CN109225150A - A kind of preparation method of the dioxide composite silica aerogel of adsorbable formaldehyde - Google Patents
A kind of preparation method of the dioxide composite silica aerogel of adsorbable formaldehyde Download PDFInfo
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- CN109225150A CN109225150A CN201811177074.7A CN201811177074A CN109225150A CN 109225150 A CN109225150 A CN 109225150A CN 201811177074 A CN201811177074 A CN 201811177074A CN 109225150 A CN109225150 A CN 109225150A
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
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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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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
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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
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Abstract
The invention discloses a kind of preparation methods of the dioxide composite silica aerogel of adsorbable formaldehyde, belong to aeroge application field.The existing porous adsorbing material similar to active carbon, the absorption of PARA FORMALDEHYDE PRILLS(91,95) not only lacks specificity, and stability difference automatically parses after easily causing absorption and release formaldehyde again, therefore, the present invention uses sol-gel method at room temperature, it is that raw material and silica progress nanoscale are compound by chitosan, during reaction, taper bottleneck is tamping using sealed membrane, the reaction condition of sealing can be prepared, be conducive to the progress of reaction, it is further acidified and amination modified, obtained modified gel has higher amino content, while and the alkyl containing chitosan itself, the reactive groups such as hydroxyl and amino, the specificity of PARA FORMALDEHYDE PRILLS(91,95) absorption also increases substantially, this adsorbent material is environmentally protective simultaneously, do not generate secondary pollution, and stability is good, do not occur the phenomenon that desorbing release formaldehyde again automatically.
Description
Technical field
The present invention relates to aeroge application field more particularly to a kind of dioxide composite silica aerogels of adsorbable formaldehyde
Preparation method.
Background technique
Aeroge, which typically refers to mutually assemble with nanometer scale ultramicro powder, is constituted nanoporous network structure, and in network
The lightweight nano solid material of gaseous state decentralized medium is full of in hole, aeroge is generally deposited in petroleum, chemical industry and metallurgy industry
?.The most common aeroge is aerosil, and aerosil is that a kind of solar heat protection heat-proof quality is very outstanding
Light nanoporous amorphous solid material, in pipeline, stove and other Thermal Equipments, and silica aerogel and composite material
Substitution Conventional insulation keeps the temperature them, can greatly reduce heat energy loss, improves utilization efficiency of heat energy.
Formaldehyde is well-known a kind of one of indoor gas pollutant, colourless and have strong impulse at room temperature
The sucking of smell, formaldehyde can be to some irreversible injuries of human body band.The administration way of city formaldehyde mainly has at present: light
Catalytic oxidation, Ozonation, metal oxidizing process and absorption method.All the time, absorption method is the most normal of indoor formaldehyde removal
With means, main its is convenient and efficient when being used to adsorb, efficiency is also relatively high, while cheap when making.However it is similar
In the porous adsorbing material of active carbon, after the absorption of PARA FORMALDEHYDE PRILLS(91,95) not only lacks specificity, and stability difference easily causes absorption
It automatically parses and release formaldehyde again.
Summary of the invention
The purpose of the present invention is to solve existing indoor formaldehydes to administer present in absorption method, is similar to active carbon and inhales
Attached shortage specificity, and stability difference easily cause absorption after automatically parse and again release formaldehyde the problem of, and one kind of proposition
The preparation method of the dioxide composite silica aerogel of adsorbable formaldehyde.
To achieve the goals above, present invention employs following technical solutions:
A kind of preparation method of the dioxide composite silica aerogel of adsorbable formaldehyde, comprising the following steps:
S1, the tetraethyl silicate resin (C for measuring 60-65ml8H12O8Si it) in conical flask, is added at room temperature into conical flask
The dehydrated alcohol of 50ml carries out uniformly mixed；
The Chitosan powder of 3-5g is added in S2, the mixed liquor into S1, taper bottleneck is tamping with sealed membrane prepare it is closed
Reaction condition is persistently stirred to react the mixed liquor in conical flask using agitating device, mixing time 10-12h；
S3, while being stirred to mixed liquor, into mixed liquor be added dropwise 2.0-3.0ml mass fraction be 5% HF it is molten
Liquid seals standing 10-12h after 14-16min is continuously added dropwise again, translucent chitosan-silicon dioxide is obtained after standing and is answered
Close gel；
S4, chitosan-silicon dioxide plural gel obtained in S3 is taken out, with the deionized water of 500-1000ml by plural gel
Washing by soaking is carried out, dehydrated alcohol static displacement 2-3 times of 500-1000ml is measured after washing 1-2 times again, replaces 5-6h every time；
S5, it measures the epoxychloropropane of 10-15ml, the dehydrated alcohol that 8-10 drop perchloric acid and 200-250ml is added is mixed
It closes uniformly, the plural gel in S4 after processing is added in mixed liquor and stands 10-12h, is washed after standing with dehydrated alcohol
1-2 times；
S6, take out S5 in plural gel heating water bath is carried out in 50 DEG C of water-bath, and be added 10-15ml ethylenediamine and
The dehydrated alcohol of 40-50ml is mixed, and is stood 10-12h after mixing, is washed 1-2 times, obtained using dehydrated alcohol after standing
To amino modified chitosan-silicon dioxide plural gel；
S7, amino modified chitosan-silicon dioxide plural gel obtained in S6 carries out to acidification, and by plural gel
It carries out cool-drying and chitosan-silicon dioxide aeroge finished product is made；
Formaldehyde Dynamic gas-mixing and adsorption devices are used after S8, experiment, and chitosan-silicon dioxide aeroge obtained is subjected to gaseous state first
The analysis of aldehyde absorption property.
Preferably, chitosan includes polymer chitosan (viscosity average molecular weigh 200kDa), low molecular chitosan in the S2
(viscosity average molecular weigh 3kDa) and O-CMC.
Preferably, in the S2 chitosan deacetylation > 90%.
Preferably, in the S7 acidification of plural gel the following steps are included: amination obtained in S6 is compound
Gel is turned 2-3 times with the n-hexane of 50-100ml, each 5-6h, by the hexa methyl silazane of 15-20ml, 50-100ml just oneself
Alkane pours into after mixing impregnates 10-12h in wet gel, then is eluted 1-2 times with n-hexane, then be placed in acetic acid solution and impregnate 1-
2h, then be placed in dehydrated alcohol and impregnate 20-30min, creeping chill drying process is carried out after washing, and it is multiple that chitosan-silicon dioxide is made
Close aeroge.
Preferably, the formaldehyde Dynamic gas-mixing and adsorption devices, including deionization water tank, formaldehyde heating device, water bath with thermostatic control pan gas
Body circulation pump and thermostat, deionization water tank upper end inside are flexibly connected with the left end pipeline A, lower end on the left of the pipeline A
It is fixedly connected with top on the left of pipeline B, lower end is provided with switch C in the middle part of the pipeline B, and the lower end the switch C is fixedly installed with
Top is fixedly connected with lower end in the middle part of pipeline D on the right side of methylene oxide detecting instrument A, the pipeline B, and upper end is provided on the right side of the pipeline B
Switch E, the formaldehyde heating device internal activity are equipped with formalin bottle, and it is molten that the formalin bottle is internally provided with formaldehyde
Liquid, formalin bottle upper end inside are flexibly connected with lower end in the middle part of pipeline A, and formalin bottle is located in the middle part of the pipeline A
It is provided with switch A on the left of upper end, is located on the right side of formalin bottle upper end in the middle part of the pipeline A and is provided with switch B, the thermostatted water
Bath is internally provided with gas source holding bottle, is flexibly connected on the right side of gas source holding bottle upper end inside left and pipeline A, the gas
Source holding bottle upper end inner right side is flexibly connected with the left end pipeline D, is provided with switch G on the left of the pipeline D；
It is fixedly connected on the downside of the pipeline D right end with gas circulator upper end left side, on the right side of the gas circulator upper end and manages
Lower end is fixedly connected on the left of road E, and the thermostat is internally provided with absorption bottle, and the absorption bottle is internally provided with dioxide composite
Silica aerogel, the absorption bottle upper end inside left are flexibly connected with lower end on the right side of pipeline E, absorption bottle upper end inner right side
It is flexibly connected with lower end on the right side of pipeline C, upper end is provided with switch F in the middle part of the pipeline C, and the upper end the switch F is fixedly installed with
It is provided with switch D on the left of methylene oxide detecting instrument B, the pipeline C, lower end is fixedly connected with the upper end pipeline A on the left of the pipeline C.
Compared with prior art, the present invention provides a kind of preparation sides of the dioxide composite silica aerogel of adsorbable formaldehyde
Method, have it is following the utility model has the advantages that
(1) present invention is gathered a kind of polysaccharide material-shell cheap and easy to get using sol-gel method under conditions of normal temperature and pressure
Sugar is raw material, compound with silica progress nanoscale, during reaction, is tamping taper bottleneck using sealed membrane,
The reaction condition that sealing can be prepared is conducive to the progress of reaction, can be stirred evenly mixed liquor using agitating device, and use
The method that assisted solution is added while stirring, is conducive to assisted solution and sufficiently reacts with mixed liquor, and carry out further to it
Acidification and a kind of new Organic-inorganic composite gel rubber material that is amino modified, and obtaining, obtained modified gel has higher
Amino content, while the reactive groups such as alkyl, hydroxyl and amino again containing chitosan itself, the specificity of PARA FORMALDEHYDE PRILLS(91,95) absorption
It increases substantially, at the same time, this adsorbent material is environmentally protective, does not generate secondary pollution；
(2) present invention is changed with pre-processing translucent plural gel obtained carrying out amination to plural gel
Property will be washed repeatedly with dehydrated alcohol in treated gel, unreacted epoxy chlorine in plural gel can be effectively removed
Propane volume perchloric acid, obtains amino modified chitosan-silicon dioxide plural gel, and amino modified plural gel have it is higher
Amino content, further by amino modified plural gel carry out acidification, before acidification using n-hexane elute repeatedly,
Remaining silane and reactant in plural gel can be effectively removed, the present invention carries out acid to plural gel using the acetic acid of low concentration
Change processing, after treatment are using soaked in absolute ethyl alcohol plural gel, can effectively remove extra acetic acid, pass through again after washing
The mode of freeze-drying is dried, and is analyzed by subsequent gases formaldehyde adsorption property, and chitosan-silicon dioxide obtained is compound
Aeroge has preferable adsorptivity, can effective formaldehyde adsorption, and do not occur desorbing the imaging of release formaldehyde again automatically；
(3) present invention is provided with formaldehyde absorbing dynamic apparatus, chitosan-silicon dioxide composite aerogel to gaseous formaldehyde have compared with
Good adsorptivity, the present invention are put into chitosan-silicon dioxide in absorption bottle first by being provided with formaldehyde Dynamic gas-mixing and adsorption devices
Composite aerogel closes switch A, C, D and G, and switch B and E are opened, and sets 70 DEG C for formaldehyde heating device, heating
It is closed after in 10min, and is fixedly installed with methylene oxide detecting instrument A in the lower end switch C, it, will for measuring the initial concentration of formaldehyde
Switch B and E are closed, and A are turned on the switch, using remaining formaldehyde gas in deionization water tank formaldehyde adsorption solution bottle, on switch F
End is fixedly installed with methylene oxide detecting instrument B, and switch D, G and F are opened, and opens simultaneously the dynamic that gas circulator carries out formaldehyde gas
Absorption, and record each time point content of formaldehyde.
Detailed description of the invention
Fig. 1 is that a kind of principle of the preparation method of the dioxide composite silica aerogel of adsorbable formaldehyde proposed by the present invention is shown
It is intended to；
Fig. 2 is a kind of embodiment 2,3 of the preparation method of the dioxide composite silica aerogel of adsorbable formaldehyde proposed by the present invention
With 4 result schematic diagram；
Fig. 3 is that a kind of formaldehyde dynamic of preparation method of the dioxide composite silica aerogel of adsorbable formaldehyde proposed by the present invention is inhaled
Adsorption device structural schematic diagram.
Figure label explanation:
1 deionization water tank, 2 formaldehyde heating devices, 3 formalin bottles, 4 thermostat water baths, 5 gas source holding bottles, 6 gases circulation
Pump, 7 thermostats, 8 absorption bottles, 9 methylene oxide detecting instrument A, 10 methylene oxide detecting instrument B, 11 pipeline A, 12 pipeline B, 13 pipeline C, 14 pipelines
D, 15 pipeline E, 16 switch A, 17 switch B, 18 switch C, 19 switch D, 20 switch E, 21 switch G, 22 switch F, 23 formalins,
24 dioxide composite silica aerogels.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation description, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.
In the description of the present invention, it is to be understood that, term " on ", "lower", "front", "rear", "left", "right", "top",
The orientation or positional relationship of the instructions such as "bottom", "inner", "outside" is to be based on the orientation or positional relationship shown in the drawings, merely to just
In description the present invention and simplify description, rather than the device or element of indication or suggestion meaning must have a particular orientation, with
Specific orientation construction and operation, therefore be not considered as limiting the invention.
A kind of embodiment 1: preparation method of the dioxide composite silica aerogel of adsorbable formaldehyde, comprising the following steps:
S1, the tetraethyl silicate resin (C for measuring 60-65ml8H12O8Si it) in conical flask, is added at room temperature into conical flask
The dehydrated alcohol of 50ml carries out uniformly mixed；
The Chitosan powder of 3-5g is added in S2, the mixed liquor into S1, taper bottleneck is tamping with sealed membrane prepare it is closed
Reaction condition is persistently stirred to react the mixed liquor in conical flask using agitating device, mixing time 10-12h；
S3, while being stirred to mixed liquor, into mixed liquor be added dropwise 2.0-3.0ml mass fraction be 5% HF it is molten
Liquid seals standing 10-12h after 14-16min is continuously added dropwise again, translucent chitosan-silicon dioxide is obtained after standing and is answered
Close gel；
S4, chitosan-silicon dioxide plural gel obtained in S3 is taken out, with the deionized water of 500-1000ml by plural gel
Washing by soaking is carried out, dehydrated alcohol static displacement 2-3 times of 500-1000ml is measured after washing 1-2 times again, replaces 5-6h every time；
S5, it measures the epoxychloropropane of 10-15ml, the dehydrated alcohol that 8-10 drop perchloric acid and 200-250ml is added is mixed
It closes uniformly, the plural gel in S4 after processing is added in mixed liquor and stands 10-12h, is washed after standing with dehydrated alcohol
1-2 times；
S6, take out S5 in plural gel heating water bath is carried out in 50 DEG C of water-bath, and be added 10-15ml ethylenediamine and
The dehydrated alcohol of 40-50ml is mixed, and is stood 10-12h after mixing, is washed 1-2 times, obtained using dehydrated alcohol after standing
To amino modified chitosan-silicon dioxide plural gel；
S7, amino modified chitosan-silicon dioxide plural gel obtained in S6 carries out to acidification, and by plural gel
It carries out cool-drying and chitosan-silicon dioxide aeroge finished product is made；
Formaldehyde Dynamic gas-mixing and adsorption devices are used after S8, experiment, and chitosan-silicon dioxide aeroge obtained is subjected to gaseous state first
The analysis of aldehyde absorption property.
Chitosan includes polymer chitosan (viscosity average molecular weigh 200kDa), low molecular chitosan (viscosity average molecular weigh in S2
3kDa) and O-CMC.
The deacetylation > 90% of chitosan in S2.
The acidification of plural gel is the following steps are included: by amination plural gel 50- obtained in S6 in S7
The n-hexane of 100ml turns 2-3 times, each 5-6h, and the n-hexane mixing of the hexa methyl silazane of 15-20ml, 50-100ml is equal
It is poured into after even and impregnates 10-12h in wet gel, then eluted 1-2 times with n-hexane, then be placed in acetic acid solution and impregnate 1-2h, then set
20-30min is impregnated in dehydrated alcohol, creeping chill drying process is carried out after washing, and the compound airsetting of chitosan-silicon dioxide is made
Glue.
The present invention uses sol-gel method under conditions of normal temperature and pressure, by a kind of polysaccharide material-shell cheap and easy to get
Glycan is raw material, compound with silica progress nanoscale, during reaction, is sealed taper bottleneck using sealed membrane
Tightly, the reaction condition that can prepare sealing is conducive to the progress of reaction, can be stirred evenly mixed liquor using agitating device, and
Using the method that assisted solution is added while stirring, is conducive to assisted solution and is sufficiently reacted with mixed liquor, and it is carried out into one
The acidification of step and amino modified, and the Organic-inorganic composite gel rubber material that obtained one kind is new, obtained modified gel have compared with
High amino content, while the reactive groups such as alkyl, hydroxyl and amino again containing chitosan itself, PARA FORMALDEHYDE PRILLS(91,95) adsorb special
Property also increases substantially, and at the same time, this adsorbent material is environmentally protective, does not generate secondary pollution.
Embodiment 2: based on embodiment 1 but different, it is with polymer chitosan (viscosity average molecular weigh 200kDa)
Raw material, by 3g polymer chitosan and 60ml tetraethyl silicate resin (C8H12O8Si it) is proportionally mixed, prepares sealing
Reaction environment further pre-processes translucent composite aerogel obtained, and the epoxy chlorine of 10ml is used after pretreatment
The dehydrated alcohol of propane, the perchloric acid of 8 drops 70% and 200ml is uniformly mixed, and amino modified polymer chitosan-dioxy can be made
SiClx plural gel further carries out acidification to amino modified polymer chitosan-silica plural gel, finally makes
Formaldehyde adsorption property analysis is carried out to macromolecule plural gel with formaldehyde Dynamic gas-mixing and adsorption devices, the result measured can be seen that high score
Seed chitosan-silicon dioxide composite aerogel (MCSA) maximum formaldehyde absorbing amount is 0.111mg/g, mainly due to high in MCSA
The viscosity average molecular weigh of molecular chitosan is higher, and the longer steric hindrance when forming covalent bond of the length of chain is larger, it is not easy to stablize
In the presence of.
Embodiment 3: being original with low molecular chitosan (viscosity average molecular weigh 3kDa) based on embodiment 1 but different
Material, 63ml tetraethyl orthosilicate is mixed with 4g, prepares the reaction environment of sealing, further to obtained translucent multiple
It closes aeroge to be pre-processed, the anhydrous second of the epoxychloropropane of 12ml, the perchloric acid of 9 drops 70% and 220ml is used after pretreatment
Alcohol is uniformly mixed, and amino modified low molecular chitosan-silica plural gel can be made, further to amino modified low molecule
Chitosan-silicon dioxide plural gel carry out acidification, into plural gel be added 10ml ethylenediamine and 40ml it is anhydrous
Ethyl alcohol is mixed, and is uniformly mixed to be placed in acetic acid and be impregnated, low molecular chitosan-silicon dioxide composite aerogel can be made
(LMWCSA), formaldehyde adsorption property analysis is carried out to low molecule plural gel using formaldehyde Dynamic gas-mixing and adsorption devices, low molecule shell is poly-
Sugar-silicon dioxide composite aerogel (LMWCSA) maximum formaldehyde removing rate has reached 83.33%, mainly since low molecule shell is poly-
Sugar chain length is relatively short, and the hydroxyl on strand is easier to form covalent bond between silicon dioxide gel.
Embodiment 4: based on embodiment 1 but different, using O-CMC as raw material, by 5g polymer shell
Glycan and 65ml tetraethyl silicate resin (C8H12O8Si it) is proportionally mixed, the epoxy chloropropionate of 15ml is used after pretreatment
The dehydrated alcohol of alkane, the perchloric acid of 10 drops 70% and 250ml is uniformly mixed, and amino modified O-CMC-dioxy can be made
SiClx plural gel further carries out acidification, Xiang Fu to amino modified O-CMC-silica plural gel
The dehydrated alcohol for closing 10ml is added in gel ethylenediamine and 40ml is mixed, and is uniformly mixed to be placed in acetic acid and be impregnated, can make
It obtains O-CMC-silicon dioxide composite aerogel (OCCSA), first is carried out to OCCSA using formaldehyde Dynamic gas-mixing and adsorption devices
The analysis of aldehyde absorption property analyzes result it is found that the adsorption capacity of OCCSA PARA FORMALDEHYDE PRILLS(91,95) is most strong, and desorption is heavy automatically without appearance
The phenomenon that new release formaldehyde is a kind of efficient gaseous formaldehyde adsorbent material compared with active carbon.
Embodiment 5: based on embodiment 1 but different, formaldehyde Dynamic gas-mixing and adsorption devices, including deionization water tank 1, first
Aldehyde heating device 2,4 gas circulator 6 of thermostat water bath and thermostat 7,1 upper end of deionization water tank inside and the left end pipeline A11
It is flexibly connected, lower end is fixedly connected with top on the left of pipeline B12 on the left of pipeline A11, and lower end is provided with switch in the middle part of pipeline B12
The lower end C18, switch C18 is fixedly installed with methylene oxide detecting instrument A9, the fixed company in top and the middle part pipeline D14 lower end on the right side of pipeline B12
It connects, upper end is provided with switch E20 on the right side of pipeline B12, and 2 internal activity of formaldehyde heating device is equipped with formalin bottle 3, and formaldehyde is molten
Liquid bottle 3 is internally provided with formalin 23, is flexibly connected inside 3 upper end of formalin bottle with lower end in the middle part of pipeline A11, pipeline
It is located on the left of formalin bottle upper end in the middle part of A11 and is provided with switch A16, is located on the right side of formalin bottle upper end in the middle part of pipeline A11
It is provided with switch B17, thermostat water bath 4 is internally provided with gas source holding bottle 5,5 upper end inside left of gas source holding bottle and pipeline
It is flexibly connected on the right side of A11,5 upper end inner right side of gas source holding bottle is flexibly connected with the left end pipeline D14, setting on the left of pipeline D14
Have and be fixedly connected on the downside of switch G21 pipeline D14 right end with 6 upper end of gas circulator left side, on the right side of 6 upper end of gas circulator and is managed
Lower end is fixedly connected on the left of road E15, and thermostat 7 is internally provided with absorption bottle 8, and absorption bottle 8 is internally provided with composite silicon dioxide
Aeroge 24, absorption 8 upper end inside left of bottle are flexibly connected with lower end on the right side of pipeline E15, absorption 8 upper end inner right side of bottle and pipe
Lower end is flexibly connected on the right side of road C13, and upper end is provided with switch F22 in the middle part of pipeline C13, and the upper end switch F22 is fixedly installed with formaldehyde
Switch D19 is provided on the left of detector B10, pipeline C13, lower end is fixedly connected with the upper end pipeline A11 on the left of pipeline C13；
The present invention is provided with formaldehyde absorbing dynamic apparatus, and chitosan-silicon dioxide composite aerogel has gaseous formaldehyde preferable
Adsorptivity, it is multiple that the present invention by being provided with formaldehyde Dynamic gas-mixing and adsorption devices, is first put into chitosan-silicon dioxide in absorption bottle
Aeroge is closed, switch A16, C18, D19 and G21 are closed, switch B17 and E20 are opened, set formaldehyde heating device 2 to
It 70 DEG C, is closed after heating in 10min, and be fixedly installed with methylene oxide detecting instrument A9 in the lower end switch C18, for measuring formaldehyde
Switch B17 and E20 are closed, turn on the switch A16 by initial concentration, utilize residue in 1 formaldehyde adsorption solution bottle 3 of deionization water tank
Formaldehyde gas, be fixedly installed with methylene oxide detecting instrument B10 in the upper end switch F22, by switch D19, G21 and F22 open, beat simultaneously
It opens gas circulator 6 and carries out the Dynamic Adsorption of formaldehyde gas, and record each time point content of formaldehyde.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
Anyone skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its
Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (5)
1. a kind of preparation method of the dioxide composite silica aerogel of adsorbable formaldehyde, which comprises the following steps:
S1, the tetraethyl silicate resin (C for measuring 60-65ml8H12O8Si it) in conical flask, is added at room temperature into conical flask
The dehydrated alcohol of 50ml carries out uniformly mixed；
The Chitosan powder of 3-5g is added in S2, the mixed liquor into S1, taper bottleneck is tamping with sealed membrane prepare it is closed
Reaction condition is persistently stirred to react the mixed liquor in conical flask using agitating device, mixing time 10-12h；
S3, while being stirred to mixed liquor, into mixed liquor be added dropwise 2.0-3.0ml mass fraction be 5% HF it is molten
Liquid seals standing 10-12h after 14-16min is continuously added dropwise again, translucent chitosan-silicon dioxide is obtained after standing and is answered
Close gel；
S4, chitosan-silicon dioxide plural gel obtained in S3 is taken out, with the deionized water of 500-1000ml by plural gel
Washing by soaking is carried out, dehydrated alcohol static displacement 2-3 times of 500-1000ml is measured after washing 1-2 times again, replaces 5-6h every time；
S5, it measures the epoxychloropropane of 10-15ml, the dehydrated alcohol that 8-10 drop perchloric acid and 200-250ml is added is mixed
It closes uniformly, the plural gel in S4 after processing is added in mixed liquor and stands 10-12h, is washed after standing with dehydrated alcohol
1-2 times；
S6, take out S5 in plural gel heating water bath is carried out in 50 DEG C of water-bath, and be added 10-15ml ethylenediamine and
The dehydrated alcohol of 40-50ml is mixed, and is stood 10-12h after mixing, is washed 1-2 times, obtained using dehydrated alcohol after standing
To amino modified chitosan-silicon dioxide plural gel；
S7, amino modified chitosan-silicon dioxide plural gel obtained in S6 carries out to acidification, and by plural gel
It carries out cool-drying and chitosan-silicon dioxide aeroge finished product is made；
Formaldehyde Dynamic gas-mixing and adsorption devices are used after S8, experiment, and chitosan-silicon dioxide aeroge obtained is subjected to gaseous state first
The analysis of aldehyde absorption property.
2. a kind of preparation method of the dioxide composite silica aerogel of adsorbable formaldehyde according to claim 1, special
Sign is: chitosan includes that polymer chitosan (viscosity average molecular weigh 200kDa), low molecular chitosan (glue equal molecule in the S2
Measure 3kDa) and O-CMC.
3. a kind of preparation method of the dioxide composite silica aerogel of adsorbable formaldehyde according to claim 1, special
Sign is: the deacetylation > 90% of chitosan in the S2.
4. a kind of preparation method of the dioxide composite silica aerogel of adsorbable formaldehyde according to claim 1, special
Sign is: the acidification of plural gel is the following steps are included: by amination plural gel 50- obtained in S6 in the S7
The n-hexane of 100ml turns 2-3 times, each 5-6h, and the n-hexane mixing of the hexa methyl silazane of 15-20ml, 50-100ml is equal
It is poured into after even and impregnates 10-12h in wet gel, then eluted 1-2 times with n-hexane, then be placed in acetic acid solution and impregnate 1-2h, then set
20-30min is impregnated in dehydrated alcohol, creeping chill drying process is carried out after washing, and the compound airsetting of chitosan-silicon dioxide is made
Glue.
5. a kind of preparation method of the dioxide composite silica aerogel of adsorbable formaldehyde according to claim 1, special
Sign is: the formaldehyde Dynamic gas-mixing and adsorption devices, including deionization water tank (1), formaldehyde heating device (2), thermostat water bath (4) gas
Body circulation pumps (6) and thermostat (7), is flexibly connected inside deionization water tank (1) upper end with the left end pipeline A(11), described
Pipeline A(11) top is fixedly connected on the left of left side lower end and pipeline B(12), the pipeline B(12) in the middle part of lower end be provided with switch C
(18), the switch C(18) lower end is fixedly installed with methylene oxide detecting instrument A(9), the pipeline B(12) right side top and pipeline D
(14) middle part lower end be fixedly connected, the pipeline B(12) right side upper end be provided with switch E(20), the formaldehyde heating device (2)
Internal activity is equipped with formalin bottle (3), and the formalin bottle (3) is internally provided with formalin (23), the formaldehyde
Is flexibly connected with lower end in the middle part of pipeline A(11) inside solution bottle (3) upper end, the pipeline A(11) in the middle part of positioned at formalin bottle
Switch A(16 is provided on the left of upper end), the pipeline A(11) middle part is located at formalin bottle upper end right side and is provided with switch B
(17), the thermostat water bath (4) is internally provided with gas source holding bottle (5), gas source holding bottle (5) the upper end inside left with
Pipeline A(11) right side is flexibly connected, and gas source holding bottle (5) the upper end inner right side is flexibly connected with the left end pipeline D(14), institute
State pipeline D(14) left side be provided with switch G(21)；
The pipeline D(14) it is fixedly connected with gas circulator (6) upper end left side on the downside of right end, on the gas circulator (6)
End right side is fixedly connected with lower end on the left of pipeline E(15), and the thermostat (7) is internally provided with absorption bottle (8), the absorption bottle
(8) it is internally provided with dioxide composite silica aerogel (24), absorption bottle (8) the upper end inside left and pipeline E(15) right side
Lower end is flexibly connected, and absorption bottle (8) the upper end inner right side is flexibly connected with lower end on the right side of pipeline C(13), the pipeline C
(13) middle part upper end is provided with switch F(22), the switch F(22) upper end is fixedly installed with methylene oxide detecting instrument B(10), the pipe
Road C(13) left side be provided with switch D(19), the pipeline C(13) on the left of lower end be fixedly connected with the upper end pipeline A(11).
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| CN201811177074.7A CN109225150A (en) | 2018-10-10 | 2018-10-10 | A kind of preparation method of the dioxide composite silica aerogel of adsorbable formaldehyde |
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