CN101524638A - Preparation method of submicron molecular sieve carbon dioxide absorbent - Google Patents
Preparation method of submicron molecular sieve carbon dioxide absorbent Download PDFInfo
- Publication number
- CN101524638A CN101524638A CN200910082844A CN200910082844A CN101524638A CN 101524638 A CN101524638 A CN 101524638A CN 200910082844 A CN200910082844 A CN 200910082844A CN 200910082844 A CN200910082844 A CN 200910082844A CN 101524638 A CN101524638 A CN 101524638A
- Authority
- CN
- China
- Prior art keywords
- molecular sieve
- preparation
- potassium
- sodium
- solution
- Prior art date
- 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.)
- Granted
Links
Images
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/20—Air quality improvement or preservation, e.g. vehicle emission control or emission reduction by using catalytic converters
Abstract
The invention relates to a preparation method of submicron molecular sieve carbon dioxide absorbent, which is characterized by comprising preparing following steps: (1) potassium-containing composition is added to be used as a directing agent and 13X molecular sieve powder with law silica alumina ratio is added to be used as a seed crystal, thereby preparing sub-micron 13X molecular sieve of low silica alumina ratio; (2) sodium or calcium salt solution is used to carry out ion exchange on K cation of the 13X submicron molecular sieve prepared in step (1); (3) the treated molecular sieve processed by exchange treatment is moulded with an adhesive; and (4) the moulded molecular sieve absorbent is then dried and activated.
Description
Technical field
The present invention relates to the sieve technology field, relate to a kind of submicron molecular sieve preparation of adsorbent method that is used for removing carbon dioxide from gas (air).In particular, employing contains the K compound and prepares sub-micron low silica-alumina ratio adsorbent of molecular sieve as directed agents and method promotion nucleation rate that adds crystal seed and reduction product molecular sieve silica alumina ratio.
Background technology
Because carbon dioxide can freeze at low temperatures and generate hydrate with steam, so in many commercial gas were used, it was a kind of undesirable impurity.The generation of solid or solid particulate matter makes gas processing, operation, transportation and storage very difficult, even may.For example, in fact the cryogenic system that is used for air separation production oxygen and nitrogen need remove carbon dioxide (1ppm or lower) and water vapour from air fully before separating.The carbon dioxide that exists in the air-flow of oil plant to hydrogen contamination and the quantity of moisture have similar requirement.There were similar requirement in nitrogen gas purity and gas processing factory to synthesis ammonia plant to carbon dioxide content and gas dew point before ethane and helium recovery and/or natural gas liquefaction.In addition, petrochemical plant must be removed monomer: carbon dioxide and water in ethene, third rare, the butylene etc., poison and the polymer performance variation to prevent polymerization catalyst.Airborne nitrogen oxide or carbohydrate can solidify at low temperatures, and are deposited in heat exchanger and the destilling tower and may make its obstruction, are to produce blast so must take precautions against these parts in advance handling liquid oxygen.Therefore, with regard to security, when the purifying air, must remove wherein nitrogen oxide and carbohydrate, in order to avoid its aggegation is in liquid oxygen.
US3865924 (Gidaspow) discloses a kind of CO
2Adsorbent, it is the mechanical impurity of activated alumina and alkali metal hydrochlorate.US4433981 (Slaugh) but a kind of adsorbent of salt impregnated alumina preparation of decomposing with alkali metal oxide or alkaline earth oxide or roasting is disclosed.US4493715 (Hogan) discloses a kind of CO that removes from alkene
2Adsorbent, it is to load on alkali metal oxide on the activated alumina, hydroxide, nitrate, acetate etc.Also have many other patent disclosure high-adsorption-capacity arranged, particularly from gas, remove CO
2The adsorbent of molecular sieve that high-adsorption-capacity is arranged.For example, US2882244 (Milton) discloses and has been used for CO
2The various crystal aluminosilicates of absorption.US3078639 (Milton) discloses a kind of being used for from air stream CO absorption
2X type zeolite.BP 1508928 (Mobil Oil) and 1051621 (Furtig etc.) disclose silica than being the faujasite zeolitic of 1.8-2.2.US4557736 (Sircar) discloses a kind of adsorbent that contains the X type molecular sieve of binary ion-exchange, and it is used for being higher than under the normal pressure from air stream adsorption of nitrogen, so that the production oxygen enrichment is put into product stream.US5868818 (Ogawa) discloses a kind of at least 90% lithium cation SiO that contains
2/ Al
2O
3Mol ratio is used for adsorbed water steam and carbon dioxide less than 3.0 crystallization X type molecular sieve.US6143057 (Bulow) disclose a kind of from air the compound molecule sieve adsorbant of separating nitrogen or carbon dioxide, at least 90% for to be not more than about 0.6 micron feature particle in the wherein said compound molecule sieve adsorbant, and this compound molecule sieve adsorbant is very responsive to carbon dioxide and oxynitrides., mention and to remove N in early days openly in communique 2000-107546 number in the Japanese patent application case
2The adsorbent of O comprises calcium ion-exchanged X type zeolite, Na-Type Mordenit (Na Mordenite), barium ions exchanging zeolite, no adhesive (binderless) calcium ion-exchanged zeolite or the like.In addition, the Japanese patent application case discloses communique in early days and discloses a kind of airborne N that removes for 2000-140550 number
2The device of O, it uses faujasite (faujasite) to adsorb N
2O.Though these products all have been used for from gas stream adsorbed water, CO
2And N
2O, but the adsorbent that is improved remains important.
Summary of the invention
The present invention is a submicron molecular sieve preparation of adsorbent method, and it is a kind of to water and CO that purpose is to provide
2Adsorbent of molecular sieve than high-adsorption-capacity is arranged.It is to adopt to contain the K compound and prepare sub-micron low silica-alumina ratio 13X molecular sieve as directed agents and the method that adds crystal seed, then with sub-micron low silica-alumina ratio 13X molecular sieve and certain density sodium or the calcium salt soln of containing, carry out the ion dynamic exchange at a certain temperature, thereby reach made adsorbent of molecular sieve improves adsorbance to water and carbon dioxide purpose.
The present invention is a kind of preparation method of submicron molecular sieve carbon dioxide absorbent, it is characterized in that:
Preparation technology may further comprise the steps:
(1) add potassium-containing compound and do crystal seed as the small quantities of powder of directed agents and low silica-alumina ratio 13X molecular sieve, the crystal seed addition is the Al that feeds intake
2O
31%~10% of quality; Prepare sub-micron low silica-alumina ratio 13X molecular sieve.
(2) utilize sodium or calcium salt soln that the K cation of the sub-micron low silica-alumina ratio Na/K type 13X molecular sieve of step (1) preparation is carried out ion-exchange; Described sodium salt solution is selected from sodium chloride solution, sodium hydroxide solution, sodium nitrate solution, sodium carbonate liquor, metabisulfite solution, sodium bicarbonate solution, SAS; Calcium salt soln is selected from calcium chloride solution; The concentration of described sodium salt or calcium salt exchange solution is 1mol/L~5mol/L; Ion-exchange temperature is 50 ℃~90 ℃; Be 1h~5h described swap time.
(3) molecular sieve and binding agent moulding after exchange is handled;
(4) adsorbent of molecular sieve of drying and the moulding of activation institute, gained synthesis of molecular sieve crystalline size is 0.2~0.6 μ m.
According to submicron molecular sieve preparation of adsorbent method of the present invention, it is characterized in that in the described step of preparation process (1): potassium-containing compound is selected from any one or a few mixture of potassium hydroxide, potassium chloride, potash, potassium sulfate, potassium acetate, potassium nitrate; The potassium-containing compound addition is K
2O/Al
2O
3Mol ratio is 1~10;
According to submicron molecular sieve preparation of adsorbent method of the present invention, it is characterized in that in the described step of preparation process (1): add low silica-alumina ratio 13X molecular sieve powder and do crystal seed, the crystal seed addition is the Al that feeds intake
2O
32%~5% of mass range.
According to submicron molecular sieve preparation of adsorbent method of the present invention, it is characterized in that the concentration of middle sodium salt of described step of preparation process (2) or calcium salt exchange solution is 3mol/L~5mol/L; Ion-exchange temperature is 60 ℃~80 ℃; Be 2h~4h described swap time.
According to submicron molecular sieve preparation of adsorbent method of the present invention, it is characterized in that in the described step of preparation process (1): potassium-containing compound addition K
2O/Al
2O
3Mol ratio is 1.5~5.
According to submicron molecular sieve preparation of adsorbent method of the present invention, it is characterized in that binding agent is selected from bentonite in the described step of preparation process (3), cover holder soil, kaolin, attapulgite; Addition is 10%~50%.
The method that sub-micron ultralow silica alumina ratio 13X adsorbent of molecular sieve that the present invention is prepared and product carry out modification has the following advantages:
1, the present invention adopts and contains the method for K compound as directed agents and adding crystal seed, synthesizes sub-micron low silica-alumina ratio 13X molecular sieve, and zeolite crystal is of a size of 0.2~0.6 μ m, and silica alumina ratio is 2.0~2.2.
2, sub-micron low silica-alumina ratio 13X molecular sieve of the present invention, through containing sodium or calcium salt soln ion-exchange, reduce K ion concentration in the molecular sieve, the present invention is minimum can be reduced to 0.45%~1.0% with the K ion concentration, significantly improves the absorption property of adsorbent of molecular sieve to water and carbon dioxide.
3, sub-micron low silica-alumina ratio adsorbent of molecular sieve of the present invention adsorbed 7.5~12.5 hours at normal temperatures, and water and carbon dioxide are still had absorption preferably.
Description of drawings
Fig. 1 is the X ray diffracting spectrum of the synthetic 13X molecular sieve of the present invention.
Fig. 2 is for adding the SEM sem photograph of the synthetic 13X molecular sieve of KOH.
Fig. 3 is the adsorption effect comparison diagram of the adsorbent of molecular sieve of preparation to carbon dioxide, wherein:
-■-embodiment 8 (NaLSX-0.50K
+)
-●-embodiment 9 (NaLSX-0.45K
+)
The embodiment of-▲-10 (Na/KLSX-1.0K
+)
The specific embodiment
Further describe feature of the present invention below by example, but the present invention is not limited to following example.
Embodiment 1
636.96g NaOH and 420.43g potassium hydroxide are added in the 5L sodium aluminate solution, so that OH
-/ SiO
2Mol ratio is 2.34, K
2O/Al
2O
3Mol ratio is 1.5, this solution is mixed with 4.125L water glass solution and stream, so that make SiO
2/ Al
2O
3Mol ratio is 2.0, wherein H
2O/Na
2The O mol ratio is 20, and the crystal seed addition is Al
2O
33% of quality, with the aging 30min of the gel mixture stirring at room that makes, then 70 ℃ of following static burn ins 6 hours, 100 ℃ of following static crystallizations 3 hours.After crystallization finishes, the rapid water cooling of crystal that generates is filtered, spend deionised water and drop to 9 to the pH value, filter cake is 80 ℃ of oven dry down.
Assay products, measuring the product crystal phase structure through X-ray diffraction is pure phase 13X molecular sieve, selects industrial 13X sieve sample as standard sample, and degree of crystallinity is set at 100%, and the product relative crystallinity is 97%.BET specific area with low temperature nitrogen absorption Instrument measuring product is 659.36m2/g, and the crystallite dimension of assay products is 0.4~0.5 μ m under electron microscope.Silica and alumina molar ratio through the x-ray fluorescence analysis product are 2.0, K
2O content 15.3%.
Embodiment 2
926.76g NaOH and 558.75g potassium chloride are added in the 5L sodium aluminate solution, so that OH
-/ SiO
2Mol ratio is 2.32, K
2O/Al
2O
3Mol ratio is 1.5, this solution is mixed with 4.125L water glass solution and stream, so that make SiO
2/ Al
2O
3Mol ratio is 2.0, wherein H
2O/Na
2The O mol ratio is 20, and the crystal seed addition is Al
2O
33% of quality, with the aging 30min of the gel mixture stirring at room that makes, then 70 ℃ of following static burn ins 6 hours, 100 ℃ of following static crystallizations 3 hours.After crystallization finishes, the rapid water cooling of crystal that generates is filtered, spend deionised water and drop to 9 to the pH value, filter cake is 80 ℃ of oven dry down.
Assay products, measuring the product crystal phase structure through X-ray diffraction is pure phase 13X molecular sieve, selects industrial 13X sieve sample as standard sample, and degree of crystallinity is set at 100%, and the product relative crystallinity is 93%.BET specific area with low temperature nitrogen absorption Instrument measuring product is 589.76m2/g, and the crystallite dimension of assay products is 0.7~1.2 μ m under electron microscope.Silica and alumina molar ratio through the x-ray fluorescence analysis product are 2.0, K
2O content 16.1%.
Embodiment 3
926.76g NaOH and 517.52g potash are added in the 5L sodium aluminate solution, so that OH
-/ SiO
2Mol ratio is 2.32, K
2O/Al
2O
3Mol ratio is 1.5, this solution is mixed with 4.125L water glass solution and stream, so that make SiO
2/ Al
2O
3Mol ratio is 2.0, wherein H
2O/Na
2The O mol ratio is 20, and the crystal seed addition is Al
2O
33% of quality, with the aging 30min of the gel mixture stirring at room that makes, then 70 ℃ of following static burn ins 6 hours, 100 ℃ of following static crystallizations 3 hours.After crystallization finishes, the rapid water cooling of crystal that generates is filtered, spend deionised water and drop to 9 to the pH value, filter cake is 80 ℃ of oven dry down.
Assay products, measuring the product crystal phase structure through X-ray diffraction is pure phase 13X molecular sieve, selects industrial 13X sieve sample as standard sample, and degree of crystallinity is set at 100%, and the product relative crystallinity is 86%.BET specific area with low temperature nitrogen absorption Instrument measuring product is 494.48m2/g, and the crystallite dimension of assay products is about 1 μ m under electron microscope.Silica and alumina molar ratio through the x-ray fluorescence analysis product are 2.0, K
2O content 15.5%.
Embodiment 4
926.76g NaOH and 652.5g potassium sulfate are added in the 5L sodium aluminate solution, so that OH
-/ SiO
2Mol ratio is 2.32, K
2O/Al
2O
3Mol ratio is 1.5, this solution is mixed with 4.125L water glass solution and stream, so that make SiO
2/ Al
2O
3Mol ratio is 2.0, wherein H
2O/Na
2The O mol ratio is 20, and the crystal seed addition is Al
2O
33% of quality, with the aging 30min of the gel mixture stirring at room that makes, then 70 ℃ of following static burn ins 6 hours, 100 ℃ of following static crystallizations 3 hours.After crystallization finishes, the rapid water cooling of crystal that generates is filtered, spend deionised water and drop to 9 to the pH value, filter cake is 80 ℃ of oven dry down.
Assay products, measuring the product crystal phase structure through X-ray diffraction is pure phase 13X molecular sieve, selects industrial 13X sieve sample as standard sample, and degree of crystallinity is set at 100%, and the product relative crystallinity is 89%.BET specific area with low temperature nitrogen absorption Instrument measuring product is 522.73m2/g, and the crystallite dimension of assay products is 0.8~1 μ m under electron microscope.Silica and alumina molar ratio through the x-ray fluorescence analysis product are 2.0, K
2O content 17.3%.
Embodiment 5
926.76g NaOH and 755.9g potassium nitrate are added in the 5L sodium aluminate solution, so that OH
-/ SiO
2Mol ratio is 2.32, K
2O/Al
2O
3Mol ratio is 1.5, this solution is mixed with 4.125L water glass solution and stream, so that make SiO
2/ Al
2The O mol ratio is 2.0, wherein H
2O/Na
2The O mol ratio is 20, and the crystal seed addition is Al
2O
33% of quality, with the aging 30min of the gel mixture stirring at room that makes, then 70 ℃ of following static burn ins 6 hours, 100 ℃ of following static crystallizations 3 hours.After crystallization finishes, the rapid water cooling of crystal that generates is filtered, spend deionised water and drop to 9 to the pH value, filter cake is 80 ℃ of oven dry down.
Assay products, measuring the product crystal phase structure through X-ray diffraction is pure phase 13X molecular sieve, selects industrial 13X sieve sample as standard sample, and degree of crystallinity is set at 100%, and product phase relative crystallinity is 92%.BET specific area with low temperature nitrogen absorption Instrument measuring product is 563.22m2/g, and the crystallite dimension of assay products is about 1 μ m under electron microscope.Silica and alumina molar ratio through the x-ray fluorescence analysis product are 2.0, K
2O content 15.9%.
Embodiment 6
926.76g NaOH and 750.83g potassium acetate are added in the 5L sodium aluminate solution, so that OH
-/ SiO
2Mol ratio is 2.32, K
2O/Al
2O
3Mol ratio is 1.5, this solution is mixed with 4.125L water glass solution and stream, so that make SiO
2/ Al
2O
3Mol ratio is 2.0, wherein H
2O/Na
2The O mol ratio is 20, and the crystal seed addition is Al
2O
33% of quality, with the aging 30min of the gel mixture stirring at room that makes, then 70 ℃ of following static burn ins 6 hours, 100 ℃ of following static crystallizations 3 hours.After crystallization finishes, the rapid water cooling of crystal that generates is filtered, spend deionised water and drop to 9 to the pH value, filter cake is 80 ℃ of oven dry down.
Assay products, measuring the product crystal phase structure through X-ray diffraction is pure phase 13X molecular sieve, selects industrial 13X sieve sample as standard sample, and degree of crystallinity is set at 100%, and the product relative crystallinity is 90%.BET specific area with low temperature nitrogen absorption Instrument measuring product is 509.74m
2/ g, the crystallite dimension of assay products is 0.7~1 μ m under electron microscope.Silica and alumina molar ratio through the x-ray fluorescence analysis product are 2.0, K
2O content 16.3%.
Embodiment 7
Repeat the synthetic step of the embodiment 1 relevant ultralow silica alumina ratio 13X of sub-micron molecular sieve, different is that raising crystal seed addition is increased to the crystal seed addition and is the Al that feeds intake
2O
35% of quality.The relative crystallinity that the generation product is analyzed the 13X molecular sieve with X-ray diffraction is 99%.The BET specific area of low temperature nitrogen absorption Instrument measuring product is 665.28m
2/ g, the crystallite dimension of assay products is 0.2~0.5 μ m under electron microscope, is 2.02 through the silica and the alumina molar ratio of x-ray fluorescence analysis product, K
2O content 14.8%.
Embodiment 8
1.7 kilograms of sodium/potassium type sub-micron low silica-alumina ratio 13X molecular sieve powder that embodiment 1 is obtained is with 8 liters of 4mol/L sodium chloride solutions, and under 60 ℃, dynamically heat treatment is 2 hours.With 10 liters of deionized water washed product, filter cake is 100 ℃ of oven dry down, and the x-ray fluorescence analysis element that generates product is formed, and shows residual K
2O content is 1.56%.With 6 liters of 5mol/L sodium chloride solutions, under 60 ℃, dynamically heat treatment is 2 hours with 1.6 kilograms of molecular sieve powder after handling.With 10 liters of deionized water washed product, filter cake is 100 ℃ of oven dry down, and the x-ray fluorescence analysis element of exchange product is formed, and shows residual K
2O content is 0.5%.
Embodiment 9
1.7 kilograms of sodium/potassium type sub-micron low silica-alumina ratio 13X molecular sieve powder sample that embodiment 7 is obtained, molecular sieve powder with embodiment 7 preparations with sodium chloride solution is described in embodiment 8 exchanges 2 times, and exchange product X-ray fluorescence analysis element is formed the result and shown residual K
2O content is 0.45%.
Embodiment 10
1.7 kilograms of sodium/potassium type sub-micron low silica-alumina ratio 13X molecular sieve powder sample that embodiment 2 is obtained, with molecular sieve powder ion-exchange 2 times, exchange product X-ray fluorescence analysis element is formed the result and is shown residual K with sodium hydroxide solution is described in embodiment 8
2O content is 1.0%.
Embodiment 11
1.7 kilograms of sodium/potassium type sub-micron low silica-alumina ratio 13X molecular sieve powder sample that embodiment 3 is obtained, with molecular sieve powder ion-exchange 2 times, exchange product X-ray fluorescence analysis element is formed the result and is shown residual K with SAS is described in embodiment 8
2O content is 1.1%.
Embodiment 12
1.7 kilograms of sodium/potassium type sub-micron low silica-alumina ratio 13X molecular sieve powder sample that embodiment 4 is obtained, with molecular sieve powder ion-exchange 2 times, exchange product X-ray fluorescence analysis element is formed the result and is shown residual K with sodium nitrate solution is described in embodiment 8
2O content is 1.3%.
Embodiment 13
1.7 kilograms of sodium/potassium type sub-micron low silica-alumina ratio 13X molecular sieve powder sample that embodiment 5 is obtained, with molecular sieve powder ion-exchange 2 times, exchange product X-ray fluorescence analysis element is formed the result and is shown residual K with metabisulfite solution is described in embodiment 8
2O content is 1.2%.
Embodiment 14
1.7 kilograms of sodium/potassium type sub-micron low silica-alumina ratio 13X molecular sieve powder sample that embodiment 6 is obtained, with molecular sieve powder ion-exchange 2 times, exchange product X-ray fluorescence analysis element is formed the result and is shown residual K with calcium chloride solution is described in embodiment 8
2O content is 1.7%.
Embodiment 15
1000g 13X molecular sieve and 252g attapulgite with embodiment 8, embodiment 9, embodiment 10 and embodiment 14 gained mixes respectively, through the extruding slivering, oven dry, roasting is 4 hours in 550 ℃ of Muffle furnaces, activates 3 hours under the blanket of nitrogen condition then in adsorptive reactor.Use the tubular type absorber at the adsorbent of molecular sieve of 20 ℃ of following test implementation examples 8, embodiment 9, embodiment 10 and embodiment 14 preparations to water and CO
2Dynamic absorption.By adsorbent equipment, suppose the critical adsorption point: water is 1ppm to compressed air, CO with linear speed 0.1 meter per second
2Be 1ppm.The present invention is with CO
2Time before the appearance critical point is decided the adsorption time of adsorbent of molecular sieve.Test specimen to CO
2Dynamically adsorpting data is as shown in table 1.
Table 1, test specimen to CO
2Dynamic adsorpting data
Embodiment | Crystalline size (μ m) | Potassium content (%) | CO in the air of absorption back 2Content (ppm) | Adsorption time (h) |
8 | 0.4~0.6 | 0.50 | 0.5~0.9 | 12 |
9 | 0.2~0.5 | 0.45 | 0.3~0.8 | 12.5 |
10 | 0.7~1.2 | 1.0 | 0.7~1 | 8.5 |
14 | 0.7~1 | 1.7 | 0.7~1 | 7.5 |
Claims (6)
1, a kind of preparation method of submicron molecular sieve carbon dioxide absorbent is characterized in that:
Preparation technology may further comprise the steps:
(1) add potassium-containing compound and do crystal seed as the small quantities of powder of directed agents and low silica-alumina ratio 13X molecular sieve, the crystal seed addition is the Al that feeds intake
2O
31%~10% of quality; Prepare sub-micron low silica-alumina ratio 13X molecular sieve.
(2) utilize sodium or calcium salt soln that the K cation of the sub-micron low silica-alumina ratio Na/K type 13X molecular sieve of step (1) preparation is carried out ion-exchange; Described sodium salt solution is selected from sodium chloride solution, sodium hydroxide solution, sodium nitrate solution, sodium carbonate liquor, metabisulfite solution, sodium bicarbonate solution, SAS; Calcium salt soln is selected from calcium chloride solution; The concentration of described sodium salt or calcium salt exchange solution is 1mol/L~5mol/L; Ion-exchange temperature is 50 ℃~90 ℃; Be 1h~5h described swap time.
(3) molecular sieve and binding agent moulding after exchange is handled;
(4) adsorbent of molecular sieve of drying and the moulding of activation institute, gained synthesis of molecular sieve crystalline size is 0.2~0.6 μ m.
2, submicron molecular sieve preparation of adsorbent method according to claim 1 is characterized in that in the described step of preparation process (1): potassium-containing compound is selected from any one or a few mixture of potassium hydroxide, potassium chloride, potash, potassium sulfate, potassium acetate, potassium nitrate; The potassium-containing compound addition is K
2O/Al
2O
3Mol ratio is 1~10.
3, submicron molecular sieve preparation of adsorbent method according to claim 1 is characterized in that in the described step of preparation process (1): add low silica-alumina ratio 13X molecular sieve powder and do crystal seed, the crystal seed addition is the Al that feeds intake
2O
32%~5% of mass range.
4, submicron molecular sieve preparation of adsorbent method according to claim 1 is characterized in that the concentration of middle sodium salt of described step of preparation process (2) or calcium salt exchange solution is 3mol/L~5mol/L; Ion-exchange temperature is 60 ℃~80 ℃; Be 2h~4h described swap time.
5, submicron molecular sieve preparation of adsorbent method according to claim 2 is characterized in that in the described step of preparation process (1): potassium-containing compound addition K
2O/Al
2O
3Mol ratio is 1.5~5.
6, submicron molecular sieve preparation of adsorbent method according to claim 1 is characterized in that binding agent is selected from bentonite in the described step of preparation process (3), covers holder soil, kaolin, attapulgite; Addition is 10%~50%.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN2009100828444A CN101524638B (en) | 2009-04-23 | 2009-04-23 | Preparation method of submicron molecular sieve carbon dioxide absorbent |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN2009100828444A CN101524638B (en) | 2009-04-23 | 2009-04-23 | Preparation method of submicron molecular sieve carbon dioxide absorbent |
Publications (2)
Publication Number | Publication Date |
---|---|
CN101524638A true CN101524638A (en) | 2009-09-09 |
CN101524638B CN101524638B (en) | 2010-12-08 |
Family
ID=41092798
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN2009100828444A Active CN101524638B (en) | 2009-04-23 | 2009-04-23 | Preparation method of submicron molecular sieve carbon dioxide absorbent |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN101524638B (en) |
Cited By (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102120588A (en) * | 2011-01-17 | 2011-07-13 | 内蒙古大学 | Method for absorbing and fixing carbon dioxide through mineral carbonization |
CN101708456B (en) * | 2009-11-23 | 2013-03-06 | 洛阳市建龙化工有限公司 | Molecular sieve adsorbent for separating oxygen from air by means of pressure swing adsorption and preparation method thereof |
CN103495378A (en) * | 2013-09-27 | 2014-01-08 | 上海绿强新材料有限公司 | Olefin purification adsorbent and method thereof for olefin purification technology |
CN106804555A (en) * | 2017-01-20 | 2017-06-09 | 唐成康 | Application and its method of modifying of the metal ion-modified zeolite molecular sieve in mosquito is caught |
CN111392743A (en) * | 2020-05-13 | 2020-07-10 | 西安交通大学 | Preparation method of low-silica-alumina-ratio faujasite molecular sieve |
CN112675811A (en) * | 2020-12-18 | 2021-04-20 | 太原理工大学 | High-efficiency separation N2O/CO2Silver exchange molecular sieve adsorbent and preparation method thereof |
CN113828274A (en) * | 2021-10-08 | 2021-12-24 | 中国地质科学院郑州矿产综合利用研究所 | Preparation method of BaSrNaLSX for adsorbing carbon dioxide under low pressure |
-
2009
- 2009-04-23 CN CN2009100828444A patent/CN101524638B/en active Active
Cited By (11)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101708456B (en) * | 2009-11-23 | 2013-03-06 | 洛阳市建龙化工有限公司 | Molecular sieve adsorbent for separating oxygen from air by means of pressure swing adsorption and preparation method thereof |
CN102120588A (en) * | 2011-01-17 | 2011-07-13 | 内蒙古大学 | Method for absorbing and fixing carbon dioxide through mineral carbonization |
CN102120588B (en) * | 2011-01-17 | 2013-08-14 | 内蒙古大学 | Method for absorbing and fixing carbon dioxide through mineral carbonization |
CN103495378A (en) * | 2013-09-27 | 2014-01-08 | 上海绿强新材料有限公司 | Olefin purification adsorbent and method thereof for olefin purification technology |
CN103495378B (en) * | 2013-09-27 | 2015-08-05 | 上海绿强新材料有限公司 | A kind of alkene purifying adsorbent and the method for alkene process for purifying thereof |
CN106804555A (en) * | 2017-01-20 | 2017-06-09 | 唐成康 | Application and its method of modifying of the metal ion-modified zeolite molecular sieve in mosquito is caught |
CN111392743A (en) * | 2020-05-13 | 2020-07-10 | 西安交通大学 | Preparation method of low-silica-alumina-ratio faujasite molecular sieve |
CN111392743B (en) * | 2020-05-13 | 2021-10-19 | 西安交通大学 | Preparation method of low-silica-alumina-ratio faujasite molecular sieve |
CN112675811A (en) * | 2020-12-18 | 2021-04-20 | 太原理工大学 | High-efficiency separation N2O/CO2Silver exchange molecular sieve adsorbent and preparation method thereof |
CN113828274A (en) * | 2021-10-08 | 2021-12-24 | 中国地质科学院郑州矿产综合利用研究所 | Preparation method of BaSrNaLSX for adsorbing carbon dioxide under low pressure |
CN113828274B (en) * | 2021-10-08 | 2023-12-08 | 中国地质科学院郑州矿产综合利用研究所 | BaSrNaLSX preparation method for adsorbing carbon dioxide under low pressure |
Also Published As
Publication number | Publication date |
---|---|
CN101524638B (en) | 2010-12-08 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN101524638B (en) | Preparation method of submicron molecular sieve carbon dioxide absorbent | |
AU608018B2 (en) | Process for separating nitrogen from mixtures thereof with less polar substances | |
CN101489648B (en) | Process and zeolitic materials for the separation of gases | |
CA2085180C (en) | Nitrogen adsorption with a ca and/or sr exchanged lithium x-zeolite | |
US6464756B1 (en) | Purification of hydrogen flowstreams by selectively adsorbing impurities therefrom | |
JP5375890B2 (en) | Carbon dioxide adsorption separation method | |
US3431219A (en) | Crystalline galliosilicates | |
JP3776813B2 (en) | Argon / oxygen selective X zeolite | |
EP2368849A1 (en) | Chabazite-type zeolite and process for production of same | |
US7608134B1 (en) | Decarbonating gas streams using zeolite adsorbents | |
CN111039303B (en) | Application of modified M-SAPO-RHO type zeolite molecular sieve as ethylene selective adsorbent | |
JP2002154821A (en) | Apparatus and method for purifying gas | |
CA2013530A1 (en) | Process for the purification of bulk gases using chabazite adsorbents | |
EP1184338A1 (en) | Production of X Zeolites | |
CA2148893A1 (en) | Li-exchanged low silica emt-containing metallosilicates | |
US3078638A (en) | Carbon dioxide removal from vapor mixtures | |
US6878657B2 (en) | Process for the preparation of a molecular sieve adsorbent for the size/shape selective separation of air | |
TWI797384B (en) | Rho zeolites and method of making the same | |
US3078636A (en) | Unsaturated hydrocarbon separation | |
EP3466879A1 (en) | Chabazite zeolite with high hydrothermal resistance and method for producing same | |
JP2950476B2 (en) | Zinc aluminosilicate | |
CN102307645B (en) | Method for selectively isolating hydrogen or helium using a natrolite-based zeolite and novel natrolite-based zeolite | |
CN110510630B (en) | Nanoscale X molecular sieve grain spherical self-assembly substance and preparation method thereof | |
JP2001347123A (en) | Adsorptive separation method for carbon dioxide | |
JP2000140549A (en) | Removal of carbon dioxide |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
C06 | Publication | ||
PB01 | Publication | ||
C10 | Entry into substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
C14 | Grant of patent or utility model | ||
GR01 | Patent grant |