CN101406844A - Method for preparing molecular sieve supported nano zinc sulphide - Google Patents
Method for preparing molecular sieve supported nano zinc sulphide Download PDFInfo
- Publication number
- CN101406844A CN101406844A CNA2008102192640A CN200810219264A CN101406844A CN 101406844 A CN101406844 A CN 101406844A CN A2008102192640 A CNA2008102192640 A CN A2008102192640A CN 200810219264 A CN200810219264 A CN 200810219264A CN 101406844 A CN101406844 A CN 101406844A
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- China
- Prior art keywords
- molecular sieve
- hours
- aqueous solution
- zinc
- supported nano
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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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- 239000002808 molecular sieve Substances 0.000 title claims abstract description 44
- 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 44
- 239000005083 Zinc sulfide Substances 0.000 title claims abstract description 28
- DRDVZXDWVBGGMH-UHFFFAOYSA-N zinc;sulfide Chemical compound [S-2].[Zn+2] DRDVZXDWVBGGMH-UHFFFAOYSA-N 0.000 title claims abstract description 21
- 238000000034 method Methods 0.000 title abstract description 10
- PTFCDOFLOPIGGS-UHFFFAOYSA-N Zinc dication Chemical compound [Zn+2] PTFCDOFLOPIGGS-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000001291 vacuum drying Methods 0.000 claims abstract description 15
- 239000007864 aqueous solution Substances 0.000 claims abstract description 13
- 239000000243 solution Substances 0.000 claims abstract description 13
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 27
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical class S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 claims description 9
- 238000005406 washing Methods 0.000 claims description 7
- 238000010521 absorption reaction Methods 0.000 claims description 5
- 238000002360 preparation method Methods 0.000 claims description 5
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 claims description 4
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 claims description 4
- 229960001763 zinc sulfate Drugs 0.000 claims description 4
- 229910000368 zinc sulfate Inorganic materials 0.000 claims description 4
- 238000001914 filtration Methods 0.000 claims description 2
- 235000005074 zinc chloride Nutrition 0.000 claims description 2
- 239000011592 zinc chloride Substances 0.000 claims description 2
- 229910052984 zinc sulfide Inorganic materials 0.000 abstract description 10
- 239000003054 catalyst Substances 0.000 abstract description 8
- 230000003197 catalytic effect Effects 0.000 abstract description 6
- 239000002245 particle Substances 0.000 abstract description 4
- 230000008929 regeneration Effects 0.000 abstract description 3
- 238000011069 regeneration method Methods 0.000 abstract description 3
- 238000011065 in-situ storage Methods 0.000 abstract description 2
- 238000011084 recovery Methods 0.000 abstract description 2
- ZNZNXSDPNKCWNO-UHFFFAOYSA-N S.CO Chemical class S.CO ZNZNXSDPNKCWNO-UHFFFAOYSA-N 0.000 abstract 2
- 238000001179 sorption measurement Methods 0.000 abstract 2
- 238000011175 product filtration Methods 0.000 description 5
- 206010013786 Dry skin Diseases 0.000 description 4
- 238000001035 drying Methods 0.000 description 4
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- 229910000679 solder Inorganic materials 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000007540 photo-reduction reaction Methods 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- UHOVQNZJYSORNB-UHFFFAOYSA-N benzene Substances C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000005695 dehalogenation reaction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 125000002485 formyl group Chemical class [H]C(*)=O 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000000243 photosynthetic effect Effects 0.000 description 1
- 238000006722 reduction reaction Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Catalysts (AREA)
Abstract
The invention discloses a method for preparing a molecular sieve loading nanometer zinc sulfide catalyst. The method is characterized by comprising the following steps: 1) a divalent zinc ion aqueous solution with the concentration of between 0.1 and 0.5 mol/L is prepared, and a molecular sieve is dipped in the aqueous solution for 3 hours, filtered and then vacuum-dried for 5 hours at 80 DEG C; 2) the molecular sieve adsorbing divalent zinc ions is dipped in a saturated hydrogen sulfide methanol solution for 5 hours; and 3) the molecular sieve treated by the saturated hydrogen sulfide methanol solution is filtered, washed and dried for 5 to 6 hours in a vacuum drying chamber at a temperature between 60 and 80 DEG C. The method utilizes the high adsorption property of the molecular sieve to adsorb the divalent zinc ions, and then in situ synthesizes nanometer zinc sulfide particles on the surface of the molecular sieve. The high adsorption property of the molecular sieve and large surface area greatly increase the catalytic activity of nanometer zinc sulfide. Meanwhile, catalyst products of the invention also have the characteristics of convenient and fast recovery and regeneration.
Description
Technical field
The present invention relates to a kind of method for preparing molecular sieve supported nano zinc sulphide, be specifically related to a kind of by molecular sieve as carrier, at molecular sieve surface synthesis of nano zinc sulphide, utilize the high surface of molecular sieve and a kind of method for preparing catalyst of nano-zinc sulfide catalytic performance.
Background technology
The nano-zinc sulfide photochemical catalyst can be used for the multiple aspects such as photo-reduction of degraded, water hydrogen manufacturing, carbon dioxide photo-reduction, organic photosynthetic one-tenth, halogeno-benzene dehalogenation, aldehyde and the derivative of organic pollution, at present existing several different methods can make the nano-zinc sulfide photochemical catalyst, as hydrothermal synthesis method, microwave process for synthesizing etc.But prepared nano-zinc sulfide is still waiting to improve aspect catalytic activity, and simultaneously, it reclaims and also is difficult to satisfactory with the regeneration aspect.
Summary of the invention
The object of the invention is to provide a kind of preparation method of molecular sieve supported nano zinc sulphide, to improve the catalytic activity of nano-zinc sulfide.
The preparation method of molecular sieve supported nano zinc sulphide of the present invention is characterized in that may further comprise the steps:
1) configuration concentration is the divalent zinc ion aqueous solution of 0.1～0.5mol/L, and molecular sieve be impregnated in this aqueous solution 3 hours, filters the back in 80 degrees centigrade of vacuum drying 5 hours;
2) molecular sieve of above-mentioned absorption divalent zinc ion be impregnated in the methanol solution of saturated hydrogen sulfide 5 hours;
3) the molecular sieve filtration washing that will handle through the methanol solution of saturated hydrogen sulfide, and in vacuum drying chamber under 60～80 degrees celsius dry 5～6 hours, promptly make molecular sieve supported nano zinc sulphide.
Preferred zinc chloride of the described divalent zinc ion aqueous solution or zinc sulfate.
Compared with prior art, the invention has the advantages that:
The present invention utilizes the high absorption property absorption divalent zinc ion of molecular sieve, then in molecular sieve surface in situ synthesis of nano zinc sulphide particles.In use the high absorption property of molecular sieve and big surface agent can increase the catalytic activity of nano-zinc sulfide greatly, and catalyst prod of the present invention also has conveniently characteristics aspect recovery and the regeneration simultaneously.
The specific embodiment
Below in conjunction with embodiment the present invention is described in further detail.
Embodiment 1:
1. configuration concentration is the solder(ing)acid of 0.2mol/L, and molecular sieve be impregnated in this aqueous solution 3 hours.Filter the back in 80 degrees centigrade of vacuum drying 5 hours.
2. the molecular sieve that will adsorb divalent zinc ion impregnated in the methanol solution of saturated hydrogen sulfide 5 hours.
3. with above product filtration washing and in vacuum drying chamber under 60～80 degrees celsius dry 6 hours, finally make molecular sieve supported nano zinc sulphide.
Embodiment 2:
1. configuration concentration is the zinc sulfate solution of 0.4mol/L, and molecular sieve be impregnated in this aqueous solution 3 hours.Filter the back in 80 degrees centigrade of vacuum drying 5 hours.
2. the molecular sieve that will adsorb divalent zinc ion impregnated in the methanol solution of saturated hydrogen sulfide 5 hours.
With above product filtration washing and in vacuum drying chamber 60～80 degrees centigrade of dryings 6 hours, finally make molecular sieve supported nano zinc sulphide.
Embodiment 3:
1. configuration concentration is the zinc sulfate solution of 0.1mol/L, and molecular sieve be impregnated in this aqueous solution 3 hours.Filter the back in 80 degrees centigrade of vacuum drying 5 hours.
2. the molecular sieve that will adsorb divalent zinc ion impregnated in the methanol solution of saturated hydrogen sulfide 5 hours.
With above product filtration washing and in vacuum drying chamber 60～80 degrees centigrade of dryings 6 hours, finally make molecular sieve supported nano zinc sulphide.
Embodiment 4:
1. configuration concentration is the solder(ing)acid of 0.5mol/L, and molecular sieve be impregnated in this aqueous solution 3 hours.Filter the back in 80 degrees centigrade of vacuum drying 5 hours.
2. the molecular sieve that will adsorb divalent zinc ion impregnated in the methanol solution of saturated hydrogen sulfide 5 hours.
With above product filtration washing and in vacuum drying chamber 60～80 degrees centigrade of dryings 6 hours, finally make molecular sieve supported nano zinc sulphide.
Embodiment 5:
1. configuration concentration is the solder(ing)acid of 0.3mol/L, and molecular sieve be impregnated in this aqueous solution 3 hours.Filter the back in 80 degrees centigrade of vacuum drying 5 hours.
2. the molecular sieve that will adsorb divalent zinc ion impregnated in the methanol solution of saturated hydrogen sulfide 5 hours.
With above product filtration washing and in vacuum drying chamber 60～80 degrees centigrade of dryings 6 hours, finally make molecular sieve supported nano zinc sulphide.
Above embodiment gained catalyst prod is observed through transmission electron microscope, and zinc sulphide particles evenly is arranged in the molecular sieve surface, and the zinc sulphide particles average grain diameter of each embodiment is between 21.2nm～29.5nm.
Above 5 embodiment gained catalyst are used for the formaldehyde reduction test, find to have improved more than 30% than the catalytic efficiency of existing method gained nano-zinc sulfide, high raising nearly 48%.
Claims (2)
1, a kind of preparation method of molecular sieve supported nano zinc sulphide is characterized in that may further comprise the steps:
1) configuration concentration is the divalent zinc ion aqueous solution of 0.1～0.5mol/L, and molecular sieve be impregnated in this aqueous solution 3 hours, filters the back in 80 degrees centigrade of vacuum drying 5 hours;
2) molecular sieve of above-mentioned absorption divalent zinc ion be impregnated in the methanol solution of saturated hydrogen sulfide 5 hours;
3) the molecular sieve filtration washing that will handle through the methanol solution of saturated hydrogen sulfide, and in vacuum drying chamber under 60～80 degrees celsius dry 5～6 hours, promptly make molecular sieve supported nano zinc sulphide.
2, the preparation method of molecular sieve supported nano zinc sulphide according to claim 1 is characterized in that the described divalent zinc ion aqueous solution is zinc chloride or zinc sulfate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2008102192640A CN101406844A (en) | 2008-11-20 | 2008-11-20 | Method for preparing molecular sieve supported nano zinc sulphide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2008102192640A CN101406844A (en) | 2008-11-20 | 2008-11-20 | Method for preparing molecular sieve supported nano zinc sulphide |
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| Publication Number | Publication Date |
|---|---|
| CN101406844A true CN101406844A (en) | 2009-04-15 |
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| CNA2008102192640A Pending CN101406844A (en) | 2008-11-20 | 2008-11-20 | Method for preparing molecular sieve supported nano zinc sulphide |
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| CN (1) | CN101406844A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103623772A (en) * | 2013-12-02 | 2014-03-12 | 上海交通大学 | Absorbent for removing and recovering liquid-phase mercury as well as preparation method and using method thereof |
| CN103623771A (en) * | 2013-12-02 | 2014-03-12 | 上海交通大学 | Waste solution mercury removal adsorbent, preparation method and application method thereof |
| CN105312066A (en) * | 2015-05-12 | 2016-02-10 | 山东科技大学 | Preparing method for zinc sulfide-montmorillonite nanometer composite material |
| CN107810974A (en) * | 2017-11-14 | 2018-03-20 | 江苏师范大学 | A kind of efficient compound air purifying preparation |
| CN115108883A (en) * | 2021-03-17 | 2022-09-27 | 山东泰和水处理科技股份有限公司 | Preparation method of benzyl chloride |
-
2008
- 2008-11-20 CN CNA2008102192640A patent/CN101406844A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103623772A (en) * | 2013-12-02 | 2014-03-12 | 上海交通大学 | Absorbent for removing and recovering liquid-phase mercury as well as preparation method and using method thereof |
| CN103623771A (en) * | 2013-12-02 | 2014-03-12 | 上海交通大学 | Waste solution mercury removal adsorbent, preparation method and application method thereof |
| CN103623771B (en) * | 2013-12-02 | 2016-02-10 | 上海交通大学 | A kind of waste liquid mercury-removing adsorbent and preparation method thereof and using method |
| CN103623772B (en) * | 2013-12-02 | 2016-04-06 | 上海交通大学 | A kind of adsorbent for removing and reclaim liquid phase mercury and preparation method thereof and using method |
| CN105312066A (en) * | 2015-05-12 | 2016-02-10 | 山东科技大学 | Preparing method for zinc sulfide-montmorillonite nanometer composite material |
| CN107810974A (en) * | 2017-11-14 | 2018-03-20 | 江苏师范大学 | A kind of efficient compound air purifying preparation |
| CN115108883A (en) * | 2021-03-17 | 2022-09-27 | 山东泰和水处理科技股份有限公司 | Preparation method of benzyl chloride |
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| Date | Code | Title | Description |
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| C06 | Publication | ||
| PB01 | Publication | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Open date: 20090415 |