CN105854817A - Silver-loaded nanometer titanium dioxide aerogel material used for adsorbing and degrading petroleum hydrocarbons and preparation method thereof - Google Patents
Silver-loaded nanometer titanium dioxide aerogel material used for adsorbing and degrading petroleum hydrocarbons and preparation method thereof Download PDFInfo
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- CN105854817A CN105854817A CN201610173209.7A CN201610173209A CN105854817A CN 105854817 A CN105854817 A CN 105854817A CN 201610173209 A CN201610173209 A CN 201610173209A CN 105854817 A CN105854817 A CN 105854817A
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- 239000000463 material Substances 0.000 title claims abstract description 55
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 51
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 48
- 239000004332 silver Substances 0.000 title claims abstract description 48
- 229910052709 silver Inorganic materials 0.000 title claims abstract description 48
- 239000004964 aerogel Substances 0.000 title claims abstract description 45
- 239000004408 titanium dioxide Substances 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 229930195733 hydrocarbon Natural products 0.000 title abstract description 4
- 150000002430 hydrocarbons Chemical class 0.000 title abstract description 4
- 239000003208 petroleum Substances 0.000 title abstract description 4
- 230000000593 degrading effect Effects 0.000 title abstract 2
- 239000000843 powder Substances 0.000 claims abstract description 40
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims abstract description 33
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 28
- 230000015556 catabolic process Effects 0.000 claims abstract description 21
- 238000006731 degradation reaction Methods 0.000 claims abstract description 21
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 19
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 18
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims abstract description 15
- 230000002209 hydrophobic effect Effects 0.000 claims abstract description 13
- 229960000583 acetic acid Drugs 0.000 claims abstract description 9
- 230000032683 aging Effects 0.000 claims abstract description 9
- 239000012362 glacial acetic acid Substances 0.000 claims abstract description 8
- 238000006073 displacement reaction Methods 0.000 claims abstract description 7
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims abstract description 7
- 235000017557 sodium bicarbonate Nutrition 0.000 claims abstract description 7
- 239000002904 solvent Substances 0.000 claims abstract description 7
- 238000012986 modification Methods 0.000 claims abstract description 6
- 230000004048 modification Effects 0.000 claims abstract description 6
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000000243 solution Substances 0.000 claims description 118
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 70
- 150000003961 organosilicon compounds Chemical class 0.000 claims description 29
- 239000003209 petroleum derivative Substances 0.000 claims description 23
- 238000010521 absorption reaction Methods 0.000 claims description 21
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 claims description 20
- 239000007788 liquid Substances 0.000 claims description 19
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 18
- 239000011259 mixed solution Substances 0.000 claims description 18
- 229940084030 carboxymethylcellulose calcium Drugs 0.000 claims description 15
- 238000000034 method Methods 0.000 claims description 15
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 12
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 10
- 238000005406 washing Methods 0.000 claims description 10
- 230000008569 process Effects 0.000 claims description 8
- 238000013019 agitation Methods 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 6
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 6
- 229910000033 sodium borohydride Inorganic materials 0.000 claims description 6
- 239000012279 sodium borohydride Substances 0.000 claims description 6
- 239000000126 substance Substances 0.000 claims description 6
- 238000001291 vacuum drying Methods 0.000 claims description 6
- FFUAGWLWBBFQJT-UHFFFAOYSA-N hexamethyldisilazane Chemical compound C[Si](C)(C)N[Si](C)(C)C FFUAGWLWBBFQJT-UHFFFAOYSA-N 0.000 claims description 5
- 238000001802 infusion Methods 0.000 claims description 5
- 239000011159 matrix material Substances 0.000 claims description 5
- 230000010355 oscillation Effects 0.000 claims description 5
- 239000002131 composite material Substances 0.000 claims description 3
- UQEAIHBTYFGYIE-UHFFFAOYSA-N hexamethyldisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)C UQEAIHBTYFGYIE-UHFFFAOYSA-N 0.000 claims description 3
- 229910052719 titanium Inorganic materials 0.000 claims description 3
- 239000010936 titanium Substances 0.000 claims description 3
- 230000001699 photocatalysis Effects 0.000 abstract description 5
- 238000007146 photocatalysis Methods 0.000 abstract description 5
- 238000001179 sorption measurement Methods 0.000 abstract description 5
- 239000013535 sea water Substances 0.000 abstract description 2
- 229920002134 Carboxymethyl cellulose Polymers 0.000 abstract 1
- 239000001768 carboxy methyl cellulose Substances 0.000 abstract 1
- 235000010948 carboxy methyl cellulose Nutrition 0.000 abstract 1
- 239000008112 carboxymethyl-cellulose Substances 0.000 abstract 1
- 238000001035 drying Methods 0.000 abstract 1
- 239000003921 oil Substances 0.000 description 19
- 239000000499 gel Substances 0.000 description 16
- 239000011347 resin Substances 0.000 description 13
- 229920005989 resin Polymers 0.000 description 13
- 239000000203 mixture Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 230000008961 swelling Effects 0.000 description 3
- MYRTYDVEIRVNKP-UHFFFAOYSA-N 1,2-Divinylbenzene Chemical group C=CC1=CC=CC=C1C=C MYRTYDVEIRVNKP-UHFFFAOYSA-N 0.000 description 2
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000018109 developmental process Effects 0.000 description 2
- 239000004088 foaming agent Substances 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- OZAIFHULBGXAKX-UHFFFAOYSA-N 2-(2-cyanopropan-2-yldiazenyl)-2-methylpropanenitrile Chemical compound N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 description 1
- 108010010803 Gelatin Proteins 0.000 description 1
- 239000005062 Polybutadiene Substances 0.000 description 1
- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- 239000008346 aqueous phase Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- CQEYYJKEWSMYFG-UHFFFAOYSA-N butyl acrylate Chemical compound CCCCOC(=O)C=C CQEYYJKEWSMYFG-UHFFFAOYSA-N 0.000 description 1
- VTYYLEPIZMXCLO-UHFFFAOYSA-L calcium carbonate Substances [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000005238 degreasing Methods 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 239000003599 detergent Substances 0.000 description 1
- 125000003438 dodecyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- 229920001971 elastomer Polymers 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000007667 floating Methods 0.000 description 1
- 230000006870 function Effects 0.000 description 1
- 239000008273 gelatin Substances 0.000 description 1
- 229920000159 gelatin Polymers 0.000 description 1
- 235000019322 gelatine Nutrition 0.000 description 1
- 235000011852 gelatine desserts Nutrition 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 229920002857 polybutadiene Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 230000035935 pregnancy Effects 0.000 description 1
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 1
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 239000005060 rubber Substances 0.000 description 1
- 238000007614 solvation Methods 0.000 description 1
- 230000002522 swelling effect Effects 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 238000003911 water pollution Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- 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
- B01J20/24—Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- 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
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- 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
- B01J20/12—Naturally occurring clays or bleaching earth
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
- B01J20/28047—Gels
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/06—Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
- B01J21/063—Titanium; Oxides or hydroxides thereof
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/26—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24
- B01J31/38—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24 of titanium, zirconium or hafnium
-
- B01J35/23—
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/288—Treatment of water, waste water, or sewage by sorption using composite sorbents, e.g. coated, impregnated, multi-layered
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/32—Hydrocarbons, e.g. oil
Abstract
The invention discloses a silver-loaded nanometer titanium dioxide aerogel material used for adsorbing and degrading petroleum hydrocarbons and a preparation method thereof, belonging to the field of seawater treatment. The preparation method comprises the following steps: a, preparing a solution A frombutyl titanate, endellite powder, hydrophobic porous carboxymethyl cellulose, absolute ethyl alcohol and toluene, preparing a solution B from absolute ethyl alcohol, glacial acetic acid and water, adding the solution B into the solution A drop by drop and adding sodium bicarbonate into the solution A so as to prepare a sol solution; b, loading the sol solution with silver so as to prepare a silver-loaded sol solution; and c, ageing the silver-loaded sol solution, carrying out solvent displacement on the silver-loaded sol solution so as to obtain silver-loaded gel, subjecting the silver-loaded gel to hydrophobic modification and drying the silver-loaded gel in vacuum so as to prepare the aerogel material. The aerogel material prepared in the invention can carry out adsorption and degradation on petroleum hydrocarbons under photocatalysis; and the aerogel material has the advantages of light weight, good strength, high porosity, great oil adsorption capacity and a fast oil adsorption rate.
Description
Technical field
The present invention relates to seawater and administer field, particularly relate to a kind of Ag-carried nanometer titanium dioxide gas for absorption degradation petroleum hydrocarbon
Gel rubber material and preparation method thereof.
Background technology
Coming in the past few decades, the fast development of the industry of China, national life level also improves constantly, but, along with industry
Development, industry the most increasingly severe to the pollution of environment.In recent years, the environmental consciousness of people is gradually strengthened, and government is for ring
Border is administered and is the most increasingly paid attention to.
In numerous pollution sources, water pollution problems is especially prominent, and wherein, the leakage of industry oil and discharge are to ocean, river
Cause huge pollution, the serious threat to environment structure.
At present, the oil in water body is adsorbed by general employing oil absorption material, and at most use is high oil-absorbing resin.High oil suction
Resin is the polymer that lipophile is monomer crosslinked, and intermolecular have three-dimensional crosslinked network shape structure, by Intramolecular oil base
The solvation of segment and oil molecule makes resin generation swelling action.Owing to high oil-absorbing resin can only occur swelling without dissolving,
Therefore oil molecule will be carried in tridimensional network, it is achieved high oil-absorbing resin oil suction and the function of guarantor's oil.
The Chinese patent of Application No. CN201510692238.X discloses a kind of high oil-absorbing resin and preparation method thereof, this height
Oil-absorbing resin includes following raw material in parts by weight: oil phase is divinylbenzene 4～8 parts, styrene 20～30 parts, propylene
Acid lauryl 20～30 parts, butyl acrylate 20～30 parts, butadiene rubber 20～30 parts, azodiisobutyronitrile 3～9 parts, toluene
40～50 parts；Aqueous phase is polyvinyl alcohol 5～9 parts, gelatin 10～20 parts, NaCl5～8 parts, CaCO35～10 parts, deionized water
500～600 parts.
But high oil-absorbing resin there is also certain weak point, such as due to the porosity of high oil-absorbing resin is the most sufficiently high,
Therefore the capacity of the oil suction of the high oil-absorbing resin of unit mass also receives certain restriction, and swelling rate is the fastest.This
Outward, the density of high oil-absorbing resin is higher, and the resin of unit volume is heavier, the most not readily transportable, collection etc..The most key
It is that oil product can only be adsorbed by high oil-absorbing resin by physical action, but oil product can not be degraded by it, it is still necessary to after recovery etc.
Oil product processes, not only inconvenient, too increases cost.
Summary of the invention
In order to solve above-mentioned technical problem, the invention provides a kind of Ag-carried nanometer titanium dioxide for absorption degradation petroleum hydrocarbon
Aerogel material and preparation method thereof.Aerogel material prepared by the present invention, can adsorb also petroleum hydrocarbon under photocatalysis
Degraded, and this aerogel material light weight, intensity is good, and porosity is high, and absorbency capacity is big, and swelling rate is fast.
The concrete technical scheme of the present invention is: a kind of Ag-carried nanometer titanium dioxide aeroge material for absorption degradation petroleum hydrocarbon
Material, the matrix of described aerogel material is titanium dioxide-galapectite-hydrophobic porous carboxymethylcellulose calcium composite, and aeroge
It is loaded with Nano Silver on the matrix of material.
The preparation method of the above-mentioned Ag-carried nanometer titanium dioxide aerogel material for absorption degradation petroleum hydrocarbon, including following step
Rapid:
A, by butyl titanate, galapectite powder, hydrophobic porous carboxymethylcellulose calcium, absolute ethyl alcohol, toluene in mass ratio
1:0.1～0.3:0.05～0.15:10～30:0.01～0.03 mixes, obtained solution A；Ice by absolute ethyl alcohol, 0.5～1.5mol/L
Acetic acid mixes with water in mass ratio 10～20:4～6:1, obtained solution B；Solution A is carried out at 50～60 DEG C ultrasonic wave shake
Swing process, solution B is added drop-wise in the solution A of 2 times of quality；Add quality in solution A is the 0.01～0.02 of solution A simultaneously
Sodium bicarbonate powder again, after continuing stirring 1～2h, prepares sol solutions.
B, in sol solutions, add quality be butyl titanate 0.1～the silver nitrate of 0.3 times and stir, then in sol solutions
Sol solutions, until the pH of sol solutions is 5, is heated to 45～55 DEG C under the conditions of lucifuge and is incubated 1～2h by dropping salpeter solution, right
After sol solutions washes unreacting substance with water, adding quality under agitation in sol solutions is butyl titanate 0.005～0.015
Sodium borohydride again, is simultaneously added dropwise sodium hydroxide solution and controls sol solutions pH between 7～8；Prepare after finally washing with water and carry
Silver sol liquid.
C, general carry silver sol liquid the most aging 24～48h, then add n-hexane in load silver sol liquid and carry out solvent displacement
36～60h, it is separated off n-hexane, obtains carrying silver gel, with the mixed solution of organo-silicon compound and n-hexane to carrying silver gel
Carry out hydrophobically modified, at 60～120 DEG C, finally after vacuum drying, prepare aerogel material.
Although traditional aerogel material has the highest porosity, but high just because of its porosity, cause its intensity relatively
Low, skeleton is particularly easy to cave in, it is not easy to shape；And when being used as oil absorption material, need long-time on the water surface, under illumination
Floating, the most aging and cause performance to reduce, therefore practicality is relatively low.The aerogel material of technical solution of the present invention, uses two
The composite of titanium oxide-galapectite-hydrophobic porous carboxymethylcellulose calcium is as matrix skeleton, and galapectite is Nano/micron size
Inorfil pipe, hydrophobic porous carboxymethylcellulose calcium can be commercially available prod or to voluntarily porous carboxymethylcellulose calcium being carried out hydrophobic changing
Property.Hydrophobic porous carboxymethylcellulose calcium has excellent adhesive property, by above-mentioned both be doped with titanium dioxide and together to prepare
After becoming aerogel material, it is possible to the intensity of aerogel material and ageing-resistant degree are significantly increased, increase the service life.And difficult energy
Valuable, owing to galapectite self also has the hollow tubular structure of Nano/micron size, with hydrophobic porous carboxymethylcellulose calcium,
After titanium dioxide is together combined, it is possible to form complicated network-like cross-linked structure, can't too much affect the porosity of aeroge,
And owing to the hole of galapectite is specific to self structure, not by crosslinking gained, therefore intensity is higher.
Titanium dioxide can carry out catalytic degradation to petroleum hydrocarbon under photocatalysis, thus water body realizes degreasing, it is not necessary to follow-up right
Greasy dirt memory post-processes.
In step a, toluene and sodium acid carbonate are as pore-foaming agent, it is possible to pore in the preparation process of sol solutions, both
Pore principle is different, and cooperate the more hole that can make, and therefore contains the hole of three kinds of different origins in this aerogel material
Gap: the hole that hole that aeroge is cross-linked to form, the tubulus of galapectite self, pore-foaming agent are made, these three pore-size differs,
Therefore, it is possible to form difference in size alienation, for different petroleum hydrocarbons, respective adsorption efficiency is the most different, therefore, it is possible to improve airsetting
The overall oil absorbing effect of glue material.
In stepb, aerogel material has been carried out carrying silver by the inventive method, and the method can improve aerogel material to silver
Load fastness, and load capacity is high.After carrying out carrying silver, Nano Silver coordinates titanium dioxide, it is possible to improve aeroge material further
The photocatalysis effect of material, thus improve the degradation efficiency to petroleum hydrocarbon.
Owing to the aerogel material of the present invention is the detergent as water body, it is therefore desirable to have preferable lipophile,
Can realize petroleum hydrocarbon is fully absorbed, and need to avoid causing because of water suction content volume to be occupied.Therefore in step c,
The inventive method has carried out hydrophobically modified to aerogel material.
As preferably, described galapectite powder through modification, method of modifying is: by galapectite powder infusion in 100～200
In the 10wt% hydrochloric acid solution of times quality, and at a temperature of 50～60 DEG C, carry out water-bath vibration 1～2h；Galapectite powder is taken out also
After Xi Jinging, the Muffle furnace of 400～500 DEG C is calcined 2～5h, finally prepares modified galapectite powder.Through modified Ai Luo
Stone powder, in modifying process, eliminates the crystallization water of inside, has opened up greatly its internal capacity, had higher adsorption activity and suction
Attached capacity.
As preferably, the particle diameter of described galapectite powder is 800～1000nm.The hollow tube of the galapectite powder of this size with
After in aerogel material, other two kinds of holes coordinate, it is possible to increase the overall oil absorption of aerogel material.
As preferably, butyl titanate described in step a, galapectite powder, hydrophobic porous carboxymethylcellulose calcium, absolute ethyl alcohol,
The mass ratio of toluene is 1:0.2:0.1:20:0.02；Described absolute ethyl alcohol, glacial acetic acid are 15:5:1 with the mass ratio of water.
As preferably, in step a, solution B is to the rate of addition 0.5～1.5mL/s of solution A.Need strictly to control solution B
Rate of addition, form colloidal sol under this speed and can form the network-like structure of high-crosslinking-degree, carry on the premise of ensureing porosity
High intensity.
As preferably, organo-silicon compound described in step c are with the mixed solution of n-hexane, and organo-silicon compound are with just own
The volume ratio of alkane is 1～2:5, and organo-silicon compound are 100:10～20 with the mixed solution of n-hexane and the mass ratio of load silver gel.
As preferably, organo-silicon compound described in step c are selected from HMDO, HMDS, pregnancy
Base disilazane, MTMS, trim,ethylchlorosilane.
As preferably, the hydrophobically modified in step c, temperature is 40～60 DEG C, and modification time is 24～48h.
It is compared with the prior art, the invention has the beneficial effects as follows: aerogel material prepared by the present invention, can under photocatalysis
Petroleum hydrocarbon is adsorbed and degrades, and this aerogel material light weight, intensity is good, and porosity is high, and absorbency capacity is big, oil suction speed
Rate is fast.
Detailed description of the invention
Below in conjunction with embodiment, the invention will be further described.
Embodiment 1
A kind of Ag-carried nanometer titanium dioxide aerogel material for absorption degradation petroleum hydrocarbon, its preparation method is as follows:
A, selection particle diameter are 800～1000nm, and purity galapectite powder more than 98%, by galapectite powder infusion in 150 times of matter
In the 10wt% hydrochloric acid solution of amount, and at a temperature of 55 DEG C, carry out water-bath vibration 1.5h；After galapectite powder is taken out and cleans,
In the Muffle furnace of 450 DEG C, calcine 3.5h, finally prepare modified galapectite powder.
By butyl titanate, modified galapectite powder, hydrophobic porous carboxymethylcellulose calcium, absolute ethyl alcohol, toluene in mass ratio
1:0.2:0.1:20:0.02 mix, obtained solution A；By absolute ethyl alcohol, glacial acetic acid and the water 15:5:1 in mass ratio of 1mol/L
Mix, obtained solution B；Solution A is carried out supersonic oscillations process at 55 DEG C, solution B is added drop-wise to 2 times of quality
Solution A in, control solution B rate of addition 1mL/s.In solution A, interpolation quality is 0.015 times of solution A simultaneously
Sodium bicarbonate powder, continue stirring 1.5h after, prepare sol solutions.
B, in sol solutions add quality be the silver nitrate of butyl titanate 0.2 times and stir, then in sol solutions drip
Sol solutions, until the pH of sol solutions is 5, is heated to 50 DEG C under the conditions of lucifuge and is incubated 1.5h, to sol solutions by salpeter solution
After washing unreacting substance with water, in sol solutions, add the sodium borohydride that quality is butyl titanate 0.01 times under agitation,
It is simultaneously added dropwise sodium hydroxide solution and controls sol solutions pH between 7～8；Prepare after finally washing with water and carry silver sol liquid.
C, the most aging 36h of silver sol liquid will be carried, and then silver sol liquid adds n-hexane carry out solvent displacement 48h to carrying,
It is separated off n-hexane, obtains carrying silver gel, with the mixed solution of organo-silicon compound and n-hexane to carrying silver gel at 50 DEG C
Carry out in the mixed solution of hydrophobically modified 36h, described organo-silicon compound and n-hexane, organo-silicon compound and the body of n-hexane
Long-pending ratio is 1.5:5, and organo-silicon compound and the mixed solution of n-hexane are 100:15 with the mass ratio of load silver gel.Described organosilicon
Compound is HMDO.At 90 DEG C, finally after vacuum drying, prepare aerogel material.
Embodiment 2
A kind of Ag-carried nanometer titanium dioxide aerogel material for absorption degradation petroleum hydrocarbon, its preparation method is as follows:
A, selection particle diameter are 800～1000nm, and purity galapectite powder more than 98%, by galapectite powder infusion in 100 times of matter
In the 10wt% hydrochloric acid solution of amount, and at a temperature of 50 DEG C, carry out water-bath vibration 2h；After galapectite powder is taken out and cleans,
The Muffle furnace of 400 DEG C is calcined 5h, finally prepares modified galapectite powder.
By butyl titanate, modified galapectite powder, hydrophobic porous carboxymethylcellulose calcium, absolute ethyl alcohol, toluene in mass ratio
1:0.1:0.05:10:0.01 mix, obtained solution A；By absolute ethyl alcohol, glacial acetic acid and the water 10:4:1 in mass ratio of 0.5mol/L
Mix, obtained solution B；Solution A is carried out supersonic oscillations process at 50 DEG C, solution B is added drop-wise to 2 times of quality
Solution A in, control solution B rate of addition 0.5mL/s.Add quality in solution A is the 0.01 of solution A simultaneously
Sodium bicarbonate powder again, after continuing stirring 1h, prepares sol solutions.
B, in sol solutions add quality be the silver nitrate of butyl titanate 0.1 times and stir, then in sol solutions drip
Sol solutions, until the pH of sol solutions is 5, is heated to 45 DEG C under the conditions of lucifuge and is incubated 2h by salpeter solution, uses sol solutions
After unreacting substance is removed in washing, in sol solutions, add the sodium borohydride that quality is butyl titanate 0.005 times under agitation,
It is simultaneously added dropwise sodium hydroxide solution and controls sol solutions pH between 7～8；Prepare after finally washing with water and carry silver sol liquid.
C, the most aging 24h of silver sol liquid will be carried, and then silver sol liquid adds n-hexane carry out solvent displacement 36h to carrying,
It is separated off n-hexane, obtains carrying silver gel, with the mixed solution of organo-silicon compound and n-hexane to carrying silver gel at 40 DEG C
Carry out in the mixed solution of hydrophobically modified 48h, described organo-silicon compound and n-hexane, organo-silicon compound and the body of n-hexane
Long-pending ratio is 1:5, and organo-silicon compound and the mixed solution of n-hexane are 100:10 with the mass ratio of load silver gel.Described siliconated
Compound is HMDS.At 60 DEG C, finally after vacuum drying, prepare aerogel material.
Embodiment 3
A kind of Ag-carried nanometer titanium dioxide aerogel material for absorption degradation petroleum hydrocarbon, its preparation method is as follows:
A, selection particle diameter are 800～1000nm, and purity galapectite powder more than 98%, by galapectite powder infusion in 200 times of matter
In the 10wt% hydrochloric acid solution of amount, and at a temperature of 60 DEG C, carry out water-bath vibration 1h；After galapectite powder is taken out and cleans,
The Muffle furnace of 500 DEG C is calcined 2h, finally prepares modified galapectite powder.
By butyl titanate, modified galapectite powder, hydrophobic porous carboxymethylcellulose calcium, absolute ethyl alcohol, toluene in mass ratio 1:
0.3:0.15:30:0.03 mixes, obtained solution A；By absolute ethyl alcohol, glacial acetic acid and the water 20:6:1 in mass ratio of 1.5mol/L
Mix, obtained solution B；Solution A is carried out supersonic oscillations process at 60 DEG C, solution B is added drop-wise to 2 times of quality
Solution A in, control solution B rate of addition 1.5mL/s.Add quality in solution A is the 0.02 of solution A simultaneously
Sodium bicarbonate powder again, after continuing stirring 2h, prepares sol solutions.
B, in sol solutions add quality be the silver nitrate of butyl titanate 0.3 times and stir, then in sol solutions drip
Sol solutions, until the pH of sol solutions is 5, is heated to 55 DEG C under the conditions of lucifuge and is incubated 1h by salpeter solution, uses sol solutions
After unreacting substance is removed in washing, in sol solutions, add the sodium borohydride that quality is butyl titanate 0.015 times under agitation,
It is simultaneously added dropwise sodium hydroxide solution and controls sol solutions pH between 7～8；Prepare after finally washing with water and carry silver sol liquid.
C, the most aging 48h of silver sol liquid will be carried, and then silver sol liquid adds n-hexane carry out solvent displacement 60h to carrying,
It is separated off n-hexane, obtains carrying silver gel, with the mixed solution of organo-silicon compound and n-hexane to carrying silver gel at 60 DEG C
Carry out in the mixed solution of hydrophobically modified 24h, described organo-silicon compound and n-hexane, organo-silicon compound and the body of n-hexane
Long-pending ratio is 2:5, and organo-silicon compound and the mixed solution of n-hexane are 100:20 with the mass ratio of load silver gel.Described organosilicon
Compound is MTMS.At 120 DEG C, finally after vacuum drying, prepare aerogel material.
Embodiment 4
A kind of Ag-carried nanometer titanium dioxide aerogel material for absorption degradation petroleum hydrocarbon, its preparation method is as follows:
A, selection particle diameter are 800～1000nm, and purity galapectite powder more than 98% by butyl titanate, galapectite powder, is dredged
Water porous carboxymethylcellulose calcium, absolute ethyl alcohol, toluene 1:0.2:0.1:20:0.02 in mass ratio mix, obtained solution A；Will
Absolute ethyl alcohol, the glacial acetic acid of 1mol/L mix with water 15:5:1 in mass ratio, obtained solution B；To solution A at 55 DEG C
Carry out supersonic oscillations process, solution B is added drop-wise in the solution A of 2 times of quality, control the rate of addition 1mL/s of solution B.
In solution A, add the sodium bicarbonate powder of 0.015 times that quality is solution A simultaneously, after continuing stirring 1.5h, prepare colloidal sol
Liquid.
B, in sol solutions add quality be the silver nitrate of butyl titanate 0.2 times and stir, then in sol solutions drip
Sol solutions, until the pH of sol solutions is 5, is heated to 50 DEG C under the conditions of lucifuge and is incubated 1.5h, to sol solutions by salpeter solution
After washing unreacting substance with water, in sol solutions, add the sodium borohydride that quality is butyl titanate 0.01 times under agitation,
It is simultaneously added dropwise sodium hydroxide solution and controls sol solutions pH between 7～8；Prepare after finally washing with water and carry silver sol liquid.
C, the most aging 36h of silver sol liquid will be carried, and then silver sol liquid adds n-hexane carry out solvent displacement 48h to carrying,
It is separated off n-hexane, obtains carrying silver gel, with the mixed solution of organo-silicon compound and n-hexane to carrying silver gel at 50 DEG C
Carry out in the mixed solution of hydrophobically modified 36h, described organo-silicon compound and n-hexane, organo-silicon compound and the body of n-hexane
Long-pending ratio is 1.5:5, and organo-silicon compound and the mixed solution of n-hexane are 100:15 with the mass ratio of load silver gel.Described organosilicon
Compound is isopyknic HMDS and trim,ethylchlorosilane.At 100 DEG C, finally after vacuum drying, prepare aeroge
Material.
The performance of the aerogel material that embodiment 1～4 prepares is as shown in the table:
| Porosity | Specific surface area | Density | Oil suction multiplying power | Tensile strength | |
| Embodiment 1 | 95% | 563m2/g | 3.68kg/m3 | 14 | 25.2Gpa |
| Embodiment 2 | 91% | 537m2/g | 4.04kg/m3 | 12 | 20.3GPa |
| Embodiment 3 | 92% | 519m2/g | 4.28kg/m3 | 11 | 22.7GPa |
| Embodiment 4 | 90% | 445m2/g | 4.51kg/m3 | 10 | 21.2GPa |
Raw materials used, equipment in the present invention, unless otherwise noted, is the conventional raw material of this area, equipment；Side used in the present invention
Method, unless otherwise noted, is the conventional method of this area.
The above, be only presently preferred embodiments of the present invention, not impose any restrictions the present invention, every according to skill of the present invention
Any simple modification, change and the equivalent transformation that above example is made by art essence, all still falls within technical solution of the present invention
Protection domain.
Claims (9)
1. the Ag-carried nanometer titanium dioxide aerogel material for absorption degradation petroleum hydrocarbon, it is characterized in that: the matrix of described aerogel material is titanium dioxide-galapectite-hydrophobic porous carboxymethylcellulose calcium composite, and is loaded with Nano Silver on the matrix of aerogel material.
The preparation method of a kind of Ag-carried nanometer titanium dioxide aerogel material for absorption degradation petroleum hydrocarbon, it is characterised in that comprise the following steps:
A, butyl titanate, galapectite powder, hydrophobic porous carboxymethylcellulose calcium, absolute ethyl alcohol, toluene 1:0.1 ~ 0.3:0.05 in mass ratio ~ 0.15:10 ~ 30:0.01 ~ 0.03 are mixed, obtained solution A；The glacial acetic acid of absolute ethyl alcohol, 0.5 ~ 1.5mol/L is mixed with water 10 ~ 20:4 in mass ratio ~ 6:1, obtained solution B；Solution A is carried out supersonic oscillations process at 50 ~ 60 DEG C, solution B is added drop-wise in the solution A of 2 times of quality；In solution A, add the sodium bicarbonate powder of 0.01 ~ 0.02 times that quality is solution A simultaneously, after continuing stirring 1 ~ 2h, prepare sol solutions；
B, in sol solutions add quality be the silver nitrate of butyl titanate 0.1 ~ 0.3 times and stir, then in sol solutions, salpeter solution is dripped until the pH of sol solutions is 5, under the conditions of lucifuge, sol solutions is heated to 45 ~ 55 DEG C and is incubated 1 ~ 2h, after sol solutions is washed with water unreacting substance, in sol solutions, add the sodium borohydride that quality is butyl titanate 0.005 ~ 0.015 times under agitation, be simultaneously added dropwise sodium hydroxide solution and control sol solutions pH between 7 ~ 8；Prepare after finally washing with water and carry silver sol liquid；
C, general carry the most aging 24 ~ 48h of silver sol liquid, then in load silver sol liquid, add n-hexane carry out solvent displacement 36 ~ 60h, it is separated off n-hexane, obtain carrying silver gel, carry out hydrophobically modified with the mixed solution of organo-silicon compound with n-hexane to carrying silver gel, at 60 ~ 120 DEG C, finally after vacuum drying, prepare aerogel material.
A kind of preparation method of the Ag-carried nanometer titanium dioxide aerogel material for absorption degradation petroleum hydrocarbon, it is characterized in that, described galapectite powder is through modification, method of modifying is: by galapectite powder infusion in the 10wt% hydrochloric acid solution of 100 ~ 200 times of quality, and carries out water-bath vibration 1 ~ 2h at a temperature of 50 ~ 60 DEG C；After galapectite powder is taken out and cleans, the Muffle furnace of 400 ~ 500 DEG C is calcined 2 ~ 5h, finally prepares modified galapectite powder.
The preparation method of a kind of Ag-carried nanometer titanium dioxide aerogel material for absorption degradation petroleum hydrocarbon, it is characterised in that the particle diameter of described galapectite powder is 800 ~ 1000nm.
A kind of preparation method of the Ag-carried nanometer titanium dioxide aerogel material for absorption degradation petroleum hydrocarbon, it is characterized in that, butyl titanate described in step a, galapectite powder, hydrophobic porous carboxymethylcellulose calcium, absolute ethyl alcohol, the mass ratio of toluene are 1:0.2:0.1:20:0.02；Described absolute ethyl alcohol, glacial acetic acid are 15:5:1 with the mass ratio of water.
The preparation method of a kind of Ag-carried nanometer titanium dioxide aerogel material for absorption degradation petroleum hydrocarbon, it is characterised in that in step a, solution B is to the rate of addition 0.5 ~ 1.5mL/s of solution A.
A kind of preparation method of the Ag-carried nanometer titanium dioxide aerogel material for absorption degradation petroleum hydrocarbon, it is characterized in that, in the mixed solution of organo-silicon compound described in step c and n-hexane, organo-silicon compound are 1 ~ 2:5 with the volume ratio of n-hexane, and organo-silicon compound are 100:10 ~ 20 with the mixed solution of n-hexane and the mass ratio of load silver gel.
A kind of preparation method of the Ag-carried nanometer titanium dioxide aerogel material for absorption degradation petroleum hydrocarbon, it is characterized in that, organo-silicon compound described in step c are selected from HMDO, HMDS, HMDS, MTMS, trim,ethylchlorosilane.
The preparation method of a kind of Ag-carried nanometer titanium dioxide aerogel material for absorption degradation petroleum hydrocarbon, it is characterised in that the hydrophobically modified in step c, temperature is 40 ~ 60 DEG C, and modification time is 24 ~ 48h.
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