CN107159107A - A kind of preparation method of graphene/silicon aeroge compound adsorbent - Google Patents
A kind of preparation method of graphene/silicon aeroge compound adsorbent Download PDFInfo
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- CN107159107A CN107159107A CN201610130115.1A CN201610130115A CN107159107A CN 107159107 A CN107159107 A CN 107159107A CN 201610130115 A CN201610130115 A CN 201610130115A CN 107159107 A CN107159107 A CN 107159107A
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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
- B01D53/04—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 with stationary adsorbents
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Abstract
Present invention relates particularly to a kind of preparation method of graphene/silicon aeroge composite adsorbing material.First prepare tetraethyl orthosilicate, the mixed solution of water and ethanol simultaneously adds hydrochloric acid solution, it is sufficiently stirred for, pH adds powdery graphite alkene and atlapulgite when reaching 2~3, then 10min is handled using ultrasonic oscillation, adding ammonia spirit makes PH be 6~7, stood under room temperature condition to gel state, gel is put into tetraethyl orthosilicate, ethanol, aging at room temperature in the mixed solution of ammoniacal liquor, then gel is placed in n-hexane and soaks 24h displacement solvents, 2d is modified in the hexane solution containing trim,ethylchlorosilane afterwards, gel is dried at normal temperatures and pressures, it is finally continuous at 50 DEG C in the way of temperature programming, 80 DEG C, each dry 6h at 100 DEG C, 2h, 1.5h obtains graphene/silicon aeroge compound adsorbent.
Description
Technical field
The invention belongs to Organic Waste Gas Pollution control field, and in particular to a kind of graphene/silicon aeroge compound adsorbent
Preparation method.
Background technology
Atmosphere pollution is one of topmost environmental problem of current China, and industrial waste gas is cause atmosphere pollution main
Reason, and the organic exhaust gas formed in oil and chemical industry production process is then intractable industrial waste gas, it is organic
Waste gas can form adverse effect to the growth course of animals and plants, can also cause human organ exhaustion, poisoning, mutation,
The serious consequences such as canceration.At present the method that is recycled to organic exhaust gas mainly including absorption method, absorption process,
The development of condensation method etc., wherein absorption method is more ripe, and this method has that easy to operate, safety, equipment is simple, choosing
Selecting property is good, desorption easily, the series of advantages such as mechanical strength is good, be recovery VOCs effective ways.
The active charcoal of conventional adsorbent and silica gel of absorption method etc., and the present invention then utilizes graphene and silica aerogel system
For a kind of compound adsorbent is gone out, graphene has many bigger serface, hole, corrosion resistance, high adsorption capacity, height
The advantages of elastic and high adsorption strength, aerosil has porous, high porosity and big specific surface area
The advantages of.Therefore, the present invention combines the advantage of graphene and silica aerogel, prepares a kind of compound-type adsorbent.
Domestic and foreign databases retrieved according to the technology of the present invention feature, show through retrieval result, there are many related compounds
The research of adsorbent is found.Received for example, Chinese patent CN102658094A proposes a kind of silica with cellulose
Rice compound adsorbent and preparation method thereof, it is characterised in that described silica and cellulose nano composite adsorbent
It is prepared from by cellulose and siliconoxide precursor mixed solution and surfactant solution for raw material.Chinese patent
CN1899683 relate to a kind of ammonia refrigeration adsorbent and its preparation method and application, more particularly to a kind of ammonia refrigeration
With attapulgite clay base composite adsorbent and its preparation and application.A kind of ferrite of Chinese patent CN103191699A propositions/
Graphene composite adsorbent and its preparation, application method, it is characterised in that ferrite weight/mass percentage composition is
40%~70%, ferrite nano particles are dispersed in the graphenic surface of sheet, the particle diameter distribution of ferrite nano particles
For 5~30nm, ferrite, graphene composite adsorbent specific surface area are 60~300m2/g.The above method has one
Fixed recovering effect, but the low problem of generally existing adsorption efficiency, present invention research is proposed for this.
The content of the invention
For problems and shortcomings present in background technology, it is a primary object of the present invention in " sol-gel " method
On the basis of, graphene and silica aerogel advantage are made full use of, using tetraethyl orthosilicate TEOS as silicon source, one is doped into
Powder quantitatively shape graphene, and add appropriate atlapulgite and make binding agent, prepare adsorption effect preferably nonpolar
Compound adsorbent.
The technical scheme is that first making the mixed solution of tetraethyl orthosilicate, water and ethanol, solution is prepared
A certain amount of hydrochloric acid solution is added thereto afterwards, while full and uniform stirring so that pH value of solution reaches 2~3 scope
When add a certain amount of powdery graphite alkene and appropriate atlapulgite, utilize ultrasonic oscillation processing 10min, stirring
50min, obtains well dispersed mixture, and certain density ammonia spirit is then added dropwise thereto while filling
Point stirring causes solution PH to be 6~7, stands to gel state under room temperature condition, and be put into tetraethyl orthosilicate, ethanol,
Aging at room temperature in the mixed solution of ammoniacal liquor, is then placed in immersion 24h progress in n-hexane molten by the gel after aging
Agent is replaced, afterwards the modified 2d in the hexane solution containing trim,ethylchlorosilane, by gained gel at normal temperatures and pressures
Drier in dry, last continuous 6h, 2h, 1.5h of being dried at 50 DEG C, 80 DEG C, 100 DEG C obtains graphite
Alkene/silica aerogel compound adsorbent.
The technical solution adopted by the present invention specifically includes following steps：
(1) sol-gel process：Silicon source tetraethyl orthosilicate, water and ethanol are mixed into (TEOS, H2O、EtOH
Mol ratio be 1:6:5) hydrochloric acid solution for adding 0.08mol/L after solution thereto, is prepared, while fully
Even stirring so that pH value of solution adds a certain amount of powdery graphite alkene (200 mesh~400 when reaching 2~3 scope
Mesh, accounts for solution quality percentage 0.5wt%~2wt%) stirring 2min, appropriate atlapulgite is added, continues to stir
2min is mixed, then 10min is handled using ultrasonic oscillation, 50min is stirred under 70 DEG C of constant temperatures, thus
Well dispersed mixture is obtained, certain density ammonia spirit is then added dropwise thereto while being sufficiently stirred for making
Solution PH is 6~7, stand to gel state under room temperature condition.
(2) gel aging and solvent displacement：Gel obtained by 1st step is put into tetraethyl orthosilicate, ethanol, ammoniacal liquor
Mixed solution at room temperature 12~24h of aging (wherein, TEOS, EtOH, ammoniacal liquor mol ratio be 1:1:1),
Then the gel after aging is placed in immersion in n-hexane and carries out solvent displacement, a n-hexane is changed per 6h, more
Change 4 times so that water and ethanol in gel are sufficiently displaced from.
(3) gel surface is modified：The hexane solution of 8% (V) trim,ethylchlorosilane is prepared, by the 2nd step institute
Obtain gel and be placed in hydrophobically modified 2d in the solution.
(4) gel drying：2d will be dried in the drier of gel obtained by 3rd step at normal temperatures and pressures, finally pressed
Graphene is obtained according to mode continuous each at 50 DEG C, 80 DEG C, 100 DEG C dry 6h, 2h, 1.5h of temperature programming
/ silica aerogel compound adsorbent.
The advantage of the invention is that：
(1) silicon source of the present invention is TEOS, products therefrom high purity.
(2) doped graphene of the present invention, products obtained therefrom intensity is big, elasticity is high.
(3) binding agent is made with atlapulgite in the present invention so that gained graphene/silicon aeroge compound adsorbent
Stability is improved, and intensity is guaranteed.
(4) present invention utilizes two kinds of hydrochlorics and ammoniacal liquor, makes sol-gel process in the state of alkali after first acid,
Improve reaction rate.
Specific embodiment
This patent is illustrated below by some embodiments, but the present invention is not limited by the example：
Embodiment 1：
(1) sol-gel process：Silicon source tetraethyl orthosilicate is mixed into (TEOS, H with water and ethanol2O、EtOH
Mol ratio be 1:6:5) hydrochloric acid solution for adding 0.08mol/L after solution thereto, is prepared, while fully
Even stirring so that pH value of solution adds a certain amount of powdery graphite alkene when reaching 2 (200 mesh account for solution quality hundred
Divide than being 2wt%) stirring 2min, appropriate atlapulgite is added, continues stirring 2min, then utilizes ultrasound
Ripple concussion processing 10min, 50min is stirred under 70 DEG C of constant temperatures, well dispersed mixture is thus obtained,
Then certain density ammonia spirit is added dropwise thereto while being sufficiently stirred for so that solution PH is 6, room temperature condition
It is lower to stand to gel state.
(2) gel aging and solvent displacement：Gel obtained by 1st step is put into tetraethyl orthosilicate, ethanol, ammoniacal liquor
Mixed solution at room temperature aging 12h (wherein, TEOS, EtOH, ammoniacal liquor mol ratio be 1:1:1), then
Gel after aging is placed in immersion in n-hexane and carries out solvent displacement, a n-hexane is changed per 6h, 4 are changed
It is secondary so that water and ethanol in gel are sufficiently displaced from.
(3) gel surface is modified：The hexane solution of 8% (V) trim,ethylchlorosilane is prepared, by the 2nd step institute
Obtain gel and be placed in hydrophobically modified 2d in the solution.
(4) gel drying：2d will be dried in the drier of gel obtained by 3rd step at normal temperatures and pressures, finally pressed
Graphene is obtained according to mode continuous each at 50 DEG C, 80 DEG C, 100 DEG C dry 4h, 2h, 1.5h of temperature programming
/ silica aerogel compound adsorbent.
Embodiment 2：
(1) sol-gel process：Silicon source tetraethyl orthosilicate is mixed into (TEOS, H with water and ethanol2O、EtOH
Mol ratio be 1:6:5) hydrochloric acid solution for adding 0.08mol/L after solution thereto, is prepared, while fully
Even stirring so that pH value of solution adds a certain amount of powdery graphite alkene when reaching 2 scope (325 mesh, account for solution
Mass percent is 2wt%) stirring 2min, appropriate atlapulgite is added, continues to stir 2min, Ran Houli
10min is handled with ultrasonic oscillation, 50min is stirred under 70 DEG C of constant temperatures, well dispersed mix thus is obtained
Compound, is then added dropwise certain density ammonia spirit while being sufficiently stirred for so that solution PH is 6, room thereto
Stood under the conditions of temperature to gel state.
(2) gel aging and solvent displacement：Gel obtained by 1st step is put into tetraethyl orthosilicate, ethanol, ammoniacal liquor
Mixed solution at room temperature aging 12h (wherein, TEOS, EtOH, ammoniacal liquor mol ratio be 1:1:1), then
Gel after aging is placed in immersion in n-hexane and carries out solvent displacement, a n-hexane is changed per 6h, 4 are changed
It is secondary so that water and ethanol in gel are sufficiently displaced from.
(3) gel surface is modified：The hexane solution of 8% (V) trim,ethylchlorosilane is prepared, by the 2nd step institute
Obtain gel and be placed in hydrophobically modified 2d in the solution.
(4) gel drying：2d will be dried in the drier of gel obtained by 3rd step at normal temperatures and pressures, finally pressed
Graphene is obtained according to mode continuous each at 50 DEG C, 80 DEG C, 100 DEG C dry 4h, 2h, 1.5h of temperature programming
/ silica aerogel compound adsorbent.
Embodiment 3：
(1) sol-gel process：Silicon source tetraethyl orthosilicate is mixed into (TEOS, H with water and ethanol2O、EtOH
Mol ratio be 1:6:5) hydrochloric acid solution for adding 0.08mol/L after solution thereto, is prepared, while fully
Even stirring so that pH value of solution adds a certain amount of powdery graphite alkene when reaching 2 scope (325 mesh, account for solution
Mass percent is 2wt%) stirring 4min, 10min then is handled using ultrasonic oscillation, in 70 DEG C of constant temperature
Under the conditions of stir 50min, thus obtain well dispersed mixture, be then added dropwise thereto certain density
Ammonia spirit is sufficiently stirred for simultaneously so that solution PH is 6, is stood to gel state under room temperature condition.
(2) gel aging and solvent displacement：Gel obtained by 1st step is put into tetraethyl orthosilicate, ethanol, ammoniacal liquor
Mixed solution at room temperature aging 12h (wherein, TEOS, EtOH, ammoniacal liquor mol ratio be 1:1:1), then
Gel after aging is placed in immersion in n-hexane and carries out solvent displacement, a n-hexane is changed per 6h, 4 are changed
It is secondary so that water and ethanol in gel are sufficiently displaced from.
(3) gel surface is modified：The hexane solution of 8% (V) trim,ethylchlorosilane is prepared, by the 2nd step institute
Obtain gel and be placed in hydrophobically modified 2d in the solution.
(4) gel drying：2d will be dried in the drier of gel obtained by 3rd step at normal temperatures and pressures, finally pressed
According to temperature programming mode continuous each at 50 DEG C, 80 DEG C, 100 DEG C dry 4h, 2h, 1.5h obtain graphene/
Silica aerogel compound adsorbent.
Embodiment 4：
(1) sol-gel process：Silicon source tetraethyl orthosilicate is mixed into (TEOS, H with water and ethanol2O、EtOH
Mol ratio be 1:6:5) hydrochloric acid solution for adding 0.08mol/L after solution thereto, is prepared, while fully
Even stirring so that pH value of solution adds a certain amount of powdery graphite alkene when reaching 2 scope (200 mesh, account for solution
Mass percent is 0.5wt%) stirring 2min, appropriate atlapulgite is added, continues to stir 2min, Ran Houli
10min is handled with ultrasonic oscillation, 50min is stirred under 70 DEG C of constant temperatures, well dispersed mix thus is obtained
Compound, is then added dropwise certain density ammonia spirit while being sufficiently stirred for so that solution PH is 6, room thereto
Stood under the conditions of temperature to gel state.
(2) gel aging and solvent displacement：Gel obtained by 1st step is put into tetraethyl orthosilicate, ethanol, ammoniacal liquor
Mixed solution at room temperature aging 12h (wherein, TEOS, EtOH, ammoniacal liquor mol ratio be 1:1:1), then
Gel after aging is placed in immersion in n-hexane and carries out solvent displacement, a n-hexane is changed per 6h, 4 are changed
It is secondary so that water and ethanol in gel are sufficiently displaced from.
(3) gel surface is modified：The hexane solution of 8% (V) trim,ethylchlorosilane is prepared, by the 2nd step institute
Obtain gel and be placed in hydrophobically modified 2d in the solution.
(4) gel drying：2d will be dried in the drier of gel obtained by 3rd step at normal temperatures and pressures, finally pressed
Graphene is obtained according to mode continuous each at 50 DEG C, 80 DEG C, 100 DEG C dry 4h, 2h, 1.5h of temperature programming
/ silica aerogel compound adsorbent.
Embodiment 5：
(1) sol-gel process：Silicon source tetraethyl orthosilicate is mixed into (TEOS, H with water and ethanol2O、EtOH
Mol ratio be 1:6:5) hydrochloric acid solution for adding 0.08mol/L after solution thereto, is prepared, while fully
Even stirring so that pH value of solution handles 10min when reaching 2 scope using ultrasonic oscillation, in 70 DEG C of constant temperature bars
50min is stirred under part, well dispersed mixture is thus obtained, certain density ammonia is then added dropwise thereto
The aqueous solution is sufficiently stirred for simultaneously so that solution PH is 6, is stood to gel state under room temperature condition.
(2) gel aging and solvent displacement：Gel obtained by 1st step is put into tetraethyl orthosilicate, ethanol, ammoniacal liquor
Mixed solution at room temperature aging 12h (wherein, TEOS, EtOH, ammoniacal liquor mol ratio be 1:1:1), then
Gel after aging is placed in immersion in n-hexane and carries out solvent displacement, a n-hexane is changed per 6h, 4 are changed
It is secondary so that water and ethanol in gel are sufficiently displaced from.
(3) gel surface is modified：The hexane solution of 8% (V) trim,ethylchlorosilane is prepared, by the 2nd step institute
Obtain gel and be placed in hydrophobically modified 2d in the solution.
(4) gel drying：2d will be dried in the drier of gel obtained by 3rd step at normal temperatures and pressures, finally pressed
Graphene is obtained according to mode continuous each at 50 DEG C, 80 DEG C, 100 DEG C dry 4h, 2h, 1.5h of temperature programming
/ silica aerogel compound adsorbent.
Graphene/silicon aeroge compound adsorbent adsorbs the performance evaluation of volatile organic matter
The synthesis absorption property of the graphene/silicon aeroge compound adsorbent of addition binding agent is by it to VOCs's
Adsorption rate, desorption efficiency, the test result of heat of adsorption are evaluated.Adsorption rate, desorption efficiency weigh method by difference and determined,
Weighed using photoelectric analytical balance the quality of adsorbent before and after Adsorption and desorption, adsorption rate under corresponding conditionses and relative
Desorption efficiency is calculated by formula (1), (2) respectively：
In formula：The adsorption rate of X --- adsorbent, %；
The desorption efficiency of Y --- adsorbent, %；
m1--- the quality of adsorbent, g before absorption；
m2--- the quality of adsorbent, g after absorption；
m3--- the quality of adsorbent, g before desorption；
m4--- the quality of adsorbent, g after desorption.
Heat of adsorption is measured by placing multi way temperature probe of tester in the different height of adsorption column, compares absorption
Front and rear temperature change.The experimental result of embodiment is as shown in table 1 below.
The comprehensive characteristic test of the compound adsorbent of table 1
According to the adsorption effect of the composite adsorbing material shown in table 1 as can be seen that embodiment 1 and embodiment 2
Adsorption and desorption performance is relatively preferable, it may thus be appreciated that VOCs contamination controls can be made according to the proposed method
Addition binding agent graphene/silicon aeroge composite adsorbing material.
Claims (7)
1. a kind of preparation method of graphene/silicon aeroge compound adsorbent, including colloidal sol, gel, aging,
The process such as solvent displacement, surface modification, dry, it is characterised in that：To the mixed of tetraethyl orthosilicate, water and ethanol
Close and hydrochloric acid solution, powdery graphite alkene and atlapulgite are added in solution；Ammoniacal liquor is added after ultrasonic oscillation processing
Solution, is stored at room temperature to gel；Gel is put into aging in the mixed solution of TEOS, EtOH, ammoniacal liquor；
Soaking solution replaces solvent in n-hexane；It is modified in the hexane solution containing trim,ethylchlorosilane；Normal temperature and pressure
Dry, graphene/silicon aeroge compound adsorbent is finally obtained in the way of temperature programming.
2. a kind of preparation method of graphene/silicon aeroge compound adsorbent according to claim 1, molten
Glue is characterised by：First according to TEOS, H2O, EtOH mol ratio are 1:6:5 make tetraethyl orthosilicate,
The mixed solution of water and ethanol, then addition 0.08mol/L hydrochloric acid solution thereto, while full and uniform stirring,
So that solution PH adds a certain amount of size when reaching 2~3 be that the mesh of 200 mesh~400, mass percent are 0.5
Wt%~2wt% powdery graphite alkene stirring 2min, adds appropriate carclazyte and continues to stir 2min.
3. a kind of preparation method of graphene/silicon aeroge compound adsorbent according to claim 1, coagulates
Glue is characterised by：Resulting solution is handled into 10min using ultrasonic oscillation, stirred under 70 DEG C of constant temperatures
50min, thus obtains well dispersed mixture, and certain density ammonia spirit is then added dropwise thereto
It is sufficiently stirred for causing solution PH to be 6~7 simultaneously, stands to gel state under room temperature condition.
4. a kind of preparation method of graphene/silicon aeroge compound adsorbent according to claim 1, always
Change is characterised by：By gained gel be put into TEOS, EtOH, ammoniacal liquor mol ratio be 1:1:1 mixed solution
In 12~24h of aging at room temperature.
5. a kind of preparation method of graphene/silicon aeroge compound adsorbent according to claim 1, molten
Agent replacement characteristic is：Gel after aging is placed in immersion in n-hexane and carries out solvent displacement, is changed per 6h
N-hexane, is changed 4 times so that water and ethanol in gel are sufficiently displaced from.
6. a kind of preparation method of graphene/silicon aeroge compound adsorbent according to claim 1, table
Face is modified and is characterised by：Gained gel is placed in the hexane solution of 8% (V) trim,ethylchlorosilane and dredged
Water is modified 2d.
7. a kind of preparation method of graphene/silicon aeroge compound adsorbent according to claim 1, does
It is dry to be characterised by：2d will be dried in the drier of gained gel at normal temperatures and pressures, finally according to temperature programming
Mode continuous each at 50 DEG C, 80 DEG C, 100 DEG C dry 6h, 2h, 1.5h obtain graphene/silicon airsetting
Glue compound adsorbent.
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| CN109351331A (en) * | 2018-11-28 | 2019-02-19 | 董佑军 | A kind of porous graphene air cleaning adsorbent material and preparation method thereof |
| CN109603748A (en) * | 2018-12-24 | 2019-04-12 | 青岛双瑞海洋环境工程股份有限公司 | For handling the composite material and preparation method of oily waste water |
| CN110422850A (en) * | 2019-06-25 | 2019-11-08 | 华南理工大学 | High-specific surface area strong-hydrophobicity graphene oxide/silicon dioxide composite aerogel atmospheric preparation method |
| CN111437794A (en) * | 2020-04-24 | 2020-07-24 | 长春工业大学 | SiO (silicon dioxide)2Preparation method of aerogel/activated carbon composite material adsorbent |
| CN111589431A (en) * | 2020-05-19 | 2020-08-28 | 兴核科学研究(福建)有限责任公司 | Preparation method of silver-attached aerogel for adsorbing iodine element |
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| CN109351331A (en) * | 2018-11-28 | 2019-02-19 | 董佑军 | A kind of porous graphene air cleaning adsorbent material and preparation method thereof |
| CN109603748A (en) * | 2018-12-24 | 2019-04-12 | 青岛双瑞海洋环境工程股份有限公司 | For handling the composite material and preparation method of oily waste water |
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| CN110422850A (en) * | 2019-06-25 | 2019-11-08 | 华南理工大学 | High-specific surface area strong-hydrophobicity graphene oxide/silicon dioxide composite aerogel atmospheric preparation method |
| CN111437794A (en) * | 2020-04-24 | 2020-07-24 | 长春工业大学 | SiO (silicon dioxide)2Preparation method of aerogel/activated carbon composite material adsorbent |
| CN111589431A (en) * | 2020-05-19 | 2020-08-28 | 兴核科学研究(福建)有限责任公司 | Preparation method of silver-attached aerogel for adsorbing iodine element |
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Application publication date: 20170915 |