CN102730719A - Industrial ammonia continuous purification apparatus and technology - Google Patents
Industrial ammonia continuous purification apparatus and technology Download PDFInfo
- Publication number
- CN102730719A CN102730719A CN2012102232837A CN201210223283A CN102730719A CN 102730719 A CN102730719 A CN 102730719A CN 2012102232837 A CN2012102232837 A CN 2012102232837A CN 201210223283 A CN201210223283 A CN 201210223283A CN 102730719 A CN102730719 A CN 102730719A
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- Prior art keywords
- 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 88
- 229910021529 ammonia Inorganic materials 0.000 title claims abstract description 34
- 238000005516 engineering process Methods 0.000 title claims abstract description 16
- 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 19
- 239000012535 impurity Substances 0.000 claims abstract description 9
- 239000002994 raw material Substances 0.000 claims abstract description 8
- 238000001816 cooling Methods 0.000 claims abstract description 5
- 239000012530 fluid Substances 0.000 claims abstract description 4
- 238000003860 storage Methods 0.000 claims abstract description 4
- 229910000069 nitrogen hydride Inorganic materials 0.000 claims description 9
- 241000282326 Felis catus Species 0.000 claims description 6
- 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
- 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
- 238000012856 packing Methods 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
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000010924 continuous production Methods 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 technology, belong to chemical field, relating to industrial liquefied ammonia is raw material, the purifying technique of the high-purity ammon that the preparation electronic industry is required.
Background technologyIn production process of semiconductor, high-purity ammon is used for compound semiconductor, FPD, solar cell manufacturing and large-scale integrated circuit.
Along with the fast development of microelectronic industry, qualitative leap will take place in ULSI (VLSI) and photodiode (LED) manufacturing technology.Therefore, to high-purity ammon purity require increasingly high.In recent years, the development of China's high-purity ammon has obtained bigger progress, and purity is near foreign level.Be accompanied by development of semiconductor, it will be inevitable selecting practical high-purity ammon.
At present, the technology of the purification ammonia technologies that adopt a tower rectifying, multistage absorption more, the rectifying that has still is step, and this technical process shortcoming is that technological parameter fluctuation is bigger, influences quality product, suddenly waits to improve.
Summary of the inventionThe present invention is in order to remedy above-mentioned technological deficiency, a kind of continuous purifying industrial ammonia device and technology to be provided, this invention employing one tower rectifying, multistage absorption, rectifying again; Realized continuous quiet run; 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 following:
A kind of continuous purifying industrial ammonia device comprises head tank, strainer, distillation tower, watercooler, multistage adsorber, rectifying tower, refrigerating fulid condensing surface, product stock jar, ammonia pump, hot water heating kettle and under meter; Head tank connects ammonia pump through pipeline, links to each other with strainer through ammonia pump, connects distillation tower then; On distillation tower, be provided with the hot water heating kettle, be provided with watercooler, through watercooler at the distillation tower top; Connect strainer once more, connect multistage adsorber then, connect strainer and under meter respectively on multistage adsorber top; The under meter the other end directly connects rectifying tower, and the rectifying tower top is provided with the refrigerating fulid condensing surface, simultaneously; Connect the hot water heating kettle at the rectifying tower the other end, connect the product stock jar at last.
Its technical process is following:
In incoming stock jar of the raw material; Remove oil and mechanical impurity with ammonia pump through strainer, strainer, enters in the distillation tower after the under meter metering with 40 ~ 50kg/h; Vaporization of hot water heating kettle and the condensation of overhead water water cooler at the bottom of tower; Distill, heat with 38 ~ 45 ℃ of hot water distillation tower 3 bottoms, and cat head is with 20 ~ 30 ℃ of water coolings.Heavy constituent impurity after the 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 about 0.9MPa.Gas phase is filtered through strainer, gets into multistage adsorber and removes wherein water and carbonic acid gas, and outlet NH3 pressure is 0.5MPa; Measure through under meter; Enter into rectifying in the rectifying tower then, fill the θ ring packing in the tower, constitute precise distillation by hot water heating kettle at the bottom of cat head freezer condenser and the tower; Cat head makes it liquefaction with-5 ~-10 ℃ of cryogenic condensation liquid cold gas NH3, heats with 15 ~ 20 ℃ of water at the bottom of the tower.Behind precise distillation, be condensed into liquefied ammonia, discharge high-purity fluid NH3 product at the bottom of the tower, can directly dash 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 technology of rectifying again, realized continuous quiet run, removal of impurity is high, thereby makes constant product quality, and purity is up to 99.99999%.
Description of drawings
Fig. 1 is the structural representation of continuous purifying industrial ammonia device.
Among the figure, 1, head tank, 2, strainer one, 3, distillation tower 4, watercooler; 5, multistage adsorber, 6, rectifying tower, 7, the refrigerating fulid condensing surface, 8, the product stock jar; 9, ammonia pump, 10, hot water heating kettle one, 11, under meter one, 12, strainer two; 13, strainer three, 14, hot water heating kettle two, 15, under meter two.
Embodiment
Below in conjunction with accompanying drawing and specific examples the present invention is elaborated:
Among the figure, comprise head tank 1, strainer 2, distillation tower 3, watercooler 4, multistage adsorber 5, rectifying tower 6, refrigerating fulid condensing surface 7, product stock jar 8, ammonia pump 9, hot water heating kettle 10 and under meter 11; Head tank 1 connects ammonia pump 9 through pipeline, links to each other with strainer 1 through ammonia pump 9, connects distillation tower 3 then; On distillation tower 3, be provided with hot water heating kettle 10, be provided with watercooler 4, through watercooler 4 at distillation tower 3 tops; Connect strainer 2 12 once more, connect multistage adsorber 8 then, connect strainer 3 13 and under meter 15 respectively on multistage adsorber 8 tops; Under meter 15 the other ends directly connect rectifying tower 6, and rectifying tower 6 tops are provided with refrigerating fulid condensing surface 7, simultaneously; Connect hot water heating kettle 2 14 at rectifying tower 6 the other ends, connect product stock jar 8 at last.
In incoming stock jar 1 of the raw material; Remove oil and mechanical impurity with ammonia pump 9 through strainer 1, strainer, enters in the distillation tower 3 after under meter one 11 meterings with 40 ~ 50kg/h; Hot water heating kettle one 10 vaporizations and 4 condensations of overhead water water cooler at the bottom of tower; Distill, heat with 38 ~ 45 ℃ of hot water distillation tower 3 bottoms, and cat head is with 20 ~ 30 ℃ of water coolings.Heavy constituent impurity after the 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 about 0.9MPa.Gas phase is filtered through strainer 2 12, gets into multistage adsorber 5 and removes wherein water and carbonic acid gas, and outlet NH3 pressure is 0.5MPa; Through under meter 2 15 meterings; Enter into rectifying in the rectifying tower 6 then, fill the θ ring packing in the tower, constitute precise distillation by cat head freezer condenser 7 and hot water heating kettle 2 14 at the bottom of the tower; Cat head makes it liquefaction with-5 ~-10 ℃ of cryogenic condensation liquid cold gas NH3, heats with 15 ~ 20 ℃ of water at the bottom of the tower.Behind precise distillation, be condensed into liquefied ammonia, discharge high-purity fluid NH3 product at the bottom of the tower, can directly dash 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 through specific embodiment:
Raw materials ammonia concentration is 99.5% industrial ammonia, and can obtain liquefied ammonia purity after adopting above-mentioned technology to purify is 99.99999%, and foreign matter content contrasts as follows:
The workshop can obtain the high-purity ammoniacal liquor NH of 32kg with 40kg raw materials ammonia per hour
3Product is an example, continuous production, and product data are following:
Claims (2)
1. continuous purifying industrial ammonia device and technology is characterized in that comprising head tank, strainer, distillation tower, watercooler, multistage adsorber, rectifying tower, refrigerating fulid condensing surface, product stock jar, ammonia pump, hot water heating kettle and under meter; Head tank connects ammonia pump through pipeline, links to each other with strainer through ammonia pump, connects distillation tower then; On distillation tower, be provided with the hot water heating kettle, be provided with watercooler, through watercooler at the distillation tower top; Connect strainer once more, connect multistage adsorber then, connect strainer and under meter respectively on multistage adsorber top; The under meter the other end directly connects rectifying tower, and the rectifying tower top is provided with the refrigerating fulid condensing surface, simultaneously; Connect the hot water heating kettle at the rectifying tower the other end, connect the product stock jar at last.
2. a kind of continuous purifying industrial ammonia device according to claim 1 and technology is characterized in that removing oil and mechanical impurity with ammonia pump through strainer in the incoming stock jar of raw material; Strainer with 40 ~ 50kg/h after under meter metering; Enter in the distillation tower, vaporization of hot water heating kettle and the condensation of overhead water water cooler are distilled at the bottom of tower; Heat with 38 ~ 45 ℃ of hot water distillation tower 3 bottoms, and cat head is with 20 ~ 30 ℃ of water coolings; Heavy constituent impurity after the 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 about 0.9MPa; Gas phase is filtered through strainer, gets into multistage adsorber and removes wherein water and carbonic acid gas, and outlet NH3 pressure is 0.5MPa; Measure through under meter; Enter into rectifying in the rectifying tower then, fill the θ ring packing in the tower, constitute precise distillation by hot water heating kettle at the bottom of cat head freezer condenser and the tower; Cat head makes it liquefaction with-5 ~-10 ℃ of cryogenic condensation liquid cold gas NH3, heats with 15 ~ 20 ℃ of water at the bottom of the tower; Behind precise distillation, be condensed into liquefied ammonia, discharge high-purity fluid NH3 product at the bottom of the tower, can directly collide 40L, 200L, 900L steel cylinder, also can be filled into product storage tank 3 (20M
3).
Priority Applications (1)
| 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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| 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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| CN102730719A true CN102730719A (en) | 2012-10-17 |
| CN102730719B CN102730719B (en) | 2014-02-26 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103073026A (en) * | 2013-02-07 | 2013-05-01 | 周礼誉 | Ammonia gas recovery system |
| CN106495183A (en) * | 2016-11-07 | 2017-03-15 | 广东华特气体股份有限公司 | A kind of purification process of ammonia |
| WO2018090460A1 (en) * | 2016-11-17 | 2018-05-24 | 天津大学 | Re-refining process and system for use with unqualified liquid ammonia in oil refining waste water production |
| CN112299445A (en) * | 2020-11-20 | 2021-02-02 | 苏州金宏气体股份有限公司 | Method for preparing ultra-pure ammonia by filler rectification |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| 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 |
| CN102464341A (en) * | 2010-11-02 | 2012-05-23 | 住友精化株式会社 | System for purifying ammonia |
| 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 |
-
2012
- 2012-07-02 CN CN201210223283.7A patent/CN102730719B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN102464341A (en) * | 2010-11-02 | 2012-05-23 | 住友精化株式会社 | System for purifying ammonia |
| 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 |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103073026A (en) * | 2013-02-07 | 2013-05-01 | 周礼誉 | Ammonia gas recovery system |
| 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 |
| CN106495183A (en) * | 2016-11-07 | 2017-03-15 | 广东华特气体股份有限公司 | A kind of purification process of ammonia |
| 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 |
| WO2018090460A1 (en) * | 2016-11-17 | 2018-05-24 | 天津大学 | Re-refining process and system for use with unqualified liquid ammonia in oil refining waste water production |
| CN112299445A (en) * | 2020-11-20 | 2021-02-02 | 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 | Publication date |
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| CN102730719B (en) | 2014-02-26 |
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Effective date of registration: 20180607 Address after: No. 8, Huayuan street, Shangcheng, Ganjingzi District, Dalian, Liaoning 2-4-1 Co-patentee after: Zhao Chao Patentee after: Zhao Yi Co-patentee after: Ji Yanqiu Co-patentee after: Wang Tianyuan Address before: 116600 Liaoning Dalian bonded area storage processing area IE-33 Patentee before: DALIAN FREE TRADE ZONE CREDIT CHEMICAL SCIENCE AND TECHNOLOGY DEVELOPMENT CO.,LTD. |
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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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Effective date of registration: 20210317 Address after: 116600 Liaoning Dalian bonded area storage processing area IE-33 Patentee after: DALIAN FREE TRADE ZONE CREDIT CHEMICAL SCIENCE AND TECHNOLOGY DEVELOPMENT Co.,Ltd. Address before: No. 8, Huayuan street, Shangcheng, Ganjingzi District, Dalian, Liaoning 2-4-1 Patentee before: Zhao Yi Patentee before: Zhao Chao Patentee before: Ji Yanqiu Patentee before: Wang Tianyuan |
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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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Address after: No. 1-1, Haike Road, Dalian Free Trade Zone, Liaoning 116600 Patentee after: Dalian Kelide Semiconductor Materials Co.,Ltd. Address before: 116600 Liaoning Dalian bonded area storage processing area IE-33 Patentee before: DALIAN FREE TRADE ZONE CREDIT CHEMICAL SCIENCE AND TECHNOLOGY DEVELOPMENT CO.,LTD. |
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Assignee: Quanjiao kelide Electronic Materials Co.,Ltd. Assignor: Zhao Yi|Zhao Chao|Ji Yanqiu|Wang Tianyuan Contract record no.: X2020340000006 Date of cancellation: 20230419 |
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Date of cancellation: 20230529 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 |