CN106824086A - A kind of carbosphere Quito point loads the preparation method of heterogeneous structure material - Google Patents
A kind of carbosphere Quito point loads the preparation method of heterogeneous structure material Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 39
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 24
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000008367 deionised water Substances 0.000 claims abstract description 18
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 18
- 238000013019 agitation Methods 0.000 claims abstract description 16
- 239000012065 filter cake Substances 0.000 claims abstract description 15
- 239000000047 product Substances 0.000 claims abstract description 14
- PNZVFASWDSMJER-UHFFFAOYSA-N acetic acid;lead Chemical compound [Pb].CC(O)=O PNZVFASWDSMJER-UHFFFAOYSA-N 0.000 claims abstract description 9
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims abstract description 7
- 239000008103 glucose Substances 0.000 claims abstract description 7
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 7
- 239000007787 solid Substances 0.000 claims abstract description 7
- 239000012043 crude product Substances 0.000 claims abstract description 6
- 239000012467 final product Substances 0.000 claims abstract description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 5
- 235000015393 sodium molybdate Nutrition 0.000 claims abstract description 5
- 239000011684 sodium molybdate Substances 0.000 claims abstract description 5
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 claims abstract description 5
- 238000005119 centrifugation Methods 0.000 claims abstract description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 22
- 238000005406 washing Methods 0.000 claims description 11
- 238000001035 drying Methods 0.000 claims description 10
- XJUNRGGMKUAPAP-UHFFFAOYSA-N dioxido(dioxo)molybdenum;lead(2+) Chemical compound [Pb+2].[O-][Mo]([O-])(=O)=O XJUNRGGMKUAPAP-UHFFFAOYSA-N 0.000 claims description 7
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical group OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 6
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 claims description 2
- 239000003814 drug Substances 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 239000002904 solvent Substances 0.000 claims description 2
- 239000000243 solution Substances 0.000 abstract description 12
- 238000010531 catalytic reduction reaction Methods 0.000 abstract description 10
- 238000000034 method Methods 0.000 abstract description 10
- 230000001699 photocatalysis Effects 0.000 abstract description 10
- 238000010521 absorption reaction Methods 0.000 abstract description 8
- 230000008569 process Effects 0.000 abstract description 6
- 229910001385 heavy metal Inorganic materials 0.000 abstract description 5
- 239000007864 aqueous solution Substances 0.000 abstract description 4
- 230000002079 cooperative effect Effects 0.000 abstract description 4
- 238000005516 engineering process Methods 0.000 abstract description 3
- 150000002500 ions Chemical class 0.000 abstract description 3
- 230000009467 reduction Effects 0.000 abstract description 3
- 238000006722 reduction reaction Methods 0.000 abstract description 3
- 239000005416 organic matter Substances 0.000 abstract description 2
- 239000006185 dispersion Substances 0.000 abstract 1
- 229910052770 Uranium Inorganic materials 0.000 description 19
- JFALSRSLKYAFGM-UHFFFAOYSA-N uranium(0) Chemical compound [U] JFALSRSLKYAFGM-UHFFFAOYSA-N 0.000 description 19
- 239000002105 nanoparticle Substances 0.000 description 8
- 238000011282 treatment Methods 0.000 description 6
- 239000002351 wastewater Substances 0.000 description 5
- 239000012153 distilled water Substances 0.000 description 4
- 239000013535 sea water Substances 0.000 description 4
- 239000002915 spent fuel radioactive waste Substances 0.000 description 4
- 239000003758 nuclear fuel Substances 0.000 description 3
- 230000000717 retained effect Effects 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- AAORDHMTTHGXCV-UHFFFAOYSA-N uranium(6+) Chemical compound [U+6] AAORDHMTTHGXCV-UHFFFAOYSA-N 0.000 description 3
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical class [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 230000008878 coupling Effects 0.000 description 2
- 238000010168 coupling process Methods 0.000 description 2
- 238000005859 coupling reaction Methods 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 238000005272 metallurgy Methods 0.000 description 2
- 238000005065 mining Methods 0.000 description 2
- 238000007146 photocatalysis Methods 0.000 description 2
- 238000007711 solidification Methods 0.000 description 2
- 230000008023 solidification Effects 0.000 description 2
- 208000019155 Radiation injury Diseases 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000009388 chemical precipitation Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 231100000045 chemical toxicity Toxicity 0.000 description 1
- 239000011258 core-shell material Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 230000002068 genetic effect Effects 0.000 description 1
- 230000003760 hair shine Effects 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 238000012805 post-processing Methods 0.000 description 1
- 238000003904 radioactive pollution Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000004083 survival effect Effects 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
Classifications
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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
- B01J20/02—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
-
- 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
- B01J20/0218—Compounds of Cr, Mo, W
-
- 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
- B01J20/0251—Compounds of Si, Ge, Sn, Pb
- B01J20/0255—Compounds of Pb
-
- 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
- B01J20/28016—Particle form
- B01J20/28021—Hollow particles, e.g. hollow spheres, microspheres or cenospheres
-
- 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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/24—Chromium, molybdenum or tungsten
- B01J23/28—Molybdenum
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- B01J35/39—
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- 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
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
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- 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
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- 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
- C02F1/70—Treatment of water, waste water, or sewage by reduction
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- G—PHYSICS
- G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
- G21F—PROTECTION AGAINST X-RADIATION, GAMMA RADIATION, CORPUSCULAR RADIATION OR PARTICLE BOMBARDMENT; TREATING RADIOACTIVELY CONTAMINATED MATERIAL; DECONTAMINATION ARRANGEMENTS THEREFOR
- G21F9/00—Treating radioactively contaminated material; Decontamination arrangements therefor
- G21F9/04—Treating liquids
- G21F9/06—Processing
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- G—PHYSICS
- G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
- G21F—PROTECTION AGAINST X-RADIATION, GAMMA RADIATION, CORPUSCULAR RADIATION OR PARTICLE BOMBARDMENT; TREATING RADIOACTIVELY CONTAMINATED MATERIAL; DECONTAMINATION ARRANGEMENTS THEREFOR
- G21F9/00—Treating radioactively contaminated material; Decontamination arrangements therefor
- G21F9/04—Treating liquids
- G21F9/06—Processing
- G21F9/12—Processing by absorption; by adsorption; by ion-exchange
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- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4806—Sorbents characterised by the starting material used for their preparation the starting material being of inorganic character
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- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
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- C—CHEMISTRY; METALLURGY
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- 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
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- C02F2101/20—Heavy metals or heavy metal compounds
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- 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
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- 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
- C02F2101/308—Dyes; Colorants; Fluorescent agents
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
Abstract
The invention belongs to new material technology field, it is related to a kind of carbosphere Quito point to load the preparation method of heterogeneous structure material, with glucose as carbon source, hydro-thermal method prepares carbosphere, in gained carbosphere dispersion acetic acid lead solution, magnetic agitation；Then solid matter centrifugation, obtains filter cake；Filter cake absolute ethyl alcohol and deionized water respectively washed once；Washed product is distributed in sodium molybdate solution, magnetic agitation；Gained crude product is separated, washs and dried, and obtains final product target product carbosphere Quito point load heterogeneous structure material.Carbosphere Quito point load heterogeneous structure material present invention obtains process is simple, preparation condition gently, with absorption and photo catalytic reduction cooperative effect, the organic matter that can be used in the aqueous solution, heavy metal ion reduction.
Description
Technical field
The invention belongs to ecological environment material nd preparing technical field, and in particular to a kind of carbosphere Quito point loads hetero-junctions
The preparation method of structure material.
Background technology
Environment and the basis that the energy is that the mankind depend on for existence and development.
With the quickening of mankind's modernization, the development of nuclear energy is increasingly paid attention to by numerous countries.According to the world
The data of nuclear energy association, end on January 1st, 2016, and in fortune nuclear-power reactor totally 439, total installed capacity amounts to 38.25 ten thousand million in the whole world
Watt, 66, reactor is being built, up to 7.03 ten thousand megawatts, the proposed nuclear-power reactor that sets is 158, and installed capacity is for installed capacity
17.92 ten thousand megawatts.China also clearly proposes the policy for greatly developing nuclear power, it is contemplated that to the year two thousand twenty, China's nuclear power installed capacity
The proportion for accounting for gross generation will bring up to 7% or so from current less than 2%.Nuclear undertaking is developed rapidly, to nuclear fuel
Supply capacity and spentnuclear fuel disposal ability bring huge challenge.
Uranium is both the main component of nuclear fuel and one of the Key radioactivity nucleic of spentnuclear fuel post processing.From spentnuclear fuel
SEPARATION OF URANIUM, can both make full use of limited uranium resource, and subsequent treatment difficulty can be reduced again, reduce treatment disposal costs.This
Outward, exploration, exploitation, smelting etc. relate to uranium operating process can all produce uranium-containing waste water, may cause environmental pollution.If uranium is in environment
In largely accumulate, as the heavy metal for having chemical toxicity and radiotoxicity concurrently, radioactivity background may be changed, cause species
Genetic distortion, the survival and development to the mankind constitute potential threat.Further, since nuclear power fast development, the sharp increase of uranium demand,
Uranium resource not enough problem in land is put in face of people.And the uranium content very abundant in seawater, up to 4,500,000,000 tons, be known
About 4500 times of land uranium ore reserves, seawater is likely to become the main source of necessary for human nuclear fuel uranium in future.
Therefore, separated from water body, be enriched with, solidification and recovery uranium have very important realistic meaning.Many times,
Uranium in the aqueous solution is with sexavalence form (UO2 2+) exist, current people mostly using chemical precipitation, absorption, extraction, it is biological prosthetic,
Hyperfiltration etc. is processed.Absorption method therein is efficient, direct, technical maturity, is widely used in the treatment of heavy metal wastewater thereby.Closely
Over 20 years, photo catalytic reduction treatment uranium (VI) solution also serves as a class simply and the method for economy is widely studied, and it is not
Can only solve the problems, such as its radioactive pollution environment, but also radionuclide in spentnuclear fuel last handling process can be controlled
Valence state, so as to realize the solidification of uranium resource, reclaim.So, one class of development has the new way of absorption and photo catalytic reduction uranium (VI) concurrently
Footpath is by with important academic significance, Social benefit and economic benefit.
Used as a carbon material that class preparation cost is low, preparation method is various, it has carbosphere to the uranium (VI) in the aqueous solution
Particularly preferred suction-operated and certain selectivity, and be based on carbosphere prepare multiple spot load semiconductor nanoparticle form heterogeneous
Structural material, the nano particle for simply introducing semiconductor in the multiple spot position of carbosphere forms heterojunction structure, most of exposed
Position can still play good suction-operated, and the treated object concentration of relative enrichment is provided for photocatalysis；Treated object is urged by light
After change effect, concentration reduction can adsorb more treated objects again, so as to the coupling for reaching absorption and photocatalysis increases
By force.The rare open report of this technology.Therefore, the preparation that a kind of carbosphere Quito point loads heterogeneous structure material is researched and developed
Method has important scientific meaning and realistic meaning.
The content of the invention
It is to solve above technical problem, it is an object of the invention to provide a kind of process is simple, preparation condition is gentle, have
Carbosphere Quito point of absorption and photo catalytic reduction cooperative effect loads the preparation method of heterogeneous structure material.
What the object of the invention was realized in：A kind of carbosphere Quito point loads the preparation method of heterogeneous structure material, its
It is critical only that and carry out in accordance with the following steps：
Step 1：With glucose as carbon source, hydro-thermal method prepares carbosphere；
Step 2：Prepare acetic acid lead solution；
Step 3：Step 1 gained carbosphere is distributed in the made acetic acid lead solution of step 2, magnetic agitation；
Step 4：By the solid matter centrifugation in step 3, filter cake is obtained；
Step 5：Filter cake absolute ethyl alcohol and deionized water in step 4 respectively washed once；
Step 6：The washed product that will be obtained in step 5 is distributed in sodium molybdate solution, magnetic agitation；
Step 7：Step 6 gained crude product is separated, wash and is dried, obtain final product the point load of target product carbosphere Quito different
Structural material material.
It is pure that the purity of medicine glucose and lead molybdate described in above-mentioned steps 1~2 is not less than chemistry.
Solution solvent for use is ethylene glycol and deionized water mixture in step 2 above.
The magnetic agitation time in above-mentioned steps 3 is not less than 10 hours.
The consumption of absolute ethyl alcohol and deionized water is not less than 20 times of filter cake volume respectively in above-mentioned steps 5.
The magnetic agitation time is not less than 10 minutes in above-mentioned steps 6.
After solid matter is separated in above-mentioned steps 7, alternately washed using deionized water, absolute ethyl alcohol, acetone, after drying i.e.
Obtain carbosphere Quito point load heterogeneous structure material.
Deionized water in above-mentioned steps 7, absolute ethyl alcohol, acetone consumption respectively with washing filter cake be mark, go from
Sub- water, absolute ethyl alcohol, acetone are 20: 20: 20: 1 with the mass ratio of washing filter cake.
In above-mentioned steps 7, alternately washing times are 3~6 times；The drying temperature be 60~80 DEG C, drying time be 4~
8h。
In step 2 above, the concentration of acetic acid lead solution is 0.1M.
The beneficial effects of the present invention are：
1st, the present invention is realized based on " a core multiple spot " novelty heterojunction structure between carbosphere and semiconductor nanoparticle, and
There is provided the preparation method of this novel structure, for the multi-functional coupling of ecological environment material nd provides a kind of new thinking.This
The multiple spot load heterogeneous structure material of invention is different from core shell structure, is introduced while carbosphere good dispersiveness is retained and partly led
The photo catalytic reduction of body nano particle, absorption and photo catalytic reduction are mutually promoted.
2nd, it is reaction raw materials that the present invention uses simple common chemicals, does not produce poisonous by-product in preparation process
Thing, environmental pollution is small, is a kind of environment-friendly type synthesis technique.
3rd, products obtained therefrom strong applicability of the present invention, the particularly organic matter that can be used in the aqueous solution, heavy metal ion, uranium
Etc. (VI) absorption and photocatalytic degradation (reduction).
In brief, present invention process is simple, and whole preparation system easily builds, easy to operate, and condition is easily-controllable, low cost
Honest and clean, target product has the superperformances such as adsorptivity, photo catalytic reduction, absorption-photo catalytic reduction cooperative effect, can be used to contaminate
The ecological environment treatments such as material waste water, effluent containing heavy metal ions, effluent from uranium mining and metallurgy and seawater extract the fields such as uranium (VI).
Brief description of the drawings
Fig. 1 show the hetero-junctions that lead molybdate nano particle multiple spot load carbosphere obtained in the embodiment of the present invention is formed
Structure material XRD；
Fig. 2 show the TEM figures of embodiment of the present invention products therefrom.
Specific embodiment
Embodiment 1：
(1) prepared by carbosphere：0.1g cetyl trimethylammonium bromides and 3g glucose are weighed respectively, are dissolved in 37.5ml
In distilled water, magnetic agitation is transferred in 50ml hydrothermal reaction kettles after 30 minutes, and hydrothermal reaction kettle is placed in baking oven, 160
20 hours are incubated at DEG C, are alternately washed 6 times with distilled water, absolute ethyl alcohol and acetone after being cooled to room temperature, retained after drying after supplying
It is continuous to use.
(2) take 60mg carbospheres to be scattered in the acetic acid lead solution of 20mL0.1M, magnetic agitation 20 hours, centrifugal filtration is solid
Body material, respectively be washed once with absolute ethyl alcohol and deionized water respectively, and material after washing is scattered in the sodium molybdate of 10mL0.1M
In solution, magnetic agitation obtains crude product after 10 minutes, crude product is separated, wash and is dried, and obtains final product target product carbosphere base
Lead molybdate nano particle multiple spot loads heterogeneous structure material.
Fig. 1 show the embodiment of the present invention and carbosphere base lead molybdate nano particle multiple spot load heterogeneous structure material is obtained
XRD, gained peak is the diffraction maximum of Crystals of Lead Molybdate.The transmission electron microscope (TEM) that Fig. 2 show the present embodiment product shines
Piece, photo display products therefrom is spherical heterostructures structure material.
Embodiment 2：
(1) prepared by carbosphere：0.1g cetyl trimethylammonium bromides and 3g glucose are weighed respectively, are dissolved in 37.5ml
In distilled water, magnetic agitation is transferred in 50ml hydrothermal reaction kettles after 30 minutes, and hydrothermal reaction kettle is placed in baking oven, 160
20 hours are incubated at DEG C, are alternately washed 6 times with distilled water, absolute ethyl alcohol and acetone after being cooled to room temperature, retained after drying after supplying
It is continuous to use.
(2) take 60mg carbospheres to be scattered in the acetic acid lead solution of 20mL0.1M, magnetic agitation 10 hours, centrifugal filtration is solid
Body material, respectively washed once with absolute ethyl alcohol and deionized water respectively, and the consumption of absolute ethyl alcohol and deionized water is not less than respectively
20 times of filter cake volume；Material after washing is scattered in the sodium molybdate solution of 10mL0.1M, magnetic agitation is obtained slightly after 10 minutes
Product, crude product is alternately washed using deionized water, absolute ethyl alcohol, acetone, deionized water, absolute ethyl alcohol, the consumption of acetone
Respectively with washing filter cake be mark, deionized water, absolute ethyl alcohol, acetone are 20: 20: 20 with the mass ratio of washing filter cake:
1, alternately washing times are 3~6 times；Dry, drying temperature is 60~80 DEG C, and drying time is 4~8h, obtains final product target product carbon
Microballoon base lead molybdate nano particle multiple spot loads heterogeneous structure material.
Present invention process is simple, and whole preparation system easily builds, easy to operate, and condition is easily-controllable, with low cost, and target is produced
Thing has the superperformances such as adsorptivity, photo catalytic reduction, absorption-photo catalytic reduction cooperative effect, can be used for waste water from dyestuff, weight
The ecological environment treatments such as metal ion waste water, effluent from uranium mining and metallurgy and seawater extract the fields such as uranium.
Although embodiments of the invention are had been presented for herein, it will be appreciated by those of skill in the art that not taking off
In the case of spirit of the invention, the embodiments herein can be changed.Above-described embodiment be it is exemplary, should not be with
The embodiments herein as interest field of the present invention restriction.
Claims (10)
1. a kind of carbosphere Quito point loads the preparation method of heterogeneous structure material, it is characterised in that carry out in accordance with the following steps：
Step 1：With glucose as carbon source, hydro-thermal method prepares carbosphere；
Step 2：Prepare acetic acid lead solution；
Step 3：Step 1 gained carbosphere is distributed in the made acetic acid lead solution of step 2, magnetic agitation；
Step 4：By the solid matter centrifugation in step 3, filter cake is obtained；
Step 5：Filter cake absolute ethyl alcohol and deionized water in step 4 respectively washed once；
Step 6：The washed product that will be obtained in step 5 is distributed in sodium molybdate solution, magnetic agitation；
Step 7：Step 6 gained crude product is separated, wash and is dried, obtain final product target product carbosphere Quito point load hetero-junctions
Structure material.
2. a kind of carbosphere Quito point according to claim 1 loads the preparation method of heterogeneous structure material, and its feature exists
In：It is pure that the purity of medicine glucose and lead molybdate described in step 1~2 is not less than chemistry.
3. a kind of carbosphere Quito point according to claim 1 loads the preparation method of heterogeneous structure material, and its feature exists
In：Solution solvent for use is ethylene glycol and deionized water mixture in the step 2.
4. a kind of carbosphere Quito point as claimed in claim 1 loads the preparation method of heterogeneous structure material, it is characterised in that：
The magnetic agitation time in the step 3 is not less than 10 hours.
5. a kind of carbosphere Quito point as claimed in claim 1 loads the preparation method of heterogeneous structure material, it is characterised in that：
In the step 5, the consumption of absolute ethyl alcohol and deionized water is not less than 20 times of filter cake volume respectively.
6. a kind of carbosphere Quito point according to claim 1 loads the preparation method of heterogeneous structure material, and its feature exists
In：The magnetic agitation time is not less than 10 minutes in the step 6.
7. a kind of carbosphere Quito point according to claim 1 loads the preparation method of heterogeneous structure material, and its feature exists
In：In the step 7, after solid matter is separated, alternately washed using deionized water, absolute ethyl alcohol, acetone, carbon is obtained final product after drying
Microballoon Quito point load heterogeneous structure material.
8. a kind of carbosphere Quito point according to claim 7 loads the preparation method of heterogeneous structure material, and its feature exists
In：In step 7, deionized water, absolute ethyl alcohol, acetone consumption respectively with washing filter cake be mark, it is deionized water, anhydrous
Ethanol, acetone are 20: 20: 20: 1 with the mass ratio of washing filter cake.
9. a kind of carbosphere Quito point according to claim 8 loads the preparation method of heterogeneous structure material, and its feature exists
In：In step 7, alternately washing times are 3~6 times；Drying temperature is 60~80 DEG C, and drying time is 4~8h.
10. a kind of carbosphere Quito point according to claim 1 loads the preparation method of heterogeneous structure material, and its feature exists
In：The concentration of acetic acid lead solution is 0.1M.
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Application publication date: 20170613 |