CN101890332A - Preparation method of special high-performance 5A molecular sieve for pressure swing adsorption - Google Patents
Preparation method of special high-performance 5A molecular sieve for pressure swing adsorption Download PDFInfo
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- CN101890332A CN101890332A CN 201010241693 CN201010241693A CN101890332A CN 101890332 A CN101890332 A CN 101890332A CN 201010241693 CN201010241693 CN 201010241693 CN 201010241693 A CN201010241693 A CN 201010241693A CN 101890332 A CN101890332 A CN 101890332A
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- Prior art keywords
- molecular sieve
- pressure swing
- performance
- swing adsorption
- preparation
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- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Links
- 239000002808 molecular sieve Substances 0.000 title claims abstract description 41
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 title claims abstract description 41
- 238000001179 sorption measurement Methods 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 238000001354 calcination Methods 0.000 claims abstract description 14
- 239000005995 Aluminium silicate Substances 0.000 claims abstract description 12
- 235000012211 aluminium silicate Nutrition 0.000 claims abstract description 12
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000000843 powder Substances 0.000 claims abstract description 12
- 238000005406 washing Methods 0.000 claims abstract description 11
- 239000000243 solution Substances 0.000 claims description 10
- 230000004913 activation Effects 0.000 claims description 9
- 238000005469 granulation Methods 0.000 claims description 9
- 230000003179 granulation Effects 0.000 claims description 9
- 235000008733 Citrus aurantifolia Nutrition 0.000 claims description 8
- 235000011941 Tilia x europaea Nutrition 0.000 claims description 8
- 238000005342 ion exchange Methods 0.000 claims description 8
- 239000004571 lime Substances 0.000 claims description 8
- 239000000126 substance Substances 0.000 claims description 7
- 239000007864 aqueous solution Substances 0.000 claims description 6
- 150000001875 compounds Chemical class 0.000 claims description 2
- 229920006395 saturated elastomer Polymers 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 abstract description 14
- 229910052757 nitrogen Inorganic materials 0.000 abstract description 7
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 6
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 238000002156 mixing Methods 0.000 abstract description 6
- 239000001301 oxygen Substances 0.000 abstract description 6
- 229910052760 oxygen Inorganic materials 0.000 abstract description 6
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical class [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 abstract description 5
- 239000002351 wastewater Substances 0.000 abstract description 5
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract description 4
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 abstract description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 abstract description 3
- 229910002091 carbon monoxide Inorganic materials 0.000 abstract description 3
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 abstract description 2
- 239000003513 alkali Substances 0.000 abstract description 2
- 239000001110 calcium chloride Substances 0.000 abstract description 2
- 229910001628 calcium chloride Inorganic materials 0.000 abstract description 2
- 238000003795 desorption Methods 0.000 abstract description 2
- DOTMOQHOJINYBL-UHFFFAOYSA-N molecular nitrogen;molecular oxygen Chemical compound N#N.O=O DOTMOQHOJINYBL-UHFFFAOYSA-N 0.000 abstract description 2
- 238000004806 packaging method and process Methods 0.000 abstract description 2
- 239000003208 petroleum Substances 0.000 abstract description 2
- 230000003213 activating effect Effects 0.000 abstract 1
- 239000004927 clay Substances 0.000 abstract 1
- 230000006835 compression Effects 0.000 abstract 1
- 238000007906 compression Methods 0.000 abstract 1
- 239000013078 crystal Substances 0.000 abstract 1
- 238000001035 drying Methods 0.000 abstract 1
- 238000000746 purification Methods 0.000 abstract 1
- 230000001131 transforming effect Effects 0.000 abstract 1
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 12
- 238000010521 absorption reaction Methods 0.000 description 8
- 239000003463 adsorbent Substances 0.000 description 6
- 238000000034 method Methods 0.000 description 6
- 239000001257 hydrogen Substances 0.000 description 4
- 229910052739 hydrogen Inorganic materials 0.000 description 4
- 238000004065 wastewater treatment Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 2
- 230000009466 transformation Effects 0.000 description 2
- 241000370738 Chlorion Species 0.000 description 1
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 230000002779 inactivation Effects 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 239000003595 mist Substances 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
Landscapes
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Silicates, Zeolites, And Molecular Sieves (AREA)
Abstract
The invention relates to a preparation method of a special high-performance 5A molecular sieve for pressure swing adsorption, which comprises the following steps of: mixing and granulating 4A molecular sieve raw powder and kaolin clay, drying, calcining, washing with alkali and transforming crystals, exchanging, activating, packaging and the like. The invention has the characteristics that saturated lime water is used for exchanging, thereby avoiding the problem of difficult wastewater processing caused by high content of wastewater chloride ions when calcium chloride is used for exchanging in traditional production. The 5A molecular sieve of the invention has large adsorption capacity, high adsorption and desorption speed and high mechanical strength, the nitrogen adsorption capacity is larger than 15ml/g, the nitrogen-oxygen adsorption ratio is larger than 3.2, the carbon monoxide adsorption capacity is larger than 30ml/g, and the compression strength is larger than 50N. The product is used for pressure swing adsorption and oxygen production, the purification of hydrogen gas and carbon monoxide and the dewaxing of petroleum refineries.
Description
Technical field
The present invention relates to a kind of preparation method of molecular sieve, be specifically related to a kind of preparation method of special high-performance 5 A molecular sieve for pressure swing adsorption.
Background technology
Transformation absorption (PSA) now has been widely used for the isolation of purified of mist as a kind of chemical unit technology.Along with the development of pressure swing adsorption and the maximization of device, be 200000Nm as handling tolerance
3/ hr separates the device of purifying hydrogen of hydrogen, and adsorbent is also had higher requirement, and requires the adsorption capacity of adsorbent big, absorption and desorption rate is fast, mechanical strength is high.Along with development and national economy, country is to the reinforcement of environmental protection dynamics simultaneously, and the wastewater treatment in the adsorbent production also is the problem that adsorbent manufacturer faces.
The 5A molecular sieve is as the adsorbent of omnibus control system, purifying hydrogen of hydrogen and carbon monoxide and petroleum refinery's dewaxing, and traditional production method is that 4A molecular screen primary powder and kaolin mixing granulation, oven dry, calcining, alkali cleaning are changeed brilliant change brilliant, CaCl
2Exchange, activation, packaging and other steps are formed, owing to make waste water chloride ion content height with the calcium chloride exchange, the waste water that chloride ion content is high causes the living beings inactivation of sewage disposal easily, runs into the problem of wastewater treatment difficulty; The adsorbents adsorb capacity that traditional in addition production method is produced is not high yet, does not satisfy the requirement of present transformation absorption large-scale plant.As the 5A molecular sieve of Chinese patent CN1087030A preparation, its nitrogen adsorbance is 9.96 to 13.5mg/g, and the oxygen adsorbance is 4.6 to 6.03mg/g, and the absorption of nitrogen oxygen is than 1.84 to 2.45; The 5A molecular sieve of CN1724141A preparation, its CO adsorbance are 23.1 to 26.4ml/g; The 5A molecular sieve of Chinese patent CN1292831C preparation, its pure oxygen productive rate are 20.00 to 23.10Nm
3/ hrkg.
Summary of the invention
The objective of the invention is to propose in order to address the deficiencies of the prior art a kind of pollution less, the preparation method of special high-performance 5 A molecular sieve for pressure swing adsorption that adsorption capacity is high.
Preparation method of the present invention is achieved in that
4A molecular screen primary powder and the kaolin that accounts for 4A molecular screen primary powder 10 to 30% weight ratios are mixed at mixer, with compound granulation on nodulizer, the oven dry of 4A molecular sieve, calcining with granulation, kaolin in the 4A molecular sieve of calcining is changeed crystalline substance make adhesive-free 4A molecular sieve, adhesive-free 4A molecular sieve and lime aqueous solution are carried out ion-exchange, and the exchange temperature is 70 to 100 ℃, is preferably 85 to 95 ℃, exchange degree is 60 to 90%, is preferably 80 to 90%; After meeting the requirements of exchange degree,,, promptly obtain special high-performance 5 A molecular sieve for pressure swing adsorption 350 to 550 ℃ of activation through washing, oven dry.
Further scheme is: described kaolin accounts for 4A molecular screen primary powder 15 to 22% weight ratios.
Wherein said lime aqueous solution is with the lime saturated aqueous solution of making soluble in water under 25 to 95 ℃;
Further scheme is: the lime solution temperature is 40 to 60 ℃.
Further scheme is: described ion-exchange temperature is 85 to 95 ℃, and exchange degree is 80 to 90%.
Further scheme is: described activation temperature is 380 to 450 ℃.
Preparation method of the present invention has the following advantages:
1, can significantly improve the adsorption capacity of 5A molecular sieve, the adsorbance of nitrogen can improve 12 to 26%, and the CO adsorbance can improve 15 to 29%;
2, method has been avoided the discharging of chlorion, reduces the content of COD in the waste water, has solved the problem of traditional production method wastewater treatment difficulty;
3, method is simple, expends cheap.
The specific embodiment:
The present invention is described in further detail below in conjunction with embodiment.
Embodiment 1
Get 80 parts of (weight) 4A molecular screen primary powders and 24 parts of (weight) kaolin mixing granulations, through sieve the 4A molecular sieve of ￠ 2 to 2.5m m, 150 ℃ of oven dry, 640 ℃ of calcinings, 4A molecular sieve after the calcining is 90 ℃ with the NaOH solution of 8% weight ratio in temperature to be changeed crystalline substance and obtains adhesive-free 4A molecular sieve, after washing, carry out ion-exchange with saturated limewater solution at 92 ℃, again when exchange degree to 70%, washing, 150 ℃ of oven dry, 420 ℃ of activation.The product strength that obtains is 53.4N/, uses the volume absorption method at 25 ℃, 101.325 * 10
3Recording the nitrogen adsorbance under the Pa is 14.36ml/g, and the adsorbance of oxygen is 4.35ml/g, and the CO adsorbance is 31.72ml/g, CH
4Adsorbance is 16.56ml/g.
Embodiment 2
80 parts of (weight) 4A molecular screen primary powders and 22 parts of (weight) kaolin mixing granulations, through sieve the 4A molecular sieve of ￠ 2 to 2.5mm, 150 ℃ of oven dry, 650 ℃ of calcinings, 4A molecular sieve after the calcining is 91 ℃ with the NaOH solution of 8% weight ratio in temperature to be changeed crystalline substance and obtains adhesive-free 4A molecular sieve, after washing, carry out ion-exchange for 92 ℃ with saturated limewater solution, again when exchange degree to 80%, washing, 150 ℃ of oven dry, 420 ℃ of activation.The product strength that obtains is 52.9N/, uses the volume absorption method at 25 ℃, 101.325 * 10
3Recording the nitrogen adsorbance under the Pa is 15.13ml/g, and the adsorbance of oxygen is 4.61ml/g, and the CO adsorbance is 32.37ml/g, CH
4Adsorbance is 17.68ml/g.
Embodiment 3
80 parts of (weight) 4A molecular screen primary powders and 22 parts of (weight) kaolin mixing granulations, through sieve the 4A molecular sieve of ￠ 2 to 2.5mm, 150 ℃ of oven dry, 635 ℃ of calcinings, 4A molecular sieve after the calcining is 91 ℃ with the NaOH solution of 8% weight ratio in temperature to be changeed crystalline substance and obtains adhesive-free 4A molecular sieve, after washing, carry out ion-exchange for 92 ℃ with saturated limewater solution, again when exchange degree to 88%, washing, 150 ℃ of oven dry, 430 ℃ of activation.The product strength that obtains is 53.9N/, uses the volume absorption method at 25 ℃, 101.325 * 10
3Recording the nitrogen adsorbance under the Pa is 16.43ml/g, and the adsorbance of oxygen is 5.11ml/g, and the CO adsorbance is 34.67ml/g, CH
4Adsorbance is 18.69ml/g.
Embodiment 4
80 parts of (weight) 4A molecular screen primary powders and 22 parts of (weight) kaolin mixing granulations, through sieve the 4A molecular sieve of ￠ 2 to 2.5mm, 150 ℃ of oven dry, 640 ℃ of calcinings, 4A molecular sieve after the calcining is 93 ℃ with the NaOH solution of 8% weight ratio in temperature to be changeed crystalline substance and obtains adhesive-free 4A molecular sieve, after washing, carry out ion-exchange for 95 ℃ with saturated limewater solution, again when exchange degree to 90%, washing, 150 ℃ of oven dry, 420 ℃ of activation.The product strength that obtains is 61.4N/, uses the volume absorption method at 25 ℃, 101.325 * 10
3Recording the nitrogen adsorbance under the Pa is 15.86ml/g, and the adsorbance of oxygen is 4.82ml/g, and the CO adsorbance is 33.82ml/g, CH
4Adsorbance is 18.28ml/g.
Claims (6)
1. the preparation method of a special high-performance 5 A molecular sieve for pressure swing adsorption, it is characterized in that 4A molecular screen primary powder and the kaolin that accounts for 4A molecular screen primary powder 10 to 30% weight ratios are mixed at mixer, with compound granulation on nodulizer, the oven dry of 4A molecular sieve, calcining with granulation, kaolin in the 4A molecular sieve of calcining is changeed crystalline substance make adhesive-free 4A molecular sieve, adhesive-free 4A molecular sieve and lime aqueous solution are carried out ion-exchange, the exchange temperature is 70 to 100 ℃, be preferably 85 to 95 ℃, exchange degree is 60 to 90%, is preferably 80 to 90%; After meeting the requirements of exchange degree,,, promptly obtain special high-performance 5 A molecular sieve for pressure swing adsorption 350 to 550 ℃ of activation through washing, oven dry.
2. the preparation method of special high-performance 5 A molecular sieve for pressure swing adsorption according to claim 1 is characterized in that described kaolin accounts for 4A molecular screen primary powder 15 to 22% weight ratios.
3. the preparation method of special high-performance 5 A molecular sieve for pressure swing adsorption according to claim 1 is characterized in that described lime aqueous solution is with the lime saturated aqueous solution of making soluble in water under 25 to 95 ℃.
4. the preparation method of special high-performance 5 A molecular sieve for pressure swing adsorption according to claim 3 is characterized in that described lime solution temperature is 40 to 60 ℃.
5. the preparation method of special high-performance 5 A molecular sieve for pressure swing adsorption according to claim 1 is characterized in that described ion-exchange temperature is 85 to 95 ℃, and exchange degree is 80 to 90%.
6. the preparation method of special high-performance 5 A molecular sieve for pressure swing adsorption according to claim 1 is characterized in that described activation temperature is 380 to 450 ℃.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010102416935A CN101890332B (en) | 2010-07-30 | 2010-07-30 | Preparation method of special high-performance 5A molecular sieve for pressure swing adsorption |
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| CN2010102416935A CN101890332B (en) | 2010-07-30 | 2010-07-30 | Preparation method of special high-performance 5A molecular sieve for pressure swing adsorption |
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| CN101890332A true CN101890332A (en) | 2010-11-24 |
| CN101890332B CN101890332B (en) | 2012-07-18 |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103566898A (en) * | 2013-09-26 | 2014-02-12 | 蚌埠华纺滤材有限公司 | Modified straw wood charcoal adsorbent and preparation method thereof |
| CN107376835A (en) * | 2017-08-18 | 2017-11-24 | 洛阳建龙微纳新材料股份有限公司 | A kind of efficiently hydrogen manufacturing adsorbent and preparation method thereof |
| CN109126692A (en) * | 2018-09-14 | 2019-01-04 | 中国地质科学院郑州矿产综合利用研究所 | Preparation method of high-performance TC-5A molecular sieve adsorbent |
| CN111111609A (en) * | 2018-10-30 | 2020-05-08 | 中国石油化工股份有限公司 | 5A molecular sieve adsorbent and preparation method and application thereof |
| CN112191280A (en) * | 2020-12-10 | 2021-01-08 | 苏州立昂新材料有限公司 | Continuous crystal transformation and ion exchange device and process |
| CN114433016A (en) * | 2020-10-31 | 2022-05-06 | 中国石油化工股份有限公司 | High-efficiency 5A molecular sieve adsorbent and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0590947A1 (en) * | 1992-10-01 | 1994-04-06 | The Boc Group, Inc. | Purification of oxygen by adsorption |
| US20030172808A1 (en) * | 2000-07-07 | 2003-09-18 | Remi Le Bec | Method for purifying hydrogen-based gas mixtures using a calcium x- zeolite |
| CN1724141A (en) * | 2005-05-25 | 2006-01-25 | 太原理工大学 | Process for preparing adsorbent of molecular sieve with high adsorption value fluorite |
-
2010
- 2010-07-30 CN CN2010102416935A patent/CN101890332B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0590947A1 (en) * | 1992-10-01 | 1994-04-06 | The Boc Group, Inc. | Purification of oxygen by adsorption |
| US20030172808A1 (en) * | 2000-07-07 | 2003-09-18 | Remi Le Bec | Method for purifying hydrogen-based gas mixtures using a calcium x- zeolite |
| CN1724141A (en) * | 2005-05-25 | 2006-01-25 | 太原理工大学 | Process for preparing adsorbent of molecular sieve with high adsorption value fluorite |
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103566898A (en) * | 2013-09-26 | 2014-02-12 | 蚌埠华纺滤材有限公司 | Modified straw wood charcoal adsorbent and preparation method thereof |
| CN107376835A (en) * | 2017-08-18 | 2017-11-24 | 洛阳建龙微纳新材料股份有限公司 | A kind of efficiently hydrogen manufacturing adsorbent and preparation method thereof |
| CN107376835B (en) * | 2017-08-18 | 2020-12-01 | 洛阳建龙微纳新材料股份有限公司 | Efficient hydrogen production adsorbent and preparation method thereof |
| CN109126692A (en) * | 2018-09-14 | 2019-01-04 | 中国地质科学院郑州矿产综合利用研究所 | Preparation method of high-performance TC-5A molecular sieve adsorbent |
| CN109126692B (en) * | 2018-09-14 | 2021-05-04 | 中国地质科学院郑州矿产综合利用研究所 | Preparation method of high-performance TC-5A molecular sieve adsorbent |
| CN111111609A (en) * | 2018-10-30 | 2020-05-08 | 中国石油化工股份有限公司 | 5A molecular sieve adsorbent and preparation method and application thereof |
| CN111111609B (en) * | 2018-10-30 | 2022-02-22 | 中国石油化工股份有限公司 | 5A molecular sieve adsorbent and preparation method and application thereof |
| CN114433016A (en) * | 2020-10-31 | 2022-05-06 | 中国石油化工股份有限公司 | High-efficiency 5A molecular sieve adsorbent and preparation method thereof |
| CN114433016B (en) * | 2020-10-31 | 2023-07-28 | 中国石油化工股份有限公司 | 5A molecular sieve adsorbent and preparation method thereof |
| CN112191280A (en) * | 2020-12-10 | 2021-01-08 | 苏州立昂新材料有限公司 | Continuous crystal transformation and ion exchange device and process |
| WO2022121223A1 (en) * | 2020-12-10 | 2022-06-16 | 苏州立昂新材料有限公司 | Continuous crystal transformation and ion exchange device and process |
| US11845073B1 (en) | 2020-12-10 | 2023-12-19 | Catlion Co., Ltd. | Continuous crystal transformation and ion exchange device and process |
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| Publication number | Publication date |
|---|---|
| CN101890332B (en) | 2012-07-18 |
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