CN106362683A - Oily water purifying agent and preparation method thereof - Google Patents
Oily water purifying agent and preparation method thereof Download PDFInfo
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- CN106362683A CN106362683A CN201610251095.3A CN201610251095A CN106362683A CN 106362683 A CN106362683 A CN 106362683A CN 201610251095 A CN201610251095 A CN 201610251095A CN 106362683 A CN106362683 A CN 106362683A
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- solution
- greasy dirt
- preparation
- normal hexane
- magnetic particle
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 69
- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- 239000012629 purifying agent Substances 0.000 title abstract 5
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims abstract description 40
- 239000004964 aerogel Substances 0.000 claims abstract description 29
- 239000002131 composite material Substances 0.000 claims abstract description 28
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims abstract description 27
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 24
- 229910052599 brucite Inorganic materials 0.000 claims abstract description 24
- 239000000835 fiber Substances 0.000 claims abstract description 23
- 239000011240 wet gel Substances 0.000 claims abstract description 22
- 238000000034 method Methods 0.000 claims abstract description 17
- 238000006073 displacement reaction Methods 0.000 claims abstract description 16
- 239000002904 solvent Substances 0.000 claims abstract description 16
- 230000032683 aging Effects 0.000 claims abstract description 8
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000012545 processing Methods 0.000 claims abstract description 3
- 239000000243 solution Substances 0.000 claims description 55
- 239000003795 chemical substances by application Substances 0.000 claims description 34
- 239000006249 magnetic particle Substances 0.000 claims description 34
- 239000002121 nanofiber Substances 0.000 claims description 31
- 150000003961 organosilicon compounds Chemical class 0.000 claims description 27
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 21
- 239000011259 mixed solution Substances 0.000 claims description 17
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 16
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 14
- 230000004048 modification Effects 0.000 claims description 11
- 238000012986 modification Methods 0.000 claims description 11
- 230000008569 process Effects 0.000 claims description 10
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 8
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 8
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- 229960000583 acetic acid Drugs 0.000 claims description 7
- 239000012362 glacial acetic acid Substances 0.000 claims description 7
- 239000011159 matrix material Substances 0.000 claims description 7
- 230000010355 oscillation Effects 0.000 claims description 7
- UQEAIHBTYFGYIE-UHFFFAOYSA-N hexamethyldisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)C UQEAIHBTYFGYIE-UHFFFAOYSA-N 0.000 claims description 6
- 229940073561 hexamethyldisiloxane Drugs 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 5
- 229910021529 ammonia Inorganic materials 0.000 claims description 4
- 238000004108 freeze drying Methods 0.000 claims description 4
- 239000002245 particle Substances 0.000 claims description 4
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims description 4
- 235000017557 sodium bicarbonate Nutrition 0.000 claims description 4
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 2
- 230000004913 activation Effects 0.000 claims description 2
- FFUAGWLWBBFQJT-UHFFFAOYSA-N hexamethyldisilazane Chemical compound C[Si](C)(C)N[Si](C)(C)C FFUAGWLWBBFQJT-UHFFFAOYSA-N 0.000 claims description 2
- 239000010936 titanium Substances 0.000 claims description 2
- 229910052719 titanium Inorganic materials 0.000 claims description 2
- 238000001035 drying Methods 0.000 abstract description 3
- 238000000746 purification Methods 0.000 abstract description 3
- 230000008901 benefit Effects 0.000 abstract description 2
- 238000002156 mixing Methods 0.000 abstract 2
- MXBCYQUALCBQIJ-RYVPXURESA-N (8s,9s,10r,13s,14s,17r)-13-ethyl-17-ethynyl-11-methylidene-1,2,3,6,7,8,9,10,12,14,15,16-dodecahydrocyclopenta[a]phenanthren-17-ol;(8r,9s,13s,14s,17r)-17-ethynyl-13-methyl-7,8,9,11,12,14,15,16-octahydro-6h-cyclopenta[a]phenanthrene-3,17-diol Chemical compound OC1=CC=C2[C@H]3CC[C@](C)([C@](CC4)(O)C#C)[C@@H]4[C@@H]3CCC2=C1.C1CC[C@@H]2[C@H]3C(=C)C[C@](CC)([C@](CC4)(O)C#C)[C@@H]4[C@@H]3CCC2=C1 MXBCYQUALCBQIJ-RYVPXURESA-N 0.000 abstract 1
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 abstract 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract 1
- 239000002253 acid Substances 0.000 abstract 1
- 239000002041 carbon nanotube Substances 0.000 abstract 1
- 229910021393 carbon nanotube Inorganic materials 0.000 abstract 1
- 239000008187 granular material Substances 0.000 abstract 1
- 239000002071 nanotube Substances 0.000 abstract 1
- 238000011084 recovery Methods 0.000 abstract 1
- 238000000926 separation method Methods 0.000 abstract 1
- 239000000499 gel Substances 0.000 description 7
- 239000003921 oil Substances 0.000 description 7
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 239000004411 aluminium Substances 0.000 description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 3
- 229910052782 aluminium Inorganic materials 0.000 description 3
- 239000010865 sewage Substances 0.000 description 3
- 238000001179 sorption measurement Methods 0.000 description 3
- 239000004408 titanium dioxide Substances 0.000 description 3
- GFLJTEHFZZNCTR-UHFFFAOYSA-N 3-prop-2-enoyloxypropyl prop-2-enoate Chemical compound C=CC(=O)OCCCOC(=O)C=C GFLJTEHFZZNCTR-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 239000000701 coagulant Substances 0.000 description 2
- 239000000945 filler Substances 0.000 description 2
- 238000005189 flocculation Methods 0.000 description 2
- 230000016615 flocculation Effects 0.000 description 2
- 229920000371 poly(diallyldimethylammonium chloride) polymer Polymers 0.000 description 2
- 229910021420 polycrystalline silicon Inorganic materials 0.000 description 2
- 239000003361 porogen Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- AHLWZBVXSWOPPL-RGYGYFBISA-N 20-deoxy-20-oxophorbol 12-myristate 13-acetate Chemical compound C([C@]1(O)C(=O)C(C)=C[C@H]1[C@@]1(O)[C@H](C)[C@H]2OC(=O)CCCCCCCCCCCCC)C(C=O)=C[C@H]1[C@H]1[C@]2(OC(C)=O)C1(C)C AHLWZBVXSWOPPL-RGYGYFBISA-N 0.000 description 1
- 229910002012 Aerosil® Inorganic materials 0.000 description 1
- ODINCKMPIJJUCX-UHFFFAOYSA-N Calcium oxide Chemical compound [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 1
- 239000005696 Diammonium phosphate Substances 0.000 description 1
- 241001602688 Pama Species 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000005708 Sodium hypochlorite Substances 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 235000019994 cava Nutrition 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000001186 cumulative effect Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- MNNHAPBLZZVQHP-UHFFFAOYSA-N diammonium hydrogen phosphate Chemical compound [NH4+].[NH4+].OP([O-])([O-])=O MNNHAPBLZZVQHP-UHFFFAOYSA-N 0.000 description 1
- 229910000388 diammonium phosphate Inorganic materials 0.000 description 1
- 235000019838 diammonium phosphate Nutrition 0.000 description 1
- YDEXUEFDPVHGHE-GGMCWBHBSA-L disodium;(2r)-3-(2-hydroxy-3-methoxyphenyl)-2-[2-methoxy-4-(3-sulfonatopropyl)phenoxy]propane-1-sulfonate Chemical compound [Na+].[Na+].COC1=CC=CC(C[C@H](CS([O-])(=O)=O)OC=2C(=CC(CCCS([O-])(=O)=O)=CC=2)OC)=C1O YDEXUEFDPVHGHE-GGMCWBHBSA-L 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000000295 fuel oil Substances 0.000 description 1
- 239000012510 hollow fiber Substances 0.000 description 1
- 239000008235 industrial water Substances 0.000 description 1
- 229910052909 inorganic silicate Inorganic materials 0.000 description 1
- 230000000813 microbial effect Effects 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical compound [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 description 1
- MZSDGDXXBZSFTG-UHFFFAOYSA-M sodium;benzenesulfonate Chemical compound [Na+].[O-]S(=O)(=O)C1=CC=CC=C1 MZSDGDXXBZSFTG-UHFFFAOYSA-M 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 239000003643 water by type Substances 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
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0211—Compounds of Ti, Zr, Hf
-
- 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
- B01J20/04—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
- B01J20/041—Oxides or hydroxides
-
- 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
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
- B01J20/205—Carbon nanostructures, e.g. nanotubes, nanohorns, nanocones, nanoballs
-
- 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
- B01J20/28002—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 physical properties
- B01J20/28009—Magnetic properties
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- 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
-
- 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
- C02F1/32—Treatment of water, waste water, or sewage by irradiation with ultraviolet light
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- Chemical & Material Sciences (AREA)
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- Chemical Kinetics & Catalysis (AREA)
- Analytical Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Dispersion Chemistry (AREA)
- Toxicology (AREA)
- Health & Medical Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Nanotechnology (AREA)
- Silicon Compounds (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention relates to the field of water purification, and discloses an oily water purifying agent and a preparation method thereof. The method comprises the following steps: mixing butyl titanate, carbon nanotubes, brucite fibers, endellite fiber nanotubes, anhydrous ethanol and toluene to prepare a solution A; mixing anhydrous ethanol, acetate acid gracial and water to prepare a solution B; dropwise adding the solution B to the solution A to prepare a sol solution; ageing the sol solution, adding anhydrous ethanol to the sol solution in order to carry out solvent displacement, adding n-hexane to the sol solution in order to carry out solvent displacement, carrying out separation to remove n-hexane in order to obtain wet gel, and hydrophobically modifying the wet gel; and drying the hydrophobically modified wet gel to prepare composite aerogel, and processing the composite aerogel to form granules or blocks in order to obtain the oily water purifying agent. The oily water purifying agent has the advantages of high oil removal efficiency, no recovery of the purifying agent, and no secondary pollution to water.
Description
Technical field
The present invention relates to Water warfare field, more particularly, to a kind of greasy dirt water scavengine agent and preparation method thereof.
Background technology
With the fast development of China's economy, at present, all in cumulative year after year, the wastewater flow rate discharged therewith is also being continuously increased for domestic consumption and industrial water consumption.In these waste water, mostly all contain greasy dirt.In order to protect increasingly destroyed environment, these oily waters are being carried out discharge front it is necessary to carry out purified treatment.Existing greasy dirt method for purifying water mainly has flocculence, physisorphtion, microbial degradation method etc..The application of wherein flocculence is relatively broad.
Chinese patent as Application No. 201310366271.4 discloses a kind of greasy dirt water scavengine agent and preparation method thereof, this greasy dirt water scavengine agent contains following component: 15～30 parts of aluminium polychlorid in terms of mass parts, 5～12 parts of PAMA, 7～16 parts of Calx, 3～10 parts of sodium hypochlorite, 3～8 parts of sodium lignin sulfonate, 3～7 parts of diammonium phosphate, 5～15 parts of benzene sulfonic acid sodium salt.The greasy dirt water scavengine agent that this invention provides has very strong flocculation, and has good bactericidal effect.
Chinese patent as Application No. 201410380852.8 discloses a kind of condensed oil sewage and processes coagulant, include following components in percentage by weight: 15.0～25.0% aluminium polychlorid, 5.0～10.0% poly- silicon zinc sulfate, 0.5～1.0% PDDA and 5.0～10.0% 3.0g polyamide-amide.Its preparation method is: by weight percentage, first aluminium polychlorid and poly- silicon zinc sulfate are added to the water, dissolving adds PDDA and 3.0g polyamide-amide completely afterwards, stirs, adjust ph value to 3.0～5.0, obtain condensed oil sewage and process coagulant.Its advantage is: consumption is few, cheap, and is applied to the handling process of multifunctional rotary flow reactor；Have rp demulsification and water purification effect concurrently, to Heavy Oil High Temperature sewage, there is good clean-up effect；Its preparation method is simple.
Although greasy dirt can be removed from water by method to a certain extent that purify oily water above by flocculence, it deoils relatively inefficient, and after flocculation, flocculent substance still easily remains in water body after filtration；And need when purifying to add in water various be dissolved in water itself and the chemical reagent that is not easily recycled, easily cause secondary pollution while deoiling.
Content of the invention
In order to solve above-mentioned technical problem, the invention provides a kind of greasy dirt water scavengine agent and preparation method thereof.This greasy dirt water scavengine agent deoils efficiency high, cleanser need not be reclaimed, and will not cause secondary pollution to water body.
The concrete technical scheme of the present invention is: a kind of greasy dirt water scavengine agent, and matrix material is the composite aerogel of titanium dioxide-CNT-brucite fiber-galapectite nanofiber pipe.
Further, described matrix material is coated with Fe 3 O 4 magnetic particle.
The preparation method of greasy dirt water scavengine agent of the present invention, comprises the following steps:
Butyl titanate, CNT, brucite fiber, galapectite nanofiber pipe, dehydrated alcohol, toluene 1:0.1-0.2:0.1-0.2:0.1-0.2:10-30:0.01-0.03 in mass ratio are mixed, obtained solution a；Dehydrated alcohol, the glacial acetic acid of 0.5-1.5mol/l are mixed with water 10-20:4-6:1 in mass ratio, obtained solution b；Supersonic oscillations process is carried out at 50-60 DEG C to solution a, solution b is added drop-wise in the solution a of 2 times of quality；Sol solutionses are obtained after stirring 1-2h.
By sol solutionses aging 24-48h at room temperature, then add dehydrated alcohol in sol solutionses and carry out solvent displacement 24-48h, then add normal hexane again in sol solutionses and carry out solvent displacement 24-48h, it is separated off normal hexane, obtain wet gel, with the mixed solution of organo-silicon compound and normal hexane, hydrophobically modified is carried out to wet gel.
Composite aerogel is obtained after being then passed through being dried, described composite aerogel is prepared into after graininess or bulk, obtains greasy dirt water scavengine agent.
Aeroge is the minimum material of the density finding in the world so far, and has the porosity of superelevation, has preferable absorption property.Wherein being most widely used of aerosil.The preparation process of aeroge is generally divided into colloidal sol preparation, gel preparation and drying steps.After prepared gel, contain a large amount of holes and three-dimensional net structure in gel, under gel state, the filling due to there being liquid supports, and its structure is relatively stable.But during gel drying is for aeroge, due to the loss of liquid, and the frame strength of gel is not high, easily caves in it is not easy to shape, after leading to become aeroge, its porosity declines.
The composite aerogel of present invention preparation, using CNT, brucite fiber, galapectite nanofiber pipe etc. is as matrix material, CNT is the tubular material of nano-scale, galapectite nanofiber pipe is the inorganic silicate hollow fiber conduit of nano-scale, brucite fiber also has nano-scale, after above-mentioned material and titanium dioxide carry out being combined, three-dimensional net structure can be played a supporting role under gel state, in dry run, its structure is not caved in, ensure that porosity, and CNT, brucite fiber, galapectite nanofiber pipe all has heat-resisting quantity, in dry run, stability is strong, after being prepared into composite aerogel simultaneously, the intensity of aeroge can be significantly increased.
In addition, because CNT, galapectite nanofiber pipe itself also have hollow structure, after being combined with titanium dioxide, the network-like cross-linked structure of complexity can be formed, the porosity of composite aerogel can't excessively be reduced, and because the hole of CNT, galapectite nanofiber pipe is specific to self structure, be not to pass through crosslinked gained the later stage, therefore stability is higher, and intensity is higher.
Because common aerogel material is that have preferably hydrophilic, accordingly act as can not playing a role very well during oil absorption material, therefore the present invention has carried out hydrophobically modified to composite aerogel, it is possible to increase efficiency of deoiling.
After composite aerogel filler oil suction reaches saturation, because titanium dioxide has efficient photocatalytic, only ultraviolet light irradiation need to be carried out it becomes possible to degrade to oil to composite aerogel filler.
Present invention also offers another kind is coated with the preparation method of the greasy dirt water scavengine agent of Fe 3 O 4 magnetic particle, comprise the following steps:
Butyl titanate, CNT, brucite fiber, galapectite nanofiber pipe, dehydrated alcohol, toluene, Fe 3 O 4 magnetic particle 1:0.1-0.2:0.1-0.2:0.1-0.2:10-30:0.01-0.03:0.02-0.04 in mass ratio are mixed, obtained solution a；Dehydrated alcohol, the glacial acetic acid of 0.5-1.5mol/l are mixed with water 10-20:4-6:1 in mass ratio, obtained solution b；Supersonic oscillations process is carried out at 50-60 DEG C to solution a, solution b is added drop-wise in the solution a of 2 times of quality；It is obtained, after stirring 1-2h, the sol solutionses being coated with Fe 3 O 4 magnetic particle；
By sol solutionses aging 24-48h at room temperature, then add dehydrated alcohol in sol solutionses and carry out solvent displacement 24-48h, then add normal hexane again in sol solutionses and carry out solvent displacement 24-48h, it is separated off normal hexane, obtain being coated with the wet gel of Fe 3 O 4 magnetic particle, with the mixed solution of organo-silicon compound and normal hexane, hydrophobically modified is carried out to wet gel；
It is obtained, after being then passed through being dried, the composite aerogel being coated with Fe 3 O 4 magnetic particle, described composite aerogel is prepared into after graininess, obtains greasy dirt water scavengine agent.
This greasy dirt water scavengine agent is designed to graininess, is coated with Fe 3 O 4 magnetic particle in its matrix material, when needing greasy dirt water scavengine agent is reclaimed, needs with magnet adsorption, more convenient.And the inventive method is just to be coated Fe 3 O 4 magnetic particle in preparing sol-process, so, when reaction forms three-dimensional net structure, Fe 3 O 4 magnetic particle is covered by wherein, carry out surrounding phase ratio with the later stage again, its covering property is more preferably, difficult for drop-off.
Further, the preparation method of described Fe 3 O 4 magnetic particle is:
The water of 100 weight portions is added in container, and leads to nitrogen 15-25min at 55-65 DEG C；By 0.5-0.55 weight portion fecl3·6h2O and 0.19-0.20 weight portion fecl2·4h2O is dissolved in the water of 10 weight portions, it is added to after logical nitrogen in described container, it is adjusted to 9-10 with ammonia ph, after reaction 10-15min, generate Fe 3 O 4 magnetic particle, hold Fe 3 O 4 magnetic particle with Magnet across chamber wall, after pouring out liquid, after Fe 3 O 4 magnetic particle is cleaned, carry out vacuum lyophilization.
Further, during preparing composite aerogel, when solution a is added drop-wise in solution b, add the sodium bicarbonate of 0.02-0.03 times that quality is solution a in solution a simultaneously.The effect of sodium bicarbonate is as toluene, it is as porogen, but both pore principles are different, cooperate the different types of hole that can make, hole containing three kinds of different origins therefore in this composite aerogel: the hole that hole that aeroge is cross-linked to form, CNT, the tubulus of galapectite nanofiber pipe itself, porogen are made, these three pore-sizes differ, therefore, it is possible to form difference in size alienation, for different greasy dirts, respective adsorption efficiency is also different, therefore, it is possible to improve the overall oil absorbing effect of composite aerogel.
Further, described CNT, brucite fiber, galapectite nanofiber pipe are respectively through activation processing: CNT or brucite fiber or galapectite nanofiber pipe be impregnated in the 10wt% hydrochloric acid solution of 150-250 times of quality, and carry out water-bath vibration 1-2h at a temperature of 50-60 DEG C；After CNT or brucite fiber or galapectite nanofiber pipe are taken out and clean, calcine 2-5h at a temperature of 400-500 DEG C.CNT after overactivation, brucite fiber, galapectite nanofiber pipe not only have higher intensity, and CNT and galapectite nanofiber pipe have more preferable adsorption activity.
Further, described CNT, the particle diameter of galapectite nanofiber pipe are 400-800nm.
Further, solution b is to the rate of addition 0.5-1.5ml/s of solution a.Need the strict rate of addition controlling solution b, under this speed, form the network-like structure that colloidal sol can form high-crosslinking-degree, improve intensity on the premise of ensureing porosity.
Further, during hydrophobically modified, in the mixed solution of described organo-silicon compound and normal hexane, organo-silicon compound are 1-2:5 with the volume ratio of normal hexane, and organo-silicon compound are 100:10-20 with the mixed solution of normal hexane and the mass ratio of wet gel；Modification temperature is 50-60 DEG C, modification time 36-50h；Described organo-silicon compound are selected from hexamethyl disiloxane, hexamethyldisiloxane, HMDS, MTMS, trim,ethylchlorosilane.
It is compared with the prior art, the invention has the beneficial effects as follows: the greasy dirt water scavengine agent of the present invention deoils efficiency high, cleanser need not be reclaimed, and will not cause secondary pollution to water body.
Specific embodiment
With reference to embodiment, the invention will be further described.
Embodiment 1
A kind of preparation method of greasy dirt water scavengine agent, comprises the following steps:
Butyl titanate, CNT, brucite fiber, galapectite nanofiber pipe, dehydrated alcohol, toluene 1:0.15:0.15:0.15:20:0.02 in mass ratio are mixed, obtained solution a；Dehydrated alcohol, the glacial acetic acid of 1mol/l are mixed with water 15:5:1 in mass ratio, obtained solution b；Supersonic oscillations process is carried out at 55 DEG C to solution a, solution b is added drop-wise in the solution a of 2 times of quality with the speed of 1ml/s；Add the sodium bicarbonate of 0.025 times that quality is solution a simultaneously in solution a, after stirring 1.5h, sol solutionses are obtained.Described CNT, the particle diameter of galapectite nanofiber pipe are 400-800nm
By sol solutionses aging 36h at room temperature, in sol solutionses, then add dehydrated alcohol carry out solvent displacement 36h, then add normal hexane again in sol solutionses and carry out solvent displacement 36h, be separated off normal hexane, obtain wet gel.With the mixed solution of organo-silicon compound and normal hexane, hydrophobically modified is carried out to wet gel, in the mixed solution of described organo-silicon compound and normal hexane, organo-silicon compound are 1.5:5 with the volume ratio of normal hexane, and organo-silicon compound are 100:15 with the mixed solution of normal hexane and the mass ratio of wet gel；Modification temperature is 55 DEG C, modification time 43h.Described organo-silicon compound are hexamethyl disiloxane.
Composite aerogel is obtained after being then passed through being dried, described composite aerogel is prepared into after bulk, obtains greasy dirt water scavengine agent.
Embodiment 2
A kind of preparation method of greasy dirt water scavengine agent, comprises the following steps:
CNT, brucite fiber, galapectite nanofiber pipe be impregnated in the 10wt% hydrochloric acid solution of 200 times of quality respectively, and carry out water-bath vibration 1.5h at a temperature of 55 DEG C；After CNT, brucite fiber, galapectite nanofiber pipe are taken out respectively and clean, calcine 3.5h at a temperature of 450 DEG C.
The water of 100 weight portions is added in container, and leads to nitrogen 20min at 60 DEG C；By 0.525 weight portion fecl3·6h2O and 0.195 weight portion fecl2·4h2O is dissolved in the water of 10 weight portions, it is added to after logical nitrogen in described container, it is adjusted to 9-10 with ammonia ph, after reaction 12.5min, generate Fe 3 O 4 magnetic particle, hold Fe 3 O 4 magnetic particle with Magnet across chamber wall, after pouring out liquid, after Fe 3 O 4 magnetic particle is cleaned, carry out vacuum lyophilization.
Butyl titanate, CNT, brucite fiber, galapectite nanofiber pipe, dehydrated alcohol, toluene, Fe 3 O 4 magnetic particle 1:0.1:0.1:0.1:10:0.01:0.02 in mass ratio are mixed, obtained solution a；Dehydrated alcohol, the glacial acetic acid of 0.5mol/l are mixed with water 10:4:1 in mass ratio, obtained solution b；Supersonic oscillations process is carried out at 50 DEG C to solution a, solution b is added drop-wise in the solution a of 2 times of quality；It is obtained, after stirring 1h, the sol solutionses being coated with Fe 3 O 4 magnetic particle；
By sol solutionses aging 24h at room temperature, in sol solutionses, then add dehydrated alcohol carry out solvent displacement 24h, then add normal hexane again in sol solutionses and carry out solvent displacement 24h, be separated off normal hexane, obtain wet gel.With the mixed solution of organo-silicon compound and normal hexane, hydrophobically modified is carried out to wet gel, in the mixed solution of described organo-silicon compound and normal hexane, organo-silicon compound are 1:5 with the volume ratio of normal hexane, and organo-silicon compound are 100:10 with the mixed solution of normal hexane and the mass ratio of wet gel；Modification temperature is 50 DEG C, modification time 36h.Described organo-silicon compound are hexamethyldisiloxane.
It is obtained, after being then passed through being dried, the composite aerogel being coated with Fe 3 O 4 magnetic particle, described composite aerogel is prepared into after graininess, obtains greasy dirt water scavengine agent.
Embodiment 3
A kind of preparation method of greasy dirt water scavengine agent, comprises the following steps:
CNT, brucite fiber, galapectite nanofiber pipe be impregnated in the 10wt% hydrochloric acid solution of 250 times of quality respectively, and carry out water-bath vibration 1h at a temperature of 60 DEG C；After CNT, brucite fiber, galapectite nanofiber pipe are taken out respectively and clean, calcine 2h at a temperature of 500 DEG C.Described CNT, the particle diameter of galapectite nanofiber pipe are 400-800nm
The water of 100 weight portions is added in container, and leads to nitrogen 15min at 65 DEG C；By 0.55 weight portion fecl3·6h2O and 0.20 weight portion fecl2·4h2O is dissolved in the water of 10 weight portions, it is added to after logical nitrogen in described container, it is adjusted to 9-10 with ammonia ph, after reaction 15min, generate Fe 3 O 4 magnetic particle, hold Fe 3 O 4 magnetic particle with Magnet across chamber wall, after pouring out liquid, after Fe 3 O 4 magnetic particle is cleaned, carry out vacuum lyophilization.
Butyl titanate, CNT, brucite fiber, galapectite nanofiber pipe, dehydrated alcohol, toluene, Fe 3 O 4 magnetic particle 1:0.2:0.2:0.2:30:0.03:0.04 in mass ratio are mixed, obtained solution a；Dehydrated alcohol, the glacial acetic acid of 1.5mol/l are mixed with water 20:6:1 in mass ratio, obtained solution b；Supersonic oscillations process is carried out at 60 DEG C to solution a, solution b is added drop-wise in the solution a of 2 times of quality；It is obtained, after stirring 1h, the sol solutionses being coated with Fe 3 O 4 magnetic particle；
By sol solutionses aging 48h at room temperature, in sol solutionses, then add dehydrated alcohol carry out solvent displacement 48h, then add normal hexane again in sol solutionses and carry out solvent displacement 48h, be separated off normal hexane, obtain wet gel.With the mixed solution of organo-silicon compound and normal hexane, hydrophobically modified is carried out to wet gel, in the mixed solution of described organo-silicon compound and normal hexane, organo-silicon compound are 2:5 with the volume ratio of normal hexane, and organo-silicon compound are 100:20 with the mixed solution of normal hexane and the mass ratio of wet gel；Modification temperature is 60 DEG C, modification time 36h.Described organo-silicon compound are MTMS.
It is obtained, after being then passed through being dried, the composite aerogel being coated with Fe 3 O 4 magnetic particle, described composite aerogel is prepared into after graininess, obtains greasy dirt water scavengine agent.
The greasy dirt water scavengine agent that embodiment 1-3 is obtained, its matrix porosity can reach 92-96%, and specific surface area reaches 500-600 m2/ g, density reaches 3.5-5kg/m3.After oily water being purified using it, after purification, water quality oil content can control within 3.0mg/l.
Raw materials used in the present invention, equipment, unless otherwise noted, is conventional raw material, the equipment of this area；Method therefor in the present invention, unless otherwise noted, is the conventional method of this area.
The above, be only presently preferred embodiments of the present invention, not the present invention imposed any restrictions, every any simple modification, change and equivalent transformation substantially above example made according to the technology of the present invention, all still falls within the protection domain of technical solution of the present invention.
Claims (10)
1. a kind of greasy dirt water scavengine agent it is characterised in that: matrix material be titanium dioxide-CNT-brucite fiber-galapectite nanofiber pipe composite aerogel.
2. as claimed in claim 1 a kind of greasy dirt water scavengine agent it is characterised in that: Fe 3 O 4 magnetic particle is coated with described matrix material.
3. as claimed in claim 1 a kind of preparation method of greasy dirt water scavengine agent it is characterised in that comprising the following steps:
Butyl titanate, CNT, brucite fiber, galapectite nanofiber pipe, dehydrated alcohol, toluene 1:0.1-0.2:0.1-0.2:0.1-0.2:10-30:0.01-0.03 in mass ratio are mixed, obtained solution a；Dehydrated alcohol, the glacial acetic acid of 0.5-1.5mol/l are mixed with water 10-20:4-6:1 in mass ratio, obtained solution b；Supersonic oscillations process is carried out at 50-60 DEG C to solution a, solution b is added drop-wise in the solution a of 2 times of quality；Sol solutionses are obtained after stirring 1-2h；
By sol solutionses aging 24-48h at room temperature, then add dehydrated alcohol in sol solutionses and carry out solvent displacement 24-48h, then add normal hexane again in sol solutionses and carry out solvent displacement 24-48h, it is separated off normal hexane, obtain wet gel, with the mixed solution of organo-silicon compound and normal hexane, hydrophobically modified is carried out to wet gel；
Composite aerogel is obtained after being then passed through being dried, described composite aerogel is prepared into after graininess or bulk, obtains greasy dirt water scavengine agent.
4. as claimed in claim 2 a kind of preparation method of greasy dirt water scavengine agent it is characterised in that comprising the following steps:
Butyl titanate, CNT, brucite fiber, galapectite nanofiber pipe, dehydrated alcohol, toluene, Fe 3 O 4 magnetic particle 1:0.1-0.2:0.1-0.2:0.1-0.2:10-30:0.01-0.03:0.02-0.04 in mass ratio are mixed, obtained solution a；Dehydrated alcohol, the glacial acetic acid of 0.5-1.5mol/l are mixed with water 10-20:4-6:1 in mass ratio, obtained solution b；Supersonic oscillations process is carried out at 50-60 DEG C to solution a, solution b is added drop-wise in the solution a of 2 times of quality；It is obtained, after stirring 1-2h, the sol solutionses being coated with Fe 3 O 4 magnetic particle；
By sol solutionses aging 24-48h at room temperature, then add dehydrated alcohol in sol solutionses and carry out solvent displacement 24-48h, then add normal hexane again in sol solutionses and carry out solvent displacement 24-48h, it is separated off normal hexane, obtain being coated with the wet gel of Fe 3 O 4 magnetic particle, with the mixed solution of organo-silicon compound and normal hexane, hydrophobically modified is carried out to wet gel；
It is obtained, after being then passed through being dried, the composite aerogel being coated with Fe 3 O 4 magnetic particle, described composite aerogel is prepared into after graininess, obtains greasy dirt water scavengine agent.
5. as claimed in claim 4 a kind of preparation method of greasy dirt water scavengine agent it is characterised in that the preparation method of described Fe 3 O 4 magnetic particle is:
The water of 100 weight portions is added in container, and leads to nitrogen 15-25min at 55-65 DEG C；By 0.5-0.55 weight portion fecl3·6h2O and 0.19-0.20 weight portion fecl2·4h2O is dissolved in the water of 10 weight portions, it is added to after logical nitrogen in described container, it is adjusted to 9-10 with ammonia ph, after reaction 10-15min, generate Fe 3 O 4 magnetic particle, hold Fe 3 O 4 magnetic particle with Magnet across chamber wall, after pouring out liquid, after Fe 3 O 4 magnetic particle is cleaned, carry out vacuum lyophilization.
6. a kind of preparation method of the greasy dirt water scavengine agent as described in claim 3 or 4 is it is characterised in that during preparing composite aerogel, when solution a is added drop-wise in solution b, add the sodium bicarbonate of 0.02-0.03 times that quality is solution a simultaneously in solution a.
7. the preparation method of a kind of greasy dirt water scavengine agent as described in claim 3 or 4, it is characterized in that, described CNT, brucite fiber, galapectite nanofiber pipe are respectively through activation processing: CNT or brucite fiber or galapectite nanofiber pipe be impregnated in the 10wt% hydrochloric acid solution of 150-250 times of quality, and carry out water-bath vibration 1-2h at a temperature of 50-60 DEG C；After CNT or brucite fiber or galapectite nanofiber pipe are taken out and clean, calcine 2-5h at a temperature of 400-500 DEG C.
8. as claimed in claim 7 a kind of preparation method of greasy dirt water scavengine agent it is characterised in that described CNT, galapectite nanofiber pipe particle diameter be 400-800nm.
9. a kind of greasy dirt water scavengine agent as described in claim 3 or 4 preparation method it is characterised in that rate of addition 0.5-1.5ml/s from solution b to solution a.
10. the preparation method of a kind of greasy dirt water scavengine agent as described in claim 3 or 4, it is characterized in that, during hydrophobically modified, in the mixed solution of described organo-silicon compound and normal hexane, organo-silicon compound are 1-2:5 with the volume ratio of normal hexane, and organo-silicon compound are 100:10-20 with the mixed solution of normal hexane and the mass ratio of wet gel；Modification temperature is 50-60 DEG C, modification time 36-50h；Described organo-silicon compound are selected from hexamethyl disiloxane, hexamethyldisiloxane, HMDS, MTMS, trim,ethylchlorosilane.
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