensing reflux blowdown system comprises respectively and one-level rectifying vaporization integration apparatus, three overhead condensers that the cat head gas phase mouth of two-stage rectification vaporization integration apparatus and degree of depth purification rectifying tower is communicated with, the liquid phase mouth of three overhead condensers is communicated with three cat head header tanks respectively, and the lower part outlet of three cat head header tanks is communicated to one-level rectifying vaporization integration apparatus respectively, the trim the top of column mouth of two-stage rectification vaporization integration apparatus and degree of depth purification rectifying tower.
5. rectifying separation according to claim 4 is produced the device of 7N electronic-grade ultra-pure ammonia, it is characterized in that this device also is provided with recovery system, this recovery system comprises three recovery condensers, the gas phase mouth of three recovery condensers is communicated with the emptying mouth of pipe of above-mentioned three overhead condensers respectively, the liquid phase mouth of three recovery condensers all is communicated to a withdrawing can, and this withdrawing can also is communicated with the raffinate row mouth of one-level rectifying vaporization integration apparatus and two-stage rectification vaporization integration apparatus.
6. rectifying separation according to claim 1 is produced the device of 7N electronic-grade ultra-pure ammonia, it is characterized in that described finished product accepts charging system and comprise the finished product condenser, the gas phase mouth of finished product condenser is communicated with in the outlet of the ammonia strainer that the outlet with degree of depth purification rectifying tower links to each other, the finished product receiving tank that is connected with finished product condenser liquid phase mouth, finished product receiving tank bottom liquid phase mouth is connected to filling pump, and the filling pump pipeline connection has finished product to fill steel cylinder.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011200666550U CN202030539U (en) | 2011-03-15 | 2011-03-15 | Device for producing 7N electronic grade hyperpure ammonia through rectification separation |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011200666550U CN202030539U (en) | 2011-03-15 | 2011-03-15 | Device for producing 7N electronic grade hyperpure ammonia through rectification separation |
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| CN202030539U true CN202030539U (en) | 2011-11-09 |
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| CN2011200666550U Expired - Lifetime CN202030539U (en) | 2011-03-15 | 2011-03-15 | Device for producing 7N electronic grade hyperpure ammonia through rectification separation |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102730719A (en) * | 2012-07-02 | 2012-10-17 | 大连保税区科利德化工科技开发有限公司 | Industrial ammonia continuous purification apparatus and technology |
| CN102728159A (en) * | 2012-07-13 | 2012-10-17 | 上海正帆科技有限公司 | Method for recovering ammonia gas from MOCVD (metallorganic chemical vapor deposition) tail gas |
| 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 |
| CN109019631A (en) * | 2018-08-24 | 2018-12-18 | 苏州金宏气体股份有限公司 | A kind of production system and production method of ultra-pure ammonia |
| CN110510636A (en) * | 2019-03-22 | 2019-11-29 | 兰州隆华特种气体科技有限公司 | A kind of industrial ammonia and high-purity ammon co-generation system and technique |
-
2011
- 2011-03-15 CN CN2011200666550U patent/CN202030539U/en not_active Expired - Lifetime
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102730719A (en) * | 2012-07-02 | 2012-10-17 | 大连保税区科利德化工科技开发有限公司 | Industrial ammonia continuous purification apparatus and technology |
| CN102728159A (en) * | 2012-07-13 | 2012-10-17 | 上海正帆科技有限公司 | Method for recovering ammonia gas from MOCVD (metallorganic chemical vapor deposition) tail gas |
| 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 |
| CN109019631A (en) * | 2018-08-24 | 2018-12-18 | 苏州金宏气体股份有限公司 | A kind of production system and production method of ultra-pure ammonia |
| CN110510636A (en) * | 2019-03-22 | 2019-11-29 | 兰州隆华特种气体科技有限公司 | A kind of industrial ammonia and high-purity ammon co-generation system and technique |
| CN110510636B (en) * | 2019-03-22 | 2024-04-16 | 兰州隆华特种气体科技有限公司 | Industrial ammonia water and high-purity ammonia co-production system and process |
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| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CX01 | Expiry of patent term |
Granted publication date: 20111109 |
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| CX01 | Expiry of patent term |