CN102730719B - Industrial ammonia continuous purification apparatus and technology - Google Patents
Industrial ammonia continuous purification apparatus and technology Download PDFInfo
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- CN102730719B CN102730719B CN201210223283.7A CN201210223283A CN102730719B CN 102730719 B CN102730719 B CN 102730719B CN 201210223283 A CN201210223283 A CN 201210223283A CN 102730719 B CN102730719 B CN 102730719B
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- tower
- distillation
- strainer
- hot water
- ammonia
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- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 title claims abstract description 81
- 229910021529 ammonia Inorganic materials 0.000 title claims abstract description 33
- 238000005516 engineering process Methods 0.000 title abstract description 8
- 238000000746 purification Methods 0.000 title abstract description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 33
- 238000004821 distillation Methods 0.000 claims abstract description 31
- 238000010438 heat treatment Methods 0.000 claims abstract description 22
- 239000012535 impurity Substances 0.000 claims abstract description 9
- 239000002994 raw material Substances 0.000 claims abstract description 8
- 239000012530 fluid Substances 0.000 claims abstract description 7
- 238000001816 cooling Methods 0.000 claims abstract description 5
- 238000003860 storage Methods 0.000 claims abstract description 4
- 238000000034 method Methods 0.000 claims description 11
- 238000009833 condensation Methods 0.000 claims description 6
- 230000005494 condensation Effects 0.000 claims description 6
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 3
- 229910000831 Steel Inorganic materials 0.000 claims description 3
- 235000011089 carbon dioxide Nutrition 0.000 claims description 3
- 239000000470 constituent Substances 0.000 claims description 3
- 235000019628 coolness Nutrition 0.000 claims description 3
- 239000000945 filler Substances 0.000 claims description 3
- JEGUKCSWCFPDGT-UHFFFAOYSA-N h2o hydrate Chemical compound O.O JEGUKCSWCFPDGT-UHFFFAOYSA-N 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 3
- 239000010959 steel Substances 0.000 claims description 3
- 238000009834 vaporization Methods 0.000 claims description 3
- 230000008016 vaporization Effects 0.000 claims description 3
- 238000010521 absorption reaction Methods 0.000 abstract description 4
- 238000003889 chemical engineering Methods 0.000 abstract 1
- 229910000069 nitrogen hydride Inorganic materials 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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Abstract
The invention relates to an industrial ammonia continuous purification apparatus and a technology employing the apparatus. The invention belongs to the field of chemical engineering. The invention relates to a purification technology with which industrial liquid ammonia is adopted as a raw material for preparing high-purity ammonia required by electronic industries. A raw material tank is connected to a liquid ammonia pump through a pipeline, and is then connected to a filter through the ammonia pump. A distillation tower is then connected. A hot water heating kettle is arranged on the distillation tower. A water cooling device is arranged on the top of the distillation tower. Through the water cooling device, another filter is connected, and a multi-stage absorbing device is connected. A third filter and a flow meter are respectively connected to the top of the multi-stage absorbing device. The other end of the flow meter is directly connected to a rectification tower. A refrigerating fluid condenser is arranged on the top of the rectification tower. The other end of the rectification tower is connected to a hot water heating kettle. A product storage tank is connected at last. According to the invention, a technology of one-tower rectification, multi-stage absorption, and re-rectification is adopted. With the technology, continuous stable operation is realized, and an impurity removal rate is high, such that the product quality is stable. The product purity reaches 99.99999%.
Description
technical fieldthe present invention relates to a kind of continuous purifying industrial ammonia device and technique, belong to chemical field, relate to and take industrial liquid ammonia as raw material, the purifying technique of the high-purity ammon that preparation electronic industry is required.
background technologyin production process of semiconductor, high-purity ammon is for compound semiconductor, flat pannel display, solar cell manufacture and large-scale integrated circuit.
Along with the fast development of microelectronic industry, will there is qualitative leap in ultra large scale integrated circuit (VLSI) and photodiode (LED) manufacturing technology.Therefore, more and more higher to the requirement of high-purity ammon purity.In recent years, the development of China's high-purity ammon has obtained greater advance, and purity approaches foreign level.Be accompanied by the development of semiconductor technology, it will be inevitable selecting practical high-purity ammon.
At present, the technique of the purification ammonia technique that adopts a tower rectifying, multistage absorption more, some rectifying or step, this technical process shortcoming is that technological parameter fluctuation is larger, affects quality product, suddenly waits to improve.
summary of the inventionthe present invention is in order to make up above-mentioned technological deficiency, and a kind of continuous purifying industrial ammonia device and technique are provided, and this invention adopts a tower rectifying, multistage absorption, rectifying again, realized continuous and stable operation, removal of impurity is high, thereby makes constant product quality, and purity is up to 99.99999%.
To achieve these goals, technical scheme of the present invention is as follows:
A continuous purifying industrial ammonia device, comprises head tank, strainer, distillation tower, watercooler, multistage adsorber, rectifying tower, refrigerating fulid condenser, product stock tank, ammonia pump, hot water heating still and under meter; Head tank is through pipeline connecting fluid ammonia pump, through ammonia pump, be connected with strainer, then connect distillation tower, on distillation tower, be provided with hot water heating still, at distillation tower top, be provided with watercooler, through watercooler, again connect strainer, then connect multistage adsorber, on multistage adsorber top, connect respectively strainer and under meter, the under meter the other end directly connects rectifying tower, rectifying tower top is provided with refrigerating fulid condenser, meanwhile, at the rectifying tower the other end, connect hot water heating still, finally connect product stock tank.
Its technical process is as follows:
In the incoming stock tank of raw material, with ammonia pump, through strainer, remove oil and mechanical impurity, strainer with 40 ~ 50kg/h after under meter metering, enter in distillation tower, the vaporization of hot water heating still and the condensation of overhead water water cooler at the bottom of tower, distill 38 ~ 45 ℃ of hot water heatings for distillation tower 3 bottoms, 20 ~ 30 ℃ of water coolings for tower top.Heavy constituent impurity after distillation is got rid of at the bottom of being transported to tower, and tower bottom pressure is controlled at 1 ~ 1.1MPa, and tower top pressure is controlled at 0.9MPa left and right.Gas phase is filtered through strainer, enter multistage adsorber and remove wherein water and carbonic acid gas, outlet NH3 pressure is 0.5MPa, through under meter, measure, then enter into rectifying in rectifying tower, in tower, fill θ ring filler, by hot water heating still at the bottom of tower top freezer condenser and tower, form precise distillation, tower top makes it liquefaction with-5 ~-10 ℃ of cryogenic condensation liquid cold gas NH3, at the bottom of tower, with 15 ~ 20 ℃ of water, heats.After precise distillation, be condensed into liquefied ammonia, at the bottom of tower, discharge high-purity fluid NH3 product, can directly rush dress 40L, 200L, 900L steel cylinder, also can be filled into product storage tank 3(20M3).
Beneficial effect of the present invention is: adopt a tower rectifying, multistage absorption, the technique of rectifying again, realized continuous and stable operation, removal of impurity is high, thereby makes constant product quality, and purity is up to 99.99999%.
Accompanying drawing explanation
Fig. 1 is the structural representation of continuous purifying industrial ammonia device.
In figure, 1, head tank, 2, strainer one, 3, distillation tower 4, watercooler, 5, multistage adsorber, 6, rectifying tower, 7, refrigerating fulid condenser, 8, product stock tank, 9, ammonia pump, 10, hot water heating still one, 11, under meter one, 12, strainer two, 13, strainer three, 14, hot water heating still two, 15, under meter two.
Embodiment
Below in conjunction with accompanying drawing and specific examples, the present invention is described in detail:
In figure, comprise head tank 1, strainer 2, distillation tower 3, watercooler 4, multistage adsorber 5, rectifying tower 6, refrigerating fulid condenser 7, product stock tank 8, ammonia pump 9, hot water heating still 10 and under meter 11, head tank 1 is through pipeline connecting fluid ammonia pump 9, through ammonia pump 9, be connected with strainer 1, then connect distillation tower 3, on distillation tower 3, be provided with hot water heating still 10, at distillation tower 3 tops, be provided with watercooler 4, through watercooler 4, again connect strainer 2 12, then connect multistage adsorber 5, on multistage adsorber 5 tops, connect respectively strainer 3 13 and under meter 15, under meter 15 the other ends directly connect rectifying tower 6, rectifying tower 6 tops are provided with refrigerating fulid condenser 7, simultaneously, at rectifying tower 6 the other ends, connect hot water heating still 2 14, finally connect product stock tank 8.
In the incoming stock tank 1 of raw material, with ammonia pump 9, through strainer 1, remove oil and mechanical impurity, strainer with 40 ~ 50kg/h after under meter 1 metering, enter in distillation tower 3, hot water heating still one 10 vaporizations and 4 condensations of overhead water water cooler at the bottom of tower, distill 38 ~ 45 ℃ of hot water heatings for distillation tower 3 bottoms, 20 ~ 30 ℃ of water coolings for tower top.Heavy constituent impurity after distillation is got rid of at the bottom of being transported to tower, and tower bottom pressure is controlled at 1 ~ 1.1MPa, and tower top pressure is controlled at 0.9MPa left and right.Gas phase is filtered through strainer 2 12, enter multistage adsorber 5 and remove wherein water and carbonic acid gas, outlet NH3 pressure is 0.5MPa, through under meter 2 15 meterings, then enter into the interior rectifying of rectifying tower 6, in tower, fill θ ring filler, by tower top freezer condenser 7 and hot water heating still 2 14 at the bottom of tower, form precise distillation, tower top makes it liquefaction with-5 ~-10 ℃ of cryogenic condensation liquid cold gas NH3, at the bottom of tower, with 15 ~ 20 ℃ of water, heats.After precise distillation, be condensed into liquefied ammonia, at the bottom of tower, discharge high-purity fluid NH3 product, can directly rush dress 40L, 200L, 900L steel cylinder, also can be filled into product storage tank 8(20M3).
In order to confirm its liquefied ammonia purification degree, the present invention carries out data declaration by specific embodiment:
Raw materials ammonia concentration is 99.5% industrial ammonia, and can obtain liquefied ammonia purity after adopting above-mentioned technique to purify is 99.99999%, and foreign matter content contrast is as follows:
Workshop can obtain the high-purity ammoniacal liquor NH of 32kg with 40kg raw materials ammonia per hour
3product is example, produces continuously, and product data are as follows:
Claims (1)
1. a continuous purifying industrial ammonia process, it is characterized in that using continuous purifying industrial ammonia device, said apparatus comprises head tank, strainer, distillation tower, watercooler, multistage adsorber, rectifying tower, refrigerating fulid condenser, product stock tank, ammonia pump, hot water heating still and under meter; Head tank is through pipeline connecting fluid ammonia pump, through ammonia pump, be connected with strainer, then connect distillation tower, on distillation tower, be provided with hot water heating still, at distillation tower top, be provided with watercooler, through watercooler, again connect strainer, then connect multistage adsorber, on multistage adsorber top, connect respectively strainer and under meter, the under meter the other end directly connects rectifying tower, rectifying tower top is provided with refrigerating fulid condenser, meanwhile, at the rectifying tower the other end, connect hot water heating still, finally connect product stock tank; Carry out in accordance with the following steps: in the incoming stock tank of raw material, with ammonia pump, through strainer, remove oil and mechanical impurity, strainer with 40 ~ 50kg/h after under meter metering, enter in distillation tower, the vaporization of hot water heating still and the condensation of overhead water water cooler at the bottom of tower, distill distillation tower (3) 38 ~ 45 ℃ of hot water heatings, 20 ~ 30 ℃ of water coolings for tower top for bottom; Heavy constituent impurity after distillation is got rid of at the bottom of being transported to tower, and tower bottom pressure is controlled at 1 ~ 1.1MPa, and tower top pressure is controlled at 0.9MPa; Gas phase is filtered through strainer, enters multistage adsorber and removes wherein water and carbonic acid gas, outlet NH
3pressure is 0.5MPa, through under meter metering, then enters into rectifying in rectifying tower, fills θ ring filler in tower, forms precise distillation ,-5 ~-10 ℃ of cryogenic condensation liquid cold gas NH for tower top by hot water heating still at the bottom of tower top freezer condenser and tower
3make it liquefaction, at the bottom of tower, with 15 ~ 20 ℃ of water, heat; After precise distillation, be condensed into liquefied ammonia, at the bottom of tower, discharge high-purity fluid NH
3product, directly fills 40L, 200L, 900L steel cylinder, or is filled into product storage tank (8) 20M
3.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210223283.7A CN102730719B (en) | 2012-07-02 | 2012-07-02 | Industrial ammonia continuous purification apparatus and technology |
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|---|---|---|---|
| CN201210223283.7A CN102730719B (en) | 2012-07-02 | 2012-07-02 | Industrial ammonia continuous purification apparatus and technology |
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| CN102730719A CN102730719A (en) | 2012-10-17 |
| CN102730719B true CN102730719B (en) | 2014-02-26 |
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN106495183B (en) * | 2016-11-07 | 2018-12-18 | 广东华特气体股份有限公司 | A kind of purification process of ammonia |
| CN106673013B (en) * | 2016-11-17 | 2018-10-09 | 天津大学 | The reprocessing process and system of unqualified liquefied ammonia in refinery(waste) water production |
| CN112299445B (en) * | 2020-11-20 | 2022-05-10 | 苏州金宏气体股份有限公司 | Method for preparing ultra-pure ammonia by filler rectification |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102249259A (en) * | 2010-05-19 | 2011-11-23 | 上海普锐克索特种气体有限公司 | Purification process of high-purity ammonia |
| JP5636261B2 (en) * | 2010-11-02 | 2014-12-03 | 住友精化株式会社 | Ammonia purification system |
| CN202030539U (en) * | 2011-03-15 | 2011-11-09 | 苏州金宏气体股份有限公司 | Device for producing 7N electronic grade hyperpure ammonia through rectification separation |
| CN202705056U (en) * | 2012-07-02 | 2013-01-30 | 大连保税区科利德化工科技开发有限公司 | Device for continuously purifying industrial ammonia |
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Application publication date: 20121017 Assignee: Quanjiao kelide Electronic Materials Co.,Ltd. Assignor: Zhao Yi|Zhao Chao|Ji Yanqiu|Wang Tianyuan Contract record no.: X2020340000006 Denomination of invention: A device and process for continuous purification of industrial ammonia Granted publication date: 20140226 License type: Exclusive License Record date: 20200806 |
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Denomination of invention: A device and process for continuous purification of industrial ammonia Effective date of registration: 20220927 Granted publication date: 20140226 Pledgee: China Minsheng Bank Co.,Ltd. Dalian Branch Pledgor: DALIAN FREE TRADE ZONE CREDIT CHEMICAL SCIENCE AND TECHNOLOGY DEVELOPMENT CO.,LTD. Registration number: Y2022980016620 |
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