CN102773073A - Preparation method of hydrophobic SiO2 aerogel-activated carbon composite material - Google Patents
Preparation method of hydrophobic SiO2 aerogel-activated carbon composite material Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 60
- 239000002131 composite material Substances 0.000 title claims abstract description 46
- 230000002209 hydrophobic effect Effects 0.000 title claims abstract description 41
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 239000004964 aerogel Substances 0.000 title abstract description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title abstract 4
- 229910052681 coesite Inorganic materials 0.000 title abstract 2
- 229910052906 cristobalite Inorganic materials 0.000 title abstract 2
- 239000000377 silicon dioxide Substances 0.000 title abstract 2
- 235000012239 silicon dioxide Nutrition 0.000 title abstract 2
- 229910052682 stishovite Inorganic materials 0.000 title abstract 2
- 229910052905 tridymite Inorganic materials 0.000 title abstract 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000003756 stirring Methods 0.000 claims abstract description 22
- 239000011240 wet gel Substances 0.000 claims abstract description 22
- 239000003054 catalyst Substances 0.000 claims abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000002904 solvent Substances 0.000 claims abstract description 12
- 238000006068 polycondensation reaction Methods 0.000 claims abstract description 11
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 9
- 239000010703 silicon Substances 0.000 claims abstract description 9
- 239000003513 alkali Substances 0.000 claims abstract description 5
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 5
- 230000007062 hydrolysis Effects 0.000 claims abstract description 4
- 238000006460 hydrolysis reaction Methods 0.000 claims abstract description 4
- 229910052799 carbon Inorganic materials 0.000 claims description 44
- 239000003610 charcoal Substances 0.000 claims description 34
- 239000002250 absorbent Substances 0.000 claims description 30
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 28
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 17
- JCVQKRGIASEUKR-UHFFFAOYSA-N triethoxy(phenyl)silane Chemical compound CCO[Si](OCC)(OCC)C1=CC=CC=C1 JCVQKRGIASEUKR-UHFFFAOYSA-N 0.000 claims description 16
- 238000002454 metastable transfer emission spectrometry Methods 0.000 claims description 14
- CPUDPFPXCZDNGI-UHFFFAOYSA-N triethoxy(methyl)silane Chemical compound CCO[Si](C)(OCC)OCC CPUDPFPXCZDNGI-UHFFFAOYSA-N 0.000 claims description 13
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 12
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 12
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 12
- 230000015572 biosynthetic process Effects 0.000 claims description 10
- 238000006073 displacement reaction Methods 0.000 claims description 10
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 8
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 7
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 4
- 230000002378 acidificating effect Effects 0.000 claims description 4
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 4
- 229910017604 nitric acid Inorganic materials 0.000 claims description 4
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 4
- 238000010306 acid treatment Methods 0.000 claims description 3
- NKSJNEHGWDZZQF-UHFFFAOYSA-N ethenyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)C=C NKSJNEHGWDZZQF-UHFFFAOYSA-N 0.000 claims description 3
- FFUAGWLWBBFQJT-UHFFFAOYSA-N hexamethyldisilazane Chemical compound C[Si](C)(C)N[Si](C)(C)C FFUAGWLWBBFQJT-UHFFFAOYSA-N 0.000 claims description 3
- PAFUSZAJKLNSKB-UHFFFAOYSA-N (3-iodophenyl)-trimethoxysilane Chemical compound CO[Si](OC)(OC)C1=CC=CC(I)=C1 PAFUSZAJKLNSKB-UHFFFAOYSA-N 0.000 claims description 2
- RBIILJCATVGHHI-UHFFFAOYSA-N [diethoxy(phenyl)silyl]methanamine Chemical compound NC[Si](OCC)(OCC)C1=CC=CC=C1 RBIILJCATVGHHI-UHFFFAOYSA-N 0.000 claims description 2
- YBHBEZSZXFLQMW-UHFFFAOYSA-N [dimethoxy(phenyl)silyl]methanamine Chemical compound CO[Si](CN)(OC)C1=CC=CC=C1 YBHBEZSZXFLQMW-UHFFFAOYSA-N 0.000 claims description 2
- ZZNQQQWFKKTOSD-UHFFFAOYSA-N diethoxy(diphenyl)silane Chemical compound C=1C=CC=CC=1[Si](OCC)(OCC)C1=CC=CC=C1 ZZNQQQWFKKTOSD-UHFFFAOYSA-N 0.000 claims description 2
- AHUXYBVKTIBBJW-UHFFFAOYSA-N dimethoxy(diphenyl)silane Chemical compound C=1C=CC=CC=1[Si](OC)(OC)C1=CC=CC=C1 AHUXYBVKTIBBJW-UHFFFAOYSA-N 0.000 claims description 2
- ZVJXKUWNRVOUTI-UHFFFAOYSA-N ethoxy(triphenyl)silane Chemical compound C=1C=CC=CC=1[Si](C=1C=CC=CC=1)(OCC)C1=CC=CC=C1 ZVJXKUWNRVOUTI-UHFFFAOYSA-N 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 125000000538 pentafluorophenyl group Chemical group FC1=C(F)C(F)=C(*)C(F)=C1F 0.000 claims description 2
- LFQCEHFDDXELDD-UHFFFAOYSA-N tetramethyl orthosilicate Chemical compound CO[Si](OC)(OC)OC LFQCEHFDDXELDD-UHFFFAOYSA-N 0.000 claims description 2
- QQQSFSZALRVCSZ-UHFFFAOYSA-N triethoxysilane Chemical compound CCO[SiH](OCC)OCC QQQSFSZALRVCSZ-UHFFFAOYSA-N 0.000 claims description 2
- UBMUZYGBAGFCDF-UHFFFAOYSA-N trimethoxy(2-phenylethyl)silane Chemical compound CO[Si](OC)(OC)CCC1=CC=CC=C1 UBMUZYGBAGFCDF-UHFFFAOYSA-N 0.000 claims description 2
- 238000001035 drying Methods 0.000 abstract description 10
- 239000000463 material Substances 0.000 abstract description 8
- 238000000034 method Methods 0.000 abstract description 7
- 239000003607 modifier Substances 0.000 abstract description 6
- 239000002253 acid Substances 0.000 abstract description 4
- 230000003301 hydrolyzing effect Effects 0.000 abstract 1
- 239000000376 reactant Substances 0.000 abstract 1
- 238000007792 addition Methods 0.000 description 14
- 239000000243 solution Substances 0.000 description 12
- 239000000499 gel Substances 0.000 description 9
- 239000008367 deionised water Substances 0.000 description 8
- 229910021641 deionized water Inorganic materials 0.000 description 8
- 238000010438 heat treatment Methods 0.000 description 8
- 239000011259 mixed solution Substances 0.000 description 8
- 230000000694 effects Effects 0.000 description 6
- 238000012986 modification Methods 0.000 description 5
- 230000004048 modification Effects 0.000 description 5
- 239000011148 porous material Substances 0.000 description 5
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 3
- 230000008929 regeneration Effects 0.000 description 3
- 238000011069 regeneration method Methods 0.000 description 3
- 238000003980 solgel method Methods 0.000 description 3
- 238000002336 sorption--desorption measurement Methods 0.000 description 3
- 239000003463 adsorbent Substances 0.000 description 2
- 239000008187 granular material Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- -1 MTES modified activated carbon Chemical class 0.000 description 1
- 230000002745 absorbent Effects 0.000 description 1
- 239000012814 acoustic material Substances 0.000 description 1
- 239000002156 adsorbate Substances 0.000 description 1
- 239000012670 alkaline solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- XZWYZXLIPXDOLR-UHFFFAOYSA-N metformin Chemical compound CN(C)C(=N)NC(N)=N XZWYZXLIPXDOLR-UHFFFAOYSA-N 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000007783 nanoporous material Substances 0.000 description 1
- 238000011017 operating method Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 235000019353 potassium silicate Nutrition 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000011343 solid material Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
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Abstract
The invention belongs to the field of preparation techniques of aerogel materials, and relates to a preparation method of a hydrophobic SiO2 aerogel-activated carbon composite material. The preparation method comprises the following steps: by using a silicon source as a reactant, water as a hydrolytic agent, anhydrous alcohol as a solvent and acid as a catalyst, adding a hydrophobic modifier to carry out hydrolysis at 40-60 DEG C while keeping stirring; after completely finishing hydrolysis, adding alkali to regulate the pH value, continuing stirring to initiate polycondensation reaction, adding the solution into previously weighed activated carbon, and applying ultrasonic to form a wet gel; replacing the solvent water of the wet gel with the anhydrous alcohol; and finally, drying to obtain the hydrophobic aerogel-activated carbon composite material. The aerogel composite material prepared by the method provided by the invention solves the problems of high price of aerogel and short service life of activated carbon.
Description
Technical field
The invention belongs to the preparation technology field of aerogel material, relate in particular to compound and adopt two step sol-gel processes to combine a kind of hydrophobic SiO of drying process with active carbon
2The preparation method of aeroge-absorbent charcoal composite material.
Background technology
Aeroge is a kind of typical nano-porous materials, SiO
2Specific area is high, porosity is big, and its surface polarity is controlled, can regulate its hydrophilic, hydrophobicity as required.SiO
2Aeroge is a kind of novel light nanoporous property amorphous solid-state material of controllable structure, has low-density (minimum 0.02g/cm
3), high-specific surface area (is up to 1000m
2/ g) and the high advantages such as (the highest by 99%) of porosity.Can be used as heat-barrier material, acoustic material, filtering material and sorbing material etc.Liu etc. are raw material with waterglass, and TMCS is a modifier, prepare contact angle and be 138 ° hydrophobic type SiO
2Aeroge, but aeroge is that cost is high as the adsorbent major defect.
Though active carbon is cheap and easy to get as adsorbent, shortcoming is to use the life-span short, is difficult for regeneration.
Therefore, if can combine the low cost of active carbon and the advantages such as big, the easy regeneration of specific area of aeroge to prepare the hydrophobic SiO that performance is good, low-cost, be prone to regeneration
2Aeroge modification activities charcoal composite adsorbing material will be a new trial.
Summary of the invention
The objective of the invention is provides a kind of hydrophobic SiO for the deficiency of improving prior art
2The preparation method of aeroge-absorbent charcoal composite material.
Technical scheme of the present invention is: a kind of hydrophobic SiO
2The preparation method of aeroge-absorbent charcoal composite material, its concrete steps are following:
(1) be 1 in molar ratio with silicon source, water, absolute ethyl alcohol and hydrophobically modified agent: (3～8): (10～20): mix (0.1～1), and adding is (0.001～0.01) with silicon source mol ratio: 1 acidic catalyst, stir abundant hydrolysis down at 40～60 ℃;
(2) add alkali in the solution that in step (1), obtains and regulate pH value, continue to stir and make it that polycondensation reaction take place, will make after the solution adding acid treatment in the active carbon, wherein active carbon is 0.1～1.3: 1 with silicon source quality ratio, leaves standstill the formation wet gel after ultrasonic;
(3) wet gel carries out solvent exchange with absolute ethyl alcohol; After dry, promptly make hydrophobic SiO
2Aeroge-absorbent charcoal composite material.
Silicon source described in the preferred steps (1) is methyl silicate or ethyl orthosilicate; Hydrophobically modified agent described in the preferred steps (1) is phenyl triethoxysilane (PTES); MTES (MTES); HMDS (HMDS); Trim,ethylchlorosilane (TMCS); Vinyltrimethoxy silane (VTMS); The triphenyl Ethoxysilane; Phenyl triethoxysilane; Phenyltrimethoxysila,e; The diphenyl diethoxy silane; Dimethoxydiphenylsilane; The phenethyl trimethoxy silane; Aminomethyl phenyl dimethoxy silane; The aminomethyl phenyl diethoxy silane; 3-iodophenyl trimethoxy silane or pentafluorophenyl group triethoxysilane; Acidic catalyst described in the preferred steps (1) is hydrochloric acid, acetic acid or nitric acid; Alkali described in the preferred steps (2) is ammoniacal liquor, NaOH, potassium hydroxide or sodium carbonate; Regulate the pH value between 6.5～8.Time swap described in the preferred steps (3) is 12～24h, and the displacement number of times is 3～8 times.Mixing time in preferred steps (1) and (2) is 40-70min.
Active carbon is used in acid treatment in the above-mentioned steps (2), promptly uses conventional processing method, is to clean H in the acid with acid
+The ratio of concentration and active carbon is (0.01～1) mol: 1g, uses centrifuge and separated form water then, and oven dry obtains again at last.Because active carbon has higher adsorption rate in acid solution than in alkaline solution.
The active carbon that adds in the above-mentioned steps (2), last active carbon makes hydrophobic SiO as carrier behind the gel
2Aeroge-absorbent charcoal composite material.
Beneficial effect:
Aeroge-the absorbent charcoal composite material of the present invention preparation is through two sol-gel processes step by step, the lightweight nanoporous solid material that obtains through super-dry.The inventive method and the aeroge-composite that is prepared by this method have following characteristics:
(1) technology simple controllable.The inventive method adopts two step sol-gel processes, and operating procedure is simple, and experimental situation is uncomplicated, and the course of reaction controllability is fine.
(2) hydrophobic performance is good.The inventive method and by the aeroge-absorbent charcoal composite material of this method preparation has been utilized the surface polarity controllability of aeroge, has realized better hydrophobic.
(3) can find out hydrophobic SiO by SEM
2Aeroge is wrapped in the activated carbon granule surface uniformly, and its skeleton is loose, has formed hydrophobic SiO
2Aeroge-absorbent charcoal composite material.
Description of drawings
Fig. 1 is the hydrophobic SiO of two kinds of modifier preparations in instance 1 and the instance 3
2The N of aeroge-absorbent charcoal composite material
2The adsorption-desorption isothermal curve; Fig. 1 (b) and (a) be respectively that embodiment 1 and 3 active carbon additions are the composite of 5g wherein.
Fig. 2 is prepared hydrophobic SiO in instance 5 and the instance 8
2The active carbon addition is to the influence of gel time in aeroge-absorbent charcoal composite material; Wherein
Be prepared hydrophobic SiO in the instance 5
2The active carbon addition is to the influence of gel time in aeroge-absorbent charcoal composite material,
Be prepared hydrophobic SiO in the instance 5
2The active carbon addition is to the influence of gel time in aeroge-absorbent charcoal composite material.
Fig. 3 is prepared hydrophobic SiO in instance 6 and the instance 7
2Aeroge-absorbent charcoal composite material graph of pore diameter distribution; Wherein a is the hydrophobic SiO when the active carbon addition is 5g in the instance 6
2Aeroge-absorbent charcoal composite material graph of pore diameter distribution, b are the hydrophobic SiO when the active carbon addition is 5g in the instance 7
2Aeroge-absorbent charcoal composite material graph of pore diameter distribution.
Fig. 4 is to be the hydrophobic SiO that 10g makes by MTES modified activated carbon addition in the instance 4
2The electromicroscopic photograph of aeroge-absorbent charcoal composite material.
The specific embodiment
Instance 1
With the positive quanmethyl silicate of 14.7ml, 7.2ml deionized water, 68ml absolute ethyl alcohol and 2.4ml phenyl triethoxysilane (PTES) and 0.3ml hydrochloric acid (1mol/L) as the mixed solution of catalyst 40 ℃ of heating and constantly stirring down, adding ammoniacal liquor behind the 40min, to regulate the pH value be 6.5.Continuing to stir 60min makes it that polycondensation reaction take place; With (wherein active carbon uses the hydrochloric acid of 0.77ml, 1.55ml, 3.1ml, 4.65ml, 6.2ml to clean respectively in the prior load weighted 2.5g of being respectively of solution adding, 5g, 10g, 15g, the 20g active carbon; And oven dry), leave standstill the formation wet gel after the sonicated.Wet gel carries out solvent exchange with absolute ethyl alcohol, and every 12h displacement is once replaced 3 times altogether.After drying obtains hydrophobic SiO
2Aeroge-absorbent charcoal composite material.
Modifier phenyl triethoxysilane (PTES), active carbon addition are the N of the composite of 5g preparation in this instance
2The adsorption-desorption isothermal curve is shown in Fig. 1 (b).
Instance 2
With the positive quanmethyl silicate of 14.7ml, 14.4ml deionized water, 93ml absolute ethyl alcohol and 4.8ml phenyl triethoxysilane (PTES) and 0.8ml acetic acid as the mixed solution of catalyst 50 ℃ of heating and constantly stirring down, adding NaOH behind the 60min, to regulate the pH value be 7.Continuing to stir 40min makes it that polycondensation reaction take place; With (wherein active carbon uses the hydrochloric acid of 7.7ml, 15.5ml, 31.0ml, 46.5ml, 62.0ml to clean respectively in the prior load weighted 2.5g of being respectively of solution adding, 5g, 10g, 15g, the 20g active carbon; And oven dry), leave standstill the formation wet gel after ultrasonic.Wet gel carries out solvent exchange with absolute ethyl alcohol, and every 24h displacement is once replaced 5 times altogether.After drying obtains hydrophobic SiO
2Aeroge-absorbent charcoal composite material.
With the positive quanmethyl silicate of 14.7ml, 7.2ml deionized water, 68ml absolute ethyl alcohol and 6ml MTES (MTES) and 0.5ml (1mol/L) hydrochloric acid as the mixed solution of catalyst 60 ℃ of heating and constantly stirring down, adding potassium hydroxide behind the 60min, to regulate the pH value be 7.5.Continuing to stir 60min makes it that polycondensation reaction take place; With (wherein active carbon uses the hydrochloric acid of 68ml, 135ml, 270ml, 405ml, 540ml to clean respectively in the prior load weighted 2.5g of being respectively of solution adding, 5g, 10g, 15g, the 20g active carbon; And oven dry), leave standstill the formation wet gel after ultrasonic.Wet gel carries out solvent exchange with absolute ethyl alcohol, and every 12h displacement is once replaced 8 times altogether.After drying obtains hydrophobic SiO
2Aeroge-absorbent charcoal composite material.
Modifier MTES (MTES), active carbon addition are the N of the composite of 5g preparation in this instance
2The adsorption-desorption isothermal curve is shown in Fig. 1 (a).In conjunction with Fig. 1 (b), from two figure, can find out, downward in whole pressure limit indent, N
2With the absorption of composite material surface be polymolecular layer absorption at the very start, explain that two kinds of curves all belong to III class thermoisopleth.At P/P
0Hydrophobic SiO is explained in the curve division when being 0.6 left and right sides
2Aeroge modification activities raw material of wood-charcoal material is the two ends open-celled structure; Adsorbance at low-pressure area is less, works as P/P
0Approached 1 o'clock, curve is tending towards parallel with the longitudinal axis; Relative pressure is high more, and adsorbance is many more, shows porose filling, and this is typical case's table that adsorbate condenses between solid particle.The composite adsorbance of two kinds of modifier preparations is suitable, but the absorption of PTES modification separates more obvious with the desorption ring.
Instance 4
With the positive tetraethyl orthosilicate of 22.4ml, 14.4ml deionized water, 93ml absolute ethyl alcohol and 8ml MTES (MTES) and 0.3ml nitric acid (1mol/L) as the mixed solution of catalyst 50 ℃ of heating and constantly stirring down, adding sodium carbonate behind the 50min, to regulate the pH value be 8.Continuing to stir 50min makes it that polycondensation reaction take place; With (wherein active carbon uses the hydrochloric acid of 0.77ml, 1.55ml, 3.1ml, 4.65ml, 6.2ml to clean respectively in the prior load weighted 2.5g of being respectively of solution adding, 5g, 10g, 15g, the 20g active carbon; And oven dry), leave standstill the formation wet gel after ultrasonic.Wet gel carries out solvent exchange with absolute ethyl alcohol, and every 24h displacement is once replaced 3 times altogether.After drying obtains hydrophobic SiO
2Aeroge-absorbent charcoal composite material.
Prepared active carbon addition is the hydrophobic SiO of 10g in this instance
2The electromicroscopic photograph of aeroge-absorbent charcoal composite material is as shown in Figure 4.Can find out hydrophobic SiO by figure
2Aeroge is wrapped in each activated carbon granule surface uniformly, and its skeleton is loose, forms hydrophobic type SiO
2Aeroge modification activities carbon composite.
With the positive tetraethyl orthosilicate of 22.4ml, 7.2ml deionized water, 68ml absolute ethyl alcohol and 12.1ml phenyl triethoxysilane (PTES) and 0.3ml hydrochloric acid (1mol/L) as the mixed solution of catalyst 40 ℃ of heating and constantly stirring down, adding ammoniacal liquor behind the 60min, to regulate the pH value be 6.5.Continuing to stir 60min makes it that polycondensation reaction take place; With (wherein active carbon uses the hydrochloric acid of 7.7ml, 15.5ml, 31.0ml, 46.5ml, 62.0ml to clean respectively in the prior load weighted 2.5g of being respectively of solution adding, 5g, 10g, 15g, the 20g active carbon; And oven dry), leave standstill the formation wet gel behind the ultrasonic 3min.Wet gel carries out solvent exchange with absolute ethyl alcohol, and every 12h displacement is once replaced 5 times altogether.After drying obtains hydrophobic SiO
2Aeroge-absorbent charcoal composite material.
In this instance different activities charcoal addition to the influence of composite gel time shown in
among Fig. 2.
Instance 6
With 22.4 positive tetraethyl orthosilicates, 14.4ml deionized water, 93ml absolute ethyl alcohol and 14.5ml phenyl triethoxysilane (PTES) and 0.3ml nitric acid (1mol/L) as the mixed solution of catalyst 50 ℃ of heating and constantly stirring down, adding NaOH behind the 70min, to regulate the pH value be 7.Continuing to stir 70min makes it that polycondensation reaction take place; With (wherein active carbon uses the hydrochloric acid of 7.7ml, 15.5ml, 31.0ml, 46.5ml, 62.0ml to clean respectively in the prior load weighted 2.5g of being respectively of solution adding, 5g, 10g, 15g, the 20g active carbon; And oven dry), leave standstill the formation wet gel behind the ultrasonic 5min.Wet gel carries out solvent exchange with absolute ethyl alcohol, and every 24h displacement is once replaced 8 times altogether.After drying obtains hydrophobic SiO
2Aeroge-absorbent charcoal composite material.
Hydrophobic SiO when the active carbon addition is 5g in this instance
2Aeroge-absorbent charcoal composite material graph of pore diameter distribution is shown in a among Fig. 3.
Instance 7
With the positive tetraethyl orthosilicate of 22.4ml, 7.2ml deionized water, 68ml absolute ethyl alcohol and 14.0ml MTES (MTES) and 0.3ml hydrochloric acid (1mol/L) as the mixed solution of catalyst 60 ℃ of heating and constantly stirring down, adding potassium hydroxide behind the 60min, to regulate the pH value be 7.5.Continuing to stir 60min makes it that polycondensation reaction take place; With (wherein active carbon uses the hydrochloric acid of 0.77ml, 1.55ml, 3.1ml, 4.65ml, 6.2ml to clean respectively in the prior load weighted 2.5g of being respectively of solution adding, 5g, 10g, 15g, the 20g active carbon; And oven dry), leave standstill the formation wet gel behind the ultrasonic 4min.Wet gel carries out solvent exchange with absolute ethyl alcohol, and every 12h displacement is once replaced 3 times altogether.After drying obtains hydrophobic SiO
2Aeroge-absorbent charcoal composite material.
Hydrophobic SiO when the active carbon addition is 5g in this instance
2Aeroge-absorbent charcoal composite material graph of pore diameter distribution in conjunction with a among Fig. 3 in the instance 6, can be found out hydrophobic SiO shown in b among Fig. 3
2The most probable aperture of aeroge modification activities carbon composite is respectively 18nm and 32nm, and the aperture mainly is distributed in 1-50nm.
Instance 8
With the positive tetraethyl orthosilicate of 22.4ml, 14.4ml deionized water, 93ml absolute ethyl alcohol and 16.0ml MTES (MTES) and 0.8ml acetic acid as the mixed solution of catalyst 50 ℃ of heating and constantly stirring down, adding sodium carbonate behind the 60min, to regulate the pH value be 8.Continuing to stir 60min makes it that polycondensation reaction take place; With (wherein active carbon uses the hydrochloric acid of 7.7ml, 15.5ml, 31.0ml, 46.5ml, 62.0ml to clean respectively in the prior load weighted 2.5g of being respectively of solution adding, 5g, 10g, 15g, the 20g active carbon; And oven dry), leave standstill the formation wet gel behind the ultrasonic 3-5min.Wet gel carries out solvent exchange with absolute ethyl alcohol, and every 24h displacement is once replaced 6 times altogether.After drying obtains hydrophobic SiO
2Aeroge-absorbent charcoal composite material.
Among Fig. 2
For different activities charcoal addition in the instance 8 is among Fig. 2 to the influence of composite gel time in conjunction with instance 5
Can find out that along with the increase of amounts of activated carbon, the gel time of composite reduces a little, this is owing to do not destroy hydrophobic SiO when adding a spot of active carbon
2The network of aeroge, when continuing to increase active carbon, gel solution and active carbon contact area increase is disperseed rapidly, causes gel time to reduce.
Claims (6)
1. hydrophobic SiO
2The preparation method of aeroge-absorbent charcoal composite material, its concrete steps are following:
(1) be 1 in molar ratio with silicon source, water, absolute ethyl alcohol and hydrophobically modified agent: (3～8): (10～20): mix (0.1～1), and adding and silicon source mol ratio are 0.001～0.01: 1 acidic catalyst, stirs abundant hydrolysis down at 40～60 ℃;
(2) add alkali in the solution that in step (1), obtains and regulate pH value, continue to stir and make it that polycondensation reaction take place, will make after the solution adding acid treatment in the active carbon, wherein active carbon is 0.1～1.3: 1 with silicon source quality ratio, leaves standstill the formation wet gel after ultrasonic;
(3) wet gel carries out solvent exchange with absolute ethyl alcohol; After dry, promptly make hydrophobic SiO
2Aeroge-absorbent charcoal composite material.
2. preparation method according to claim 1 is characterized in that the silicon source described in the step (1) is methyl silicate or ethyl orthosilicate.
3. preparation method according to claim 1 is characterized in that the hydrophobically modified agent described in the step (1) is phenyl triethoxysilane, MTES, HMDS, trim,ethylchlorosilane, vinyltrimethoxy silane, triphenyl Ethoxysilane, phenyl triethoxysilane, phenyltrimethoxysila,e, diphenyl diethoxy silane, dimethoxydiphenylsilane, phenethyl trimethoxy silane, aminomethyl phenyl dimethoxy silane, aminomethyl phenyl diethoxy silane, 3-iodophenyl trimethoxy silane or pentafluorophenyl group triethoxysilane.
4. preparation method according to claim 1 is characterized in that the acidic catalyst described in the step (1) is hydrochloric acid, acetic acid or nitric acid.
5. preparation method according to claim 1 is characterized in that the alkali described in the step (2) is ammoniacal liquor, NaOH, potassium hydroxide or sodium carbonate; Regulate the pH value between 6.5～8.
6. preparation method according to claim 1 is characterized in that the time swap described in the step (3) is 12～24h, and the displacement number of times is 3～8 times.
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| CN102974315A (en) * | 2012-12-10 | 2013-03-20 | 中国矿业大学 | Load type amino functional meso-porous silicon adsorbent and preparation method thereof |
| CN102989414A (en) * | 2012-11-22 | 2013-03-27 | 中国石油大学(华东) | Preparation method of super-hydrophobic active carbon modified material |
| CN103272565A (en) * | 2013-06-06 | 2013-09-04 | 北方民族大学 | Preparation method of super-hydrophobic active carbon |
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