CN102188958A - Novel preparation method of silicon oxide adsorbing agent and application of silicon oxide adsorbing agent - Google Patents
Novel preparation method of silicon oxide adsorbing agent and application of silicon oxide adsorbing agent Download PDFInfo
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- CN102188958A CN102188958A CN2010190870418A CN201019087041A CN102188958A CN 102188958 A CN102188958 A CN 102188958A CN 2010190870418 A CN2010190870418 A CN 2010190870418A CN 201019087041 A CN201019087041 A CN 201019087041A CN 102188958 A CN102188958 A CN 102188958A
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- 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
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- 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
- Y02C—CAPTURE, STORAGE, SEQUESTRATION OR DISPOSAL OF GREENHOUSE GASES [GHG]
- Y02C20/00—Capture or disposal of greenhouse gases
- Y02C20/20—Capture or disposal of greenhouse gases of methane
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- 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
- Y02C—CAPTURE, STORAGE, SEQUESTRATION OR DISPOSAL OF GREENHOUSE GASES [GHG]
- Y02C20/00—Capture or disposal of greenhouse gases
- Y02C20/40—Capture or disposal of greenhouse gases of CO2
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Abstract
The invention discloses a novel preparation method of a silicon oxide adsorbing agent and application of the preparation method. The preparation method comprises the following steps of: carrying ABx on a surface of silicon oxide by using an immersion method, wherein A is the sodium (Na) element, the potassium (K) element, the calcium (Ca) element, the barium (Ba) element, the magnesium (Mg) element or the ferrum (Fe) element, B is the fluorine (F) element, the chlorine (Cl) element, the bromine (Br) or the iodine (I) element, and x is 1, 2 or 3; drying silica gel which is immersed with the ABx at the temperature of 80 to 160 DEG C; and putting a dried sample into a muffle furnace, and roasting at the temperature of 300 to 500 DEG C to prepare the novel silica gel adsorbing agent. The silica gel adsorbing agent has an excellent effect of removing carbon dioxide from methane gas, is simple in preparation and controllable in process.
Description
Technical field
The present invention relates to a kind of novel silica preparation of adsorbent method and application, be specifically related to a kind of rubbish landfill gas or other and contain the preparation of adsorbent method that removes carbon dioxide in the methane gas of carbon dioxide.
Background technology
Along with the continuous development of urbanization process, municipal refuse be treated as a problem demanding prompt solution.Current, the method that most countries generally adopts is a garbage loading embeading, the gas-phase product that anaerobic digestion produced in this process is become rubbish landfill gas (Landfill Gas, LFG), mainly containing methane and carbon dioxide forms, account for more than 95% of landfill gas cumulative volume, wherein methane accounts for 40～70%, and carbon dioxide accounts for 30～50%.Carbon dioxide and methane all are the important chemical raw materials for production, and methane still is a kind of biomass energy of high-quality, therefore, isolate the methane and the very important practical significance of carbon dioxide tool of high concentration from rubbish landfill gas.
Transformation adsorbing separation gaseous mixture has plurality of advantages such as energy consumption is low, technology is simple, automaticity is high, small investment, operating flexibility is big, environmental benefit is good and is widely studied and applied.Adsorbent is the emphasis of transformation absorption research as the core place of this technology always.Sorbing material commonly used is because many disadvantages all can not reach satisfied adsorbing separation effect.
Therefore, be even more important except that the adsorbent with high efficiency of additive capability just seems by modification exploitation to conventional sorbing material.
Summary of the invention
First technical problem that the present invention will solve provides a kind of novel, silica gel absorber efficiently.
Silica gel absorber of the present invention is to be loaded with AB at silicon oxide surface
X, wherein, A is Na, K, Ca, Ba, Mg or Fe element, and B is F, ClBr or I element, and x is 1,2 or 3, and described silica gel absorber is prepared as follows and obtains: described silica gel absorber is prepared as follows: with silica gel is carrier, with AB
XBeing precursor, is that solvent is made into maceration extract with the deionized water, and the mass ratio of described silica gel and A element is 1: 0.005～0.1, adopts infusion process with AB
XBe carried on described silica gel surface, will be impregnated with AB again
XSilica gel 80～160 ℃ of down oven dry, then the sample of drying is put into Muffle furnace 300～500 ℃ of roastings, be described novel silica gel adsorbent.
Second technical problem that the present invention will solve provides a kind of method for preparing above-mentioned silica gel absorber.
The technical solution used in the present invention is as follows:
A kind of preparation method of silica gel absorber comprises the steps:
A) by the AB of the saturated water adsorptive value of getting silica gel configuration certain volume
XMaceration extract dropwise adds maceration extract in the described silica gel, and silica gel is fully flooded; The mass ratio of the metal element A of described silica gel and load is 1: 0.005～0.1;
B) will be impregnated with AB
XSilica gel in air dry oven, be heated to 80～160 ℃, carry out drying and dewater;
C) Muffle furnace that dried sample is put under the air atmosphere under 300～500 ℃, further handle, making area load has AB
XSilica gel, be described silica gel absorber.
Below above-mentioned preparation method is done and specify.
In the step a), described dipping method is commonly used wet impregnation and incipient impregnation, the preferred equi-volume impregnating of the present invention.
In the step a), described dipping method, the suitable raising of dipping temperature, the growth of dip time help improving dipping efficient, carry out 4～12 hours under the preferred 20-60 of incipient impregnation of the present invention ℃.
In the step b), the AB that is impregnated with of the present invention
XThe drying of silica gel generally in air dry oven, carry out, described drying is recommended in carried out under 80～160 ℃ 12～24 hours.
In the step c), roasting of the present invention is recommended to carry out 3-5 hour under preferred 300～500 ℃.
The 3rd technical problem that the present invention will solve is with described AB
XThe modified silica-gel adsorbent is used as carbon dioxide absorber, isolates methane from the gaseous mixture of carbon dioxide and methane.
Metal-modified silica gel absorber of the present invention can at room temperature use, be applicable to very wide gaseous mixture scope, carbon dioxide content 30～60% all has excellent separating effect, is far superior to unmodified silica gel, is the high-efficiency adsorbent of a kind of effective separation of methane and carbon dioxide.
Compared with prior art, beneficial effect of the present invention is embodied in:
1) AB of the present invention
XThe remodeling silica gel absorber, with the silica gel of function admirable as carrier, at its area load inorganic metal salt.Because the factors such as electronic effect of metal A make that the silica gel after the load is further improved on many performances, outstanding shows: adsorption capacity is stronger, and is better to the selectivity of methane and carbon dioxide.As methane in the separating of garbage landfill gas and carbon dioxide the time, shown good effect with metal-modified silica gel absorber of the present invention.
2) AB of the present invention
XModified silica-gel preparation of adsorbent method is simple, realizes easily.Adopt equi-volume impregnating with AB
XDirectly load to the silica gel surface, removing redundant moisture and form with carrier silica gel surface and functional group by dry and roasting has the AB that pretends usefulness
XLoad layer is described silica gel absorber.Compare with additive method, this preparation method is simpler, and preparation process does not have the waste liquid generation.
Description of drawings
Fig. 1 is a used carrier silica gel low temperature nitrogen adsorption/desorption curve map of the present invention.
Fig. 2 is a used carrier silica gel graph of pore diameter distribution of the present invention.
Fig. 3 is the breakthrough curve of silica gel absorber of the present invention under rich He condition.
Fig. 4 is the breakthrough curve of Comparative Examples one described unmodified silica gel under rich He condition.
The specific embodiment
Below in conjunction with accompanying drawing the present invention is further described.
Na, K, Ca, Ba, Mg or Fe element, B are F, Cl Br or I
Take by weighing 0.3g K Cl and place beaker, add the 20ml deionized water and stirring and make its dissolving.Take by weighing 25g silica gel and place the magnetic crucible, will join maceration extract dropwise add in the crucible, do not stop to stir, all be impregnated in the silica gel until all maceration extracts.At normal temperatures, the absorption dipping is after 4 hours, and it is following dry 24 hours at 80 ℃ to put into air dry oven.The 300 ℃ of following roastings 3 hours in Muffle furnace of dried sample.Promptly obtaining area load has the silica gel absorber of K Cl.
Embodiment 2
Take by weighing 0.5g NaCl and place beaker, add the 20ml deionized water and stirring and make its dissolving.Take by weighing 25g silica gel and place the magnetic crucible, will join maceration extract dropwise add in the crucible, do not stop to stir, all be impregnated in the silica gel until all maceration extracts.At normal temperatures, the absorption dipping is after 4 hours, and it is following dry 15 hours at 100 ℃ to put into air dry oven.The 500 ℃ of following roastings 3 hours in Muffle furnace of dried sample.Promptly obtaining area load has the silica gel absorber of NaCl.
Embodiment 3
Take by weighing 0.5g CaCl
2Place beaker, add the 20ml deionized water and stirring and make its dissolving.Take by weighing 25g silica gel and place the magnetic crucible, will join maceration extract dropwise add in the crucible, do not stop to stir, all be impregnated in the silica gel until all maceration extracts.At normal temperatures, the absorption dipping is after 8 hours, and it is following dry 12 hours at 130 ℃ to put into air dry oven.The 400 ℃ of following roastings 3 hours in Muffle furnace of dried sample.Promptly obtain area load CaCl is arranged
2Silica gel absorber.
Embodiment 4
Take by weighing 0.4g MgCl
2Place beaker, add the 20ml deionized water and stirring and make its dissolving.Take by weighing 25g silica gel and place the magnetic crucible, will join maceration extract dropwise add in the crucible, do not stop to stir, all be impregnated in the silica gel until all maceration extracts.At normal temperatures, the absorption dipping is after 12 hours, and it is following dry 12 hours at 130 ℃ to put into air dry oven.The 400 ℃ of following roastings 5 hours in Muffle furnace of dried sample.Promptly obtain area load MgCl is arranged
2Silica gel absorber.
Embodiment 5
Take by weighing 0.45g BaCl
2Place beaker, add the 20ml deionized water and stirring and make its dissolving.Take by weighing 25g silica gel and place the magnetic crucible, will join maceration extract dropwise add in the crucible, do not stop to stir, all be impregnated in the silica gel until all maceration extracts.At normal temperatures, the absorption dipping is after 8 hours, and it is following dry 14 hours at 160 ℃ to put into air dry oven.The 500 ℃ of following roastings 3 hours in Muffle furnace of dried sample.Promptly obtain area load BaCl is arranged
2Silica gel absorber.
Embodiment 6
Take by weighing 0.8g FeCl
3Place beaker, add the 20ml deionized water and stirring and make its dissolving.Take by weighing 25g silica gel and place the magnetic crucible, will join maceration extract dropwise add in the crucible, do not stop to stir, all be impregnated in the silica gel until all maceration extracts.At normal temperatures, the absorption dipping is after 6 hours, and it is following dry 10 hours at 150 ℃ to put into air dry oven.The 450 ℃ of following roastings 5 hours in Muffle furnace of dried sample.Promptly obtain area load FeCl is arranged
3Silica gel absorber.
Fig. 1 is a used carrier silica gel low temperature nitrogen adsorption/desorption curve map of the present invention, Fig. 2 is a used carrier low temperature nitrogen adsorption/desorption curve map of the present invention, carrier has bigger specific area and more regular meso-hole structure as can be known, provides superior carrier environment to adsorbing.
The present invention places a kind of adsorbent bed of adsorbing separation evaluation system with Application Example, comparative example one, comparative example two said silica gel absorbers, feeds the gaseous mixture of methane and carbon dioxide under rich He condition, measures the adsorbance and the separation factor of adsorbent.
Adsorbing separation evaluation system of the present invention comprises adsorption separation device, gaseous mass spectrum, equipment such as gas-chromatography.Adsorbent bed is the stainless steel column structure, internal diameter 8mm, and wall thickness 2mm, length 480mm, adsorbent bed is connected by crossover sub with pipeline.
Application Example
Get the described area load of 20g MgCl is arranged
2Silica gel absorber, under rich He condition, mixed gas flow is 1ml/min, gaseous mixture consist of He: CO
2: CH
4=1: 1: 1,15 ℃ of adsorption temps, adsorptive pressure 0.5MPa.Find MgCl through adsorption test
2-silica gel absorber is to CH
4And CO
2Have good adsorptive selectivity, can access separating effect preferably, breakthrough curve is seen Fig. 3; While MgCl
2-silica gel absorber has bigger CO
2Adsorbance is a kind of efficient decarburization adsorbent that big application prospect is arranged.
Comparative example one
Get the unmodified silica gel of 20g and compare test, under rich He condition, mixed gas flow is 1ml/min, and gaseous mixture consists of He: CO
2: CH
4=1: 1: 1,15 ℃ of adsorption temps, adsorptive pressure 0.5MPa.Find that through adsorption test unmodified silica gel also has certain separating power to methane and carbon dioxide, breakthrough curve is seen Fig. 4.From the unit adsorbance of each sample of sorbent of table 1 and separation factor table as can be known, MgCl
2-silica gel absorber is compared with unmodified silica gel, its carbon dioxide adsorption obtain to a certain degree raising, and separating property is greatly improved.Therefore, MgCl
2-silica gel absorber is a kind of efficient decarburization adsorbent that big application prospect is arranged.
Comparative example two
Get 20g and use 1% CaCl
2Modified silica-gel compares test, and under rich He condition, mixed gas flow is 1ml/min, gaseous mixture consist of He: CO
2: CH
4=1: 1: 1,15 ℃ of adsorption temps, adsorptive pressure 0.5MPa.Find that through adsorption test adsorbent is to CO
2And CH
4Absorption property all have largely and to improve.
The unit adsorbance of each sample of sorbent of table 1 and separation factor table
| Adsorbent | ?CH 4Standard adsorbance (ml/g) | ?CO 2Standard adsorbance (ml/g) | Separation factor |
| Unmodified silica gel | 2.67 | 17.87 | 6.15 |
| MgCl 2-silica gel | 1.83 | 23.71 | 11.93 |
| CaCl 2-silica gel | 5.48 | 27.39 | 9.61 |
Annotate: separation factor
Wherein, x, y represent the mutually gentle phase mole fraction of certain component absorption respectively; N represents the adsorbance of certain component in absorption mutually; I, j represent to be present in gas phase and absorption component i and j mutually respectively; a
IjThe separation factor of expression component i and j.
Claims (10)
1. the silica gel absorber based on silica is characterized in that described adsorbent is to be loaded with AB at silicon oxide surface
X, wherein, A is Na, K, Ca, Ba, Mg or Fe element, and B is F, Cl Br or I element, and x is 1,2 or 3.
2. a method for preparing the described silica gel absorber of claim 1 is characterized in that with silica gel being carrier, with AB
XBeing precursor, is that solvent is made into maceration extract with the deionized water, and the mass ratio of described silica gel and A element is 1: 0.005～0.1, adopts infusion process with AB
XBe carried on described silica gel surface, will be impregnated with AB again
XSilica gel 80～160 ℃ of down oven dry, then the sample of drying is put into Muffle furnace 300～500 ℃ of roastings, be described novel silica gel adsorbent; Be specially following steps:
A) AB of configuration certain volume
XMaceration extract dropwise adds maceration extract in the silica gel, and silica gel is fully flooded;
B) will be impregnated with AB
XSilica gel in air dry oven, be heated to 80～160 ℃, carry out drying and dewater;
C) Muffle furnace that dried sample is put under the air atmosphere under 300～500 ℃, further handle, the area load that makes has AB
XSilica gel, be described silica gel absorber.
3. the preparation method of silica gel absorber as claimed in claim 2 is characterized in that the described silica gel specific area of step a) is greater than 500m
2/ g, average pore size 2～6nm.
4. the preparation method of silica gel absorber as claimed in claim 2 is characterized in that the described infusion process of step a) is an equi-volume impregnating, and promptly the maceration extract volume is the saturated water adsorptive value of carrier silica gel.
5. the preparation method of silica gel absorber as claimed in claim 2 is characterized in that the mass ratio of described infusion process silica gel of step a) and elements A is 1: 0.005～0.1.
6. as the preparation method of the described silica gel absorber of claim 2～4, it is characterized in that the described dipping of step a) is to carry out 4～12 hours under 20-60 ℃ of temperature.
7. the preparation method of silica gel absorber as claimed in claim 2 is characterized in that the dry used time of step b) is 12～24 hours.
8. the preparation method of silica gel absorber as claimed in claim 2 is characterized in that the described roasting time of step c) is 3～5 hours.
9. as the preparation method of claim 2 or 4 described silica gel absorbers, the unit mass saturated water adsorptive value that it is characterized in that the described silica gel of step a) is 0.65～0.85ml/g.
10. silica gel absorber as claimed in claim 1 contains the application of carbon dioxide absorber in the methane gas of carbon dioxide as rubbish landfill gas or other.
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| CN2010190870418A CN102188958A (en) | 2010-03-01 | 2010-03-01 | Novel preparation method of silicon oxide adsorbing agent and application of silicon oxide adsorbing agent |
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|---|---|---|---|
| CN2010190870418A CN102188958A (en) | 2010-03-01 | 2010-03-01 | Novel preparation method of silicon oxide adsorbing agent and application of silicon oxide adsorbing agent |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114192103A (en) * | 2021-11-15 | 2022-03-18 | 乳山市大洋硅胶有限公司 | Preparation method of ethane adsorption silica gel |
| CN118437280A (en) * | 2024-05-07 | 2024-08-06 | 上海樱琦干燥剂有限公司 | Composite drying agent and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1152017A (en) * | 1995-12-15 | 1997-06-18 | 深圳广宇工业(集团)公司 | Refrigerating adsorbent |
| WO2008133520A1 (en) * | 2007-05-01 | 2008-11-06 | Norit Nederland B.V. | Composite adsorbent material |
| CN101357321A (en) * | 2008-09-18 | 2009-02-04 | 上海交通大学 | Preparation method of silica gel composite absorbent |
-
2010
- 2010-03-01 CN CN2010190870418A patent/CN102188958A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1152017A (en) * | 1995-12-15 | 1997-06-18 | 深圳广宇工业(集团)公司 | Refrigerating adsorbent |
| WO2008133520A1 (en) * | 2007-05-01 | 2008-11-06 | Norit Nederland B.V. | Composite adsorbent material |
| CN101357321A (en) * | 2008-09-18 | 2009-02-04 | 上海交通大学 | Preparation method of silica gel composite absorbent |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114192103A (en) * | 2021-11-15 | 2022-03-18 | 乳山市大洋硅胶有限公司 | Preparation method of ethane adsorption silica gel |
| CN118437280A (en) * | 2024-05-07 | 2024-08-06 | 上海樱琦干燥剂有限公司 | Composite drying agent and preparation method thereof |
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Application publication date: 20110921 |