CN106732410B - A kind of preparation method of amino modified silicon substrate carbon dioxide absorber - Google Patents
A kind of preparation method of amino modified silicon substrate carbon dioxide absorber Download PDFInfo
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
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- B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
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- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/103—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate comprising silica
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/32—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating
- B01J20/3202—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating characterised by the carrier, support or substrate used for impregnation or coating
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- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/32—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating
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- Y02C20/40—Capture or disposal of greenhouse gases of CO2
Abstract
The invention discloses a kind of preparation methods of amino modified silicon substrate carbon dioxide absorber, including subcritical grafting is modified and ultrasonic immersing is modified two steps；Reaction dissolvent, amino-organosilanes are added in beaker, at the uniform velocity stir, add silicon substrate carrier, continue to stir at room temperature, mixture is transferred in autoclave, solid product is filtered after heat treatment, and is respectively rinsed twice with dehydrated alcohol and water, obtains organosilane-modified silica-base material after dry；Anhydrous methanol and organic amine modifying agent are added in beaker and at the uniform velocity stirred, add above-mentioned organosilane-modified silica-base material, continue to stir after being sealed with plastic film, then microwave oscillation, remove sealing film to continue to stir to methanol to volatilize to finish, obtains amino modified silicon substrate carbon dioxide absorber after dry.The carbon dioxide absorber carbon dioxide adsorption ability with higher prepared using this method, preferable absorption stability can more efficiently trap carbon dioxide.
Description
Technical field
The present invention relates to a kind of preparation methods of amino modified silicon substrate carbon dioxide absorber, belong to carbon dioxide adsorption
Agent preparation technical field.
Background technique
With the continuous growth of world population economy, world energy consumption is also quicklyd increase.The burning of fossil fuel generates
With give off a large amount of CO2Gas is the main reason for causing global warming, while CO2It is also a kind of potential carbon money
Source.Current tellurian resource growing tension, many countries are dedicated to CO2The research for capturing and sealing up for safekeeping and utilize, wherein from cigarette
Separation and collection CO in road gas2More and more it is concerned by people.Currently, CO2Trapping isolation technics has liquid solvent absorption process, inhales
Attached method, bioanalysis, membrane separation process and low-temperature freezing etc..Wherein method of reproduction is more mature and is answered for alkanolamine solution absorption-
With, such as in the industrial production, carbonated exhaust gas can be passed through alkanolamine solution, carbon dioxide be isolated, later appropriate
Place by heat hydramine carbon dioxide is discharged again.Alkanolamine solution absorbent has high thermal stability and high degradation resistant
The characteristics of property, but alkanolamine solution absorption and regeneration technology, there are at high cost, the expense of carbon dioxide separation process accounts about entire two
Aoxidize the 70% of carbon capture storage system (CCS).In addition, that there are equipment installations is perishable for hydramine solvent absorption regeneration techniques, absorb
The defects of agent regeneration energy consumption is big and the toxicity of absorbent itself.
Compared with liquid alkanolamine solution adsorbent, solid absorbent has cost of investment low, adsorbent reactivation energy consumption
Few feature.The equipment installation etching problem in liquid amine absorption process can also be effectively avoided simultaneously.Therefore, solid is utilized
Adsorbent carries out collecting carbonic anhydride, provides an energy conservation to reduce CO2 emission and recycling this potential carbon resource
Effective new way.Existing porosu solid adsorbent material includes clay, aluminium oxide, active carbon, Organometallic framework material, boiling
Stone, mesoporous silica-base material etc..Wherein silicon substrate porous material is cheaply easy because having specific surface area height, aperture controllable, synthesis material
The advantages that obtaining, it has also become scholars study focus of attention.But if silicon substrate porous material is only used only as solid absorption
Carbon dioxide is adsorbed in agent, because entire adsorption process relies primarily on the physical absorption in duct, the selectivity of adsorbent
It is all relatively low with adsorbance, greatly limit its industrial application.Therefore people make shape by carrying out the modifications of various modes to it
At silicon-based modifying composite material chemisorption is carried out while physical absorption, to improve carbon dioxide adsorption.Wherein
It is amino modified to the progress of silicon substrate porous material, increase the basic site of material surface, effect is more obvious.It is amino modified generally
It is divided into and impregnates modified and graft modification, though absorption relative quantity height, after repeatedly adsorption desorption recycles, active group are modified wherein impregnating
It shunts and loses seriously, cause adsorbent stability poor.Chinese patent CN201110147916.6 discloses a kind of mesoporous silicon/organic
Organic amine is supported on silica-base material surface with infusion process by matter compound type carbon dioxide adsorbent, and there are long-time stability differences
Disadvantage.Grafting modification is more stable, but adsorbance is relatively low.Chinese patent CN103920463A discloses a kind of reflux grafting modification
Silicon substrate solid amine carbon dioxide absorber, although more stable, adsorbance is lower.Therefore it is high, hot steady to develop a kind of adsorption capacity
It is qualitative it is good, that good adsorbent is recycled is most important to carbon dioxide capture.
Summary of the invention
The present invention is intended to provide a kind of preparation method of amino modified silicon substrate carbon dioxide absorber.
The present invention provides a kind of preparation methods of amino modified silicon substrate carbon dioxide absorber, including subcritical grafting
Modified two steps of modified and ultrasonic immersing；
The subcritical grafting modifying process the following steps are included:
Solvent is added in beaker, amino-organosilanes are added, is placed on magnetic stirring apparatus and at the uniform velocity stirs 5-
10min, adds silicon substrate carrier, continues to stir 5-10min at room temperature, the mixture in beaker is transferred to autoclave
It is interior, then reaction kettle is placed in 90-100 DEG C of drying box, carries out the solid product in autoclave after 8-12h
It filters, and is respectively rinsed twice with dehydrated alcohol and water, obtained solid is placed in 85-110 DEG C of drying box dry 12h, is had
The silane-modified silica-base material of machine；
The ultrasonic immersing modifying process the following steps are included:
After anhydrous methanol is added in beaker, organic amine modifying agent and magnetic stirring apparatus rotor are added, then burning
Cup, which is placed on magnetic stirring apparatus, at the uniform velocity stirs 10-20min, adds the resulting organosilane-modified silica-base material of step (1),
Beaker mouth is sealed with plastic film, continues to stir 10-20min, then beaker is placed in microwave oscillator and vibrates 2-3h, so
The sealing film on beaker is removed afterwards while beaker is placed on magnetic stirring apparatus to continue to stir to methanol volatilization and is finished, then
Dry 10-12h beaker is placed in 70-90 DEG C of drying box to get amino modified silicon substrate carbon dioxide absorber.
In above-mentioned preparation method, the silicon substrate carrier is any one of MCM-41, SBA-15 or 80-150 mesh silica gel.
In above-mentioned preparation method, the amino-organosilanes are aminoethylaminopropyl methyldiethoxysilane or 3- ammonia
Propyl-triethoxysilicane.
In above-mentioned preparation method, the autoclave is the autoclave of polytetrafluoroethyllining lining.
In above-mentioned preparation method, the organic amine modifying agent is tetraethylenepentamine, polyethyleneimine, diethylenetriamine
It is any.
In above-mentioned preparation method, solvent used in the subcritical grafting modifying process is for dehydrated alcohol or without water beetle
Benzene.
Further, the solid-to-liquid ratio of silicon substrate carrier and dehydrated alcohol is 1g/50-100ml.
Alternatively, the solid-to-liquid ratio of silicon substrate carrier and dry toluene is 1g/50-100ml.
In above-mentioned preparation method, the solid-to-liquid ratio of the silicon substrate carrier and amino-organosilanes is 1g/0.5-3ml.
In above-mentioned preparation method, the mass ratio of the organosilane-modified silica-base material and organic amine modifying agent is
1g/0.35-3g；The solid-to-liquid ratio of organic amine modifying agent and anhydrous methanol is 1g/15-20ml.
The present invention utilizes the silicon hydroxyl in the silanol group and silica-base material cell walls of amino silane by subcritical grafting procedures
Condensation reaction occurs for base, aminoalkyl chain is fixed on channel surfaces, to improve channel surfaces basic sites.Meanwhile fixed alkane
Base chain has certain peptizaiton to the organic amine modifying agent of dipping, to improve amino utilization ratio, reaches raising carbon dioxide
The effect of adsorbance.And at high temperature, fixed alkyl chain is lost the organic amine for reducing dipping from duct and plays centainly
Effect so that the stability of adsorbent is correspondinglyd increase.
Beneficial effects of the present invention: by the way that subcritical grafting procedures are combined with ultrasonic immersing process, adsorbent it is steady
Qualitative and carbon dioxide adsorbance is improved simultaneously；The carbon dioxide absorber prepared using this method is with higher
Carbon dioxide adsorption ability, preferable thermal stability, can more efficiently trap carbon dioxide.
Detailed description of the invention
Fig. 1 is 1 gained adsorbent De contamination cyclical stability test chart of embodiment.
Fig. 2 is 2 gained adsorbent De contamination cyclical stability test chart of embodiment.
Fig. 3 is 3 gained adsorbent De contamination cyclical stability test chart of embodiment.
Specific embodiment
The present invention is further illustrated below by embodiment, but is not limited to following embodiment.
Embodiment 1:
1, a kind of preparation method of amino modified silicon substrate carbon dioxide absorber, comprising the following steps:
150ml dehydrated alcohol is added in 250ml beaker, 1ml 3- aminopropyl triethoxysilane (APTES) is added,
It is placed on magnetic stirring apparatus and at the uniform velocity stirs 10min, add 2g MCM-41, continue to stir 10min at room temperature, in beaker
Mixture is transferred in the autoclave for the polytetrafluoroethyllining lining that capacity is 200ml, and then autoclave is placed on
In 100 DEG C of drying box, the solidliquid mixture in autoclave is filtered after 12h, and each with dehydrated alcohol and water
It rinses twice, obtained solid is placed in 85 DEG C of drying box dry 12h, obtains organosilane-modified silica-base material, is denoted as
MCM-41-APTES。
20ml anhydrous methanol is added in the beaker of 100ml, 0.7g tetraethylenepentamine (TEPA) is added and magnetic force stirs
Device rotor is mixed, then beaker is placed on magnetic stirring apparatus and at the uniform velocity stirs 10min, 1g MCM-41-APTES is added, then uses
Plastic film seals beaker mouth, continues after stirring 20min, beaker is placed in microwave oscillator and vibrates 2h, then beaker
On sealing film remove, while beaker is placed on magnetic stirring apparatus and continues stirring to methanol volatilization and finishes, then beaker
It is placed on the silicon substrate carbon dioxide absorber that dry 12h is amino modified to get " two-step method " in 85 DEG C of drying box, is denoted as MCM-
41-APTES-TEPA。
2, carbon dioxide adsorption is tested
Carbon dioxide adsorption is carried out to above-mentioned products obtained therefrom MCM-41-APTES-TEPA using fixed bed reactors to divide
Analysis, studies its carbon dioxide adsorption at 45 DEG C, 55 DEG C, 65 DEG C, 75 DEG C and 95 DEG C.
First by the MCM-41-APTES-TEPA absorbent filling of 1.5g in fixed bed, formed adsorption column, then with
The gas flow rate degree of 100ml/min is passed through nitrogen, and temperature is increased to 120 DEG C, keeps 90min at 120 DEG C.It later will be warm
Degree drops to required test temperature, and nitrogen is switched to the mixed of carbon dioxide that carbon dioxide volumetric concentration is 20% and nitrogen
Gas is closed, gaseous mixture gas flow rate is 60ml/min.Concentration point is carried out to by the gas after adsorption column with flue gas analyzer simultaneously
Analysis, then calculates carbon dioxide adsorption with following formula (1).Test result is listed in Table 1 below.
(1)
In above formula,q- carbon dioxide adsorption, mmolg-1
Q- mixed gas flow, mlmin-1
t- adsorption reaction carries out time, s
C 0Carbon dioxide volume fraction, % in-gaseous mixture
C—tCarbon dioxide volume fraction, % in moment absorption tail gas
WThe quality of-adsorbent, g.
The carbon dioxide adsorption test result of 1 MCM-41-APTES-TEPA of table
It can be seen from Table 1 that carbon dioxide adsorption declines again after gradually rising as temperature increases, at 75 DEG C,
Reach highest adsorbance, is 3.95mmol/g.
3, adsorbent De contamination cyclical stability is tested
Test is parsed to the sample MCM-41-APTES-TEPA temp.-changing adsorption for carrying out 10 times using fixed bed reactors,
Adsorption process is to carry out, parse under carbon dioxide and nitrogen mixture atmosphere that gas concentration lwevel is 20% at 75 DEG C
Journey is carried out under nitrogen atmosphere at 120 DEG C.First by the MCM-41-APTES-TEPA absorbent filling of 1.5g in fixation
In bed, adsorption column is formed, nitrogen is then passed through with the gas flow rate degree of 100ml/min, and temperature is increased to 120 DEG C, 120
90min is kept at DEG C.75 DEG C are reduced the temperature to later, and nitrogen is switched into the titanium dioxide that carbon dioxide volumetric concentration is 20%
The gaseous mixture of carbon and nitrogen, gaseous mixture gas flow rate are 60ml/min.Simultaneously with flue gas analyzer to the gas after passing through adsorption column
Body carries out concentration analysis, and gaseous mixture is switched to pure nitrogen gas again again after adsorption process, nitrogen flow 100ml/min, and
Temperature is increased to 120 DEG C, adsorbent is allowed to desorb 60min at 120 DEG C.The above process is repeated 10 times.Test result is shown in Fig. 1
It is shown.
As seen in Figure 1, survey is parsed by carrying out 10 temp.-changing adsorptions to sample MCM-41-APTES-TEPA
Examination, the carbon dioxide adsorption of sample are held essentially constant, and illustrate that sample has preferable absorption stability.
Embodiment 2:
1, a kind of preparation method of amino modified silicon substrate carbon dioxide absorber, comprising the following steps:
150ml dehydrated alcohol is added in 250ml beaker, 1ml3- aminopropyl triethoxysilane (APTES) is added,
It is placed on magnetic stirring apparatus and at the uniform velocity stirs 10min, add 2g SBA-15, continue to stir 10min at room temperature, in beaker
Mixture is transferred in the autoclave for the polytetrafluoroethyllining lining that capacity is 200ml, and then autoclave is placed on
In 100 DEG C of drying box, the solidliquid mixture in autoclave is filtered after 12h, and each with dehydrated alcohol and water
It rinses twice, obtained solid is placed in 85 DEG C of drying box dry 12h, obtains organosilane-modified silica-base material, is denoted as
SBA-15-APTES。
20ml anhydrous methanol is added in the beaker of 100ml, 0.7g tetraethylenepentamine (TEPA) is added and magnetic force stirs
Device rotor is mixed, then beaker is placed on magnetic stirring apparatus and at the uniform velocity stirs 10min, 1g SBA-15-APTES is added, then uses
Plastic film seals beaker mouth, continues after stirring 20min, beaker is placed in microwave oscillator and vibrates 2h, then beaker
On sealing film remove simultaneously, beaker is placed on magnetic stirring apparatus continue stirring to methanol volatilization finish, then beaker
It is placed on the silicon substrate carbon dioxide absorber that dry 12h is amino modified to get " two-step method " in 85 DEG C of drying box, is denoted as SBA-
15-APTES-TEPA。
2, carbon dioxide adsorption is tested
Carbon dioxide adsorption is carried out to above-mentioned products obtained therefrom SBA-15-APTES-TEPA using fixed bed reactors to divide
Analysis, studies its carbon dioxide adsorption at 45 DEG C, 55 DEG C, 65 DEG C, 75 DEG C and 95 DEG C.
First by the SBA-15-APTES-TEPA absorbent filling of 1.5g in fixed bed, formed adsorption column, then with
The gas flow rate degree of 100ml/min is passed through nitrogen, and temperature is increased to 120 DEG C, keeps 90min at 120 DEG C.It later will be warm
Degree drops to required test temperature, and nitrogen is switched to the mixed of carbon dioxide that carbon dioxide volumetric concentration is 20% and nitrogen
Gas is closed, gaseous mixture gas flow rate is 60ml/min.Concentration point is carried out to by the gas after adsorption column with flue gas analyzer simultaneously
Analysis, then calculates carbon dioxide adsorption with formula (1).Test result is listed in Table 2 below.
The carbon dioxide adsorption test result of 2 SBA-15-APTES-TEPA of table
It can be seen from Table 2 that decline after the adsorbance of carbon dioxide gradually rises as the temperature rises, at 75 DEG C again
When, reach highest adsorbance, is 5.17mmol/g.
3, adsorbent De contamination cyclical stability is tested
Test is parsed to the sample SBA-15-APTES-TEPA temp.-changing adsorption for carrying out 10 times using fixed bed reactors,
Adsorption process is to carry out, parse under carbon dioxide and nitrogen mixture atmosphere that gas concentration lwevel is 20% at 75 DEG C
Journey is carried out under nitrogen atmosphere at 120 DEG C.First by the SBA-15-APTES-TEPA absorbent filling of 1.5g in fixation
In bed, adsorption column is formed, nitrogen is then passed through with the gas flow rate degree of 100ml/min, and temperature is increased to 120 DEG C, 120
90min is kept at DEG C.75 DEG C are reduced the temperature to later, and nitrogen is switched into the titanium dioxide that carbon dioxide volumetric concentration is 20%
The gaseous mixture of carbon and nitrogen, gaseous mixture gas flow rate are 60ml/min.Simultaneously with flue gas analyzer to the gas after passing through adsorption column
Body carries out concentration analysis, and gaseous mixture is switched to pure nitrogen gas again again after adsorption process, nitrogen flow 100ml/min, and
Temperature is increased to 120 DEG C, adsorbent is allowed to desorb 60min at 120 DEG C.The above process is repeated 10 times.Test result is shown in Fig. 2
It is shown.
As seen in Figure 2, survey is parsed by carrying out 10 temp.-changing adsorptions to sample SBA-15-APTES-TEPA
Examination, the carbon dioxide adsorption of sample are held essentially constant, and illustrate that sample has preferable absorption stability.
Embodiment 3:
1, a kind of preparation method of amino modified silicon substrate carbon dioxide absorber, comprising the following steps:
150ml dehydrated alcohol is added in 250ml beaker, 1ml3- aminopropyl triethoxysilane (APTES) is added,
It is placed on magnetic stirring apparatus and at the uniform velocity stirs 10min, add 2g silica gel, continue to stir 10min at room temperature, beaker
In mixture be transferred to capacity be 200ml polytetrafluoroethyllining lining autoclave in, then autoclave is put
Set in 100 DEG C of drying box, filter the solidliquid mixture in autoclave after 12h, and with dehydrated alcohol and
Water respectively rinses twice, and obtained solid is placed in 85 DEG C of drying box dry 12h, obtains organosilane-modified silica-base material, remembers
For silica gel-APTES.
20ml anhydrous methanol is added in the beaker of 100ml, 0.7g tetraethylenepentamine (TEPA) is added and magnetic force stirs
Device rotor is mixed, then beaker is placed on magnetic stirring apparatus and at the uniform velocity stirs 10min, adds 1g silica gel-APTES, so
Beaker mouth is sealed with plastic film afterwards, continue stir 20min after, beaker is placed in microwave oscillator and vibrates 2h, then
Sealing film on beaker removes simultaneously, beaker is placed on magnetic stirring apparatus continue stirring to methanol volatilization finish, then
Beaker is placed on the silicon substrate carbon dioxide absorber that dry 12h is amino modified to get " two-step method " in 85 DEG C of drying box, is denoted as
silica gel-APTES-TEPA。
2, carbon dioxide adsorption is tested
Carbon dioxide adsorption is carried out to above-mentioned products obtained therefrom silica gel-APTES-TEPA using fixed bed reactors
Analysis, its carbon dioxide adsorption at 45 DEG C, 55 DEG C, 65 DEG C, 75 DEG C and 95 DEG C is studied.
First by the silica gel-APTES-TEPA absorbent filling of 1.5g in fixed bed, adsorption column is formed, then
It is passed through nitrogen with the gas flow rate degree of 100ml/min, and temperature is increased to 120 DEG C, keeps 90min at 120 DEG C.Later will
Temperature drops to required test temperature, and nitrogen is switched to carbon dioxide that carbon dioxide volumetric concentration is 20% and nitrogen
Gaseous mixture, gaseous mixture gas flow rate are 60ml/min.Concentration is carried out to by the gas after adsorption column with flue gas analyzer simultaneously
Analysis, then calculates carbon dioxide adsorption with formula (1).Test result is listed in Table 3 below.
The carbon dioxide adsorption test result of 3 silica gel-APTES-TEPA of table
It can be seen from Table 3 that decline after being gradually risen with the adsorbance of temperature elevated carbon dioxide, at 75 DEG C again
When, reach highest adsorbance, is 4.85mmol/g.
3, adsorbent De contamination cyclical stability is tested
The sample silica gel-APTES-TEPA temp.-changing adsorption for carrying out 10 times is parsed using fixed bed reactors and is surveyed
Examination, adsorption process are to carry out at 75 DEG C under carbon dioxide and nitrogen mixture atmosphere that gas concentration lwevel is 20%,
Resolving is carried out under nitrogen atmosphere at 120 DEG C.First by the silica gel-APTES-TEPA adsorbent of 1.5g
It is filled in fixed bed, forms adsorption column, nitrogen is then passed through with the gas flow rate degree of 100ml/min, and temperature is increased to
120 DEG C, 90min is kept at 120 DEG C.75 DEG C are reduced the temperature to later, and nitrogen is switched into carbon dioxide volumetric concentration and is
20% carbon dioxide and the gaseous mixture of nitrogen, gaseous mixture gas flow rate are 60ml/min.Simultaneously with flue gas analyzer to pass through inhale
Gas after attached column carries out concentration analysis, gaseous mixture is switched to pure nitrogen gas again again after adsorption process, nitrogen flow is
100ml/min, and temperature is increased to 120 DEG C, allow adsorbent to desorb 60min at 120 DEG C.The above process is repeated 10 times.It surveys
Test result is as shown in Figure 3.
As seen in Figure 3, it is parsed by carrying out 10 temp.-changing adsorptions to sample silica gel-APTES-TEPA
Test, the carbon dioxide adsorption of sample are held essentially constant, and illustrate that sample has preferable absorption stability.
Claims (8)
1. a kind of preparation method of amino modified silicon substrate carbon dioxide absorber, which is characterized in that change including subcritical grafting
Property and microwave impregnate modified two steps；
(1) subcritical grafting modifying process the following steps are included:
Reaction dissolvent is added in beaker, amino-organosilanes are added, is placed on magnetic stirring apparatus and at the uniform velocity stirs 5-
10min, adds silicon substrate carrier, continues to stir 5-10min at room temperature, the mixture in beaker is transferred to autoclave
It is interior, then reaction kettle is placed in 90-100 DEG C of drying box, carries out the solid product in autoclave after 8-12h
It filters, and is respectively rinsed twice with dehydrated alcohol and water, obtained solid is placed in 85-110 DEG C of drying box dry 12h, is had
The silane-modified silica-base material of machine；
The silicon substrate carrier is one of MCM-41, SBA-15 or 80-150 mesh silica gel；
(2) microwave dipping modifying process the following steps are included:
After anhydrous methanol is added in beaker, organic amine modifying agent and magnetic stirring apparatus rotor are added, then beaker is put
10-20min is at the uniform velocity stirred on magnetic stirring apparatus, the resulting organosilane-modified silica-base material of step (1) is added, with modeling
Material film seals beaker mouth, continues stirring 10-20min to prevent anhydrous methanol from volatilizing and beaker is then placed on microwave oscillation
2-3h is vibrated in device, then the sealing film on beaker is removed, while beaker is placed on magnetic stirring apparatus and continues stirring to first
Alcohol volatilization finishes, and beaker is placed on dry 10-12h in 70-90 DEG C of drying box and inhaled to get amino modified silicon substrate carbon dioxide
Attached dose.
2. the preparation method of amino modified silicon substrate carbon dioxide absorber according to claim 1, it is characterised in that: institute
The amino-organosilanes stated are aminoethylaminopropyl methyldiethoxysilane or 3- aminopropyl triethoxysilane.
3. the preparation method of amino modified silicon substrate carbon dioxide absorber according to claim 1, it is characterised in that: institute
The autoclave stated is the autoclave of polytetrafluoroethyllining lining.
4. the preparation method of amino modified silicon substrate carbon dioxide absorber according to claim 1, it is characterised in that: institute
The organic amine modifying agent stated be tetraethylenepentamine, polyethyleneimine, diethylenetriamine it is any.
5. the preparation method of amino modified silicon substrate carbon dioxide absorber according to claim 1, it is characterised in that: institute
Stating reaction dissolvent used in subcritical grafting modifying process is dehydrated alcohol or dry toluene.
6. the preparation method of amino modified silicon substrate carbon dioxide absorber according to claim 5, it is characterised in that: sub-
In critical grafting modifying process, the solid-to-liquid ratio of silicon substrate carrier and reaction dissolvent is 1g/50-100mL.
7. the preparation method of amino modified silicon substrate carbon dioxide absorber according to claim 1, it is characterised in that: sub-
In critical grafting modifying process, the solid-to-liquid ratio of the silicon substrate carrier and amino-organosilanes is 1g/0.5-3mL.
8. the preparation method of amino modified silicon substrate carbon dioxide absorber according to claim 1, it is characterised in that: institute
The mass ratio of the organosilane-modified silica-base material and organic amine modifying agent stated is 1g/0.35-3g；Organic amine modifying agent and nothing
The solid-to-liquid ratio of water methanol is 1g/15-20mL.
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