CN108176346A - A kind of preparation method and application of the velvet-like polymolecularity carbonitride of magnetism swan - Google Patents
A kind of preparation method and application of the velvet-like polymolecularity carbonitride of magnetism swan Download PDFInfo
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- CN108176346A CN108176346A CN201810042377.1A CN201810042377A CN108176346A CN 108176346 A CN108176346 A CN 108176346A CN 201810042377 A CN201810042377 A CN 201810042377A CN 108176346 A CN108176346 A CN 108176346A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 230000005389 magnetism Effects 0.000 title claims abstract description 9
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 claims abstract description 76
- 150000003071 polychlorinated biphenyls Chemical class 0.000 claims abstract description 38
- 239000000243 solution Substances 0.000 claims abstract description 35
- 238000000034 method Methods 0.000 claims abstract description 20
- ISPYQTSUDJAMAB-UHFFFAOYSA-N 2-chlorophenol Chemical compound OC1=CC=CC=C1Cl ISPYQTSUDJAMAB-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000007864 aqueous solution Substances 0.000 claims abstract description 7
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000004202 carbamide Substances 0.000 claims abstract description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 30
- 239000012153 distilled water Substances 0.000 claims description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- 239000000203 mixture Substances 0.000 claims description 9
- 238000013033 photocatalytic degradation reaction Methods 0.000 claims description 8
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 7
- 239000002105 nanoparticle Substances 0.000 claims description 7
- 235000019441 ethanol Nutrition 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 5
- 229910021577 Iron(II) chloride Inorganic materials 0.000 claims description 5
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 5
- 239000000908 ammonium hydroxide Substances 0.000 claims description 5
- NMCUIPGRVMDVDB-UHFFFAOYSA-L iron dichloride Chemical compound Cl[Fe]Cl NMCUIPGRVMDVDB-UHFFFAOYSA-L 0.000 claims description 5
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 5
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 2
- 238000001179 sorption measurement Methods 0.000 abstract description 43
- 230000015556 catabolic process Effects 0.000 abstract description 11
- 238000006731 degradation reaction Methods 0.000 abstract description 11
- 230000008569 process Effects 0.000 abstract description 10
- 238000003786 synthesis reaction Methods 0.000 abstract description 9
- 239000000126 substance Substances 0.000 abstract description 7
- 230000015572 biosynthetic process Effects 0.000 abstract description 6
- 229910052799 carbon Inorganic materials 0.000 abstract description 6
- 239000002131 composite material Substances 0.000 abstract description 6
- 238000012545 processing Methods 0.000 abstract description 6
- 239000003344 environmental pollutant Substances 0.000 abstract description 5
- 231100000719 pollutant Toxicity 0.000 abstract description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 4
- 238000005516 engineering process Methods 0.000 abstract description 4
- 238000002203 pretreatment Methods 0.000 abstract description 3
- 238000005119 centrifugation Methods 0.000 abstract description 2
- 238000000975 co-precipitation Methods 0.000 abstract description 2
- 238000009833 condensation Methods 0.000 abstract description 2
- 230000005494 condensation Effects 0.000 abstract description 2
- 238000001914 filtration Methods 0.000 abstract description 2
- 238000010521 absorption reaction Methods 0.000 description 19
- 239000002114 nanocomposite Substances 0.000 description 14
- 239000000463 material Substances 0.000 description 13
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 12
- 150000001875 compounds Chemical class 0.000 description 11
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 9
- 230000000694 effects Effects 0.000 description 8
- 239000002086 nanomaterial Substances 0.000 description 8
- 230000003993 interaction Effects 0.000 description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 239000003463 adsorbent Substances 0.000 description 6
- 238000004458 analytical method Methods 0.000 description 6
- 238000002414 normal-phase solid-phase extraction Methods 0.000 description 6
- 239000011780 sodium chloride Substances 0.000 description 6
- LINPIYWFGCPVIE-UHFFFAOYSA-N 2,4,6-trichlorophenol Chemical compound OC1=C(Cl)C=C(Cl)C=C1Cl LINPIYWFGCPVIE-UHFFFAOYSA-N 0.000 description 5
- 239000007788 liquid Substances 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 230000008859 change Effects 0.000 description 4
- 238000000605 extraction Methods 0.000 description 4
- 239000010865 sewage Substances 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- 239000012491 analyte Substances 0.000 description 3
- 238000010790 dilution Methods 0.000 description 3
- 239000012895 dilution Substances 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 239000012071 phase Substances 0.000 description 3
- 150000003839 salts Chemical class 0.000 description 3
- 239000012086 standard solution Substances 0.000 description 3
- 239000011550 stock solution Substances 0.000 description 3
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 2
- 238000001157 Fourier transform infrared spectrum Methods 0.000 description 2
- 230000006378 damage Effects 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 235000013305 food Nutrition 0.000 description 2
- 230000036541 health Effects 0.000 description 2
- 239000010842 industrial wastewater Substances 0.000 description 2
- 238000001819 mass spectrum Methods 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 230000000630 rising effect Effects 0.000 description 2
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- 239000002594 sorbent Substances 0.000 description 2
- 238000002336 sorption--desorption measurement Methods 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 238000002604 ultrasonography Methods 0.000 description 2
- 239000003643 water by type Substances 0.000 description 2
- 230000004580 weight loss Effects 0.000 description 2
- FIDRAVVQGKNYQK-UHFFFAOYSA-N 1,2,3,4-tetrahydrotriazine Chemical group C1NNNC=C1 FIDRAVVQGKNYQK-UHFFFAOYSA-N 0.000 description 1
- 241000251468 Actinopterygii Species 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 229910017135 Fe—O Inorganic materials 0.000 description 1
- 241001465754 Metazoa Species 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- XKMRRTOUMJRJIA-UHFFFAOYSA-N ammonia nh3 Chemical compound N.N XKMRRTOUMJRJIA-UHFFFAOYSA-N 0.000 description 1
- 150000001491 aromatic compounds Chemical class 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 231100000704 bioconcentration Toxicity 0.000 description 1
- 230000000711 cancerogenic effect Effects 0.000 description 1
- 231100000357 carcinogen Toxicity 0.000 description 1
- 239000003183 carcinogenic agent Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 231100000481 chemical toxicant Toxicity 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000010494 dissociation reaction Methods 0.000 description 1
- 230000005593 dissociations Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 230000009881 electrostatic interaction Effects 0.000 description 1
- 238000000921 elemental analysis Methods 0.000 description 1
- 238000010828 elution Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000012851 eutrophication Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000013505 freshwater Substances 0.000 description 1
- 230000000855 fungicidal effect Effects 0.000 description 1
- 239000000417 fungicide Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 230000002363 herbicidal effect Effects 0.000 description 1
- 239000004009 herbicide Substances 0.000 description 1
- 125000000623 heterocyclic group Chemical group 0.000 description 1
- 238000004128 high performance liquid chromatography Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 239000002917 insecticide Substances 0.000 description 1
- 230000002452 interceptive effect Effects 0.000 description 1
- 239000000543 intermediate Substances 0.000 description 1
- 238000000622 liquid--liquid extraction Methods 0.000 description 1
- 238000001334 liquid-phase micro-extraction Methods 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 229920005588 metal-containing polymer Polymers 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 231100000350 mutagenesis Toxicity 0.000 description 1
- 238000002703 mutagenesis Methods 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 244000052769 pathogen Species 0.000 description 1
- 230000001717 pathogenic effect Effects 0.000 description 1
- 230000002688 persistence Effects 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 231100000572 poisoning Toxicity 0.000 description 1
- 230000000607 poisoning effect Effects 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
- 239000000941 radioactive substance Substances 0.000 description 1
- 239000011541 reaction mixture Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000002470 solid-phase micro-extraction Methods 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 238000010025 steaming Methods 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
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- 238000001757 thermogravimetry curve Methods 0.000 description 1
- 239000011864 timber preservative Substances 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 231100000167 toxic agent Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 239000003440 toxic substance Substances 0.000 description 1
- 238000003911 water pollution 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
- B01J20/0203—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
- B01J20/0259—Compounds of N, P, As, Sb, Bi
-
- 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
- B01J20/28—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
-
- 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
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/24—Nitrogen compounds
-
- B01J35/39—
-
- 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
-
- 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
- C02F2101/36—Organic compounds containing halogen
-
- 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 composite material synthesis and analyzing and processing technical field, are related to carbonitride, are related to a kind of magnetic velvet-like polymolecularity carbonitride of swan (V g C3N4/Fe3O4) preparation method and application.V g C are made through one step thermal condensation of high temperature in aqueous solution of urea by the present invention3N4, then ultrasonic disperse, by chemical coprecipitation its surface fix Fe3O4With magnetism, the synthetic operation is simple.The present invention is also by the velvet-like polymolecularity carbonitride of magnetic swan (V g C3N4/Fe3O4) be added in Polychlorinated biphenyls or chlorophenol solution and carry out adsorption treatment, there is pre-treatment simple operation, the rate of adsorption fast (30s), be easily isolated, be reusable, in sample handling processes, centrifugation or filtering are needed not move through, reduces the loss of sample.Can degradation treatment be carried out with parachlorphenol.The pre-treating method established provides new thinking and technology to handle other nonpolar pollutant samples for containing carbon-based ring structure.
Description
Technical field
The invention belongs to composite material synthesis and analyzing and processing technical field, are related to carbonitride, are related to a kind of magnetic swan
Velvet-like polymolecularity carbonitride (V-g-C3N4/Fe3O4) preparation method and application.
Background technology
The earth is referred to as " Mercury ball ", it is well known that although it is waters that earth surface has 71%, but ocean salt just accounts for
The 97.5% of waters, removes the two-stage covered by iceberg, the fresh water that the mankind can utilize only accounts for the 0.2% of earth total Water.
However, with the discharge of industrial wastewater in recent years and sanitary sewage etc., the annual COD in China is emitted on 24,000,000 tons
Left and right, ammonia nitrogen discharge capacity is at 2,450,000 tons or so, and considerably beyond current environmental carrying capacity, water quality is by a large amount of ground contaminations.Water is ten thousand
The source of object, not only the mankind, tellurian biology are equally all to be unable to do without water.Chemical toxicant, organic aerobic object in sewage, nothing
Machine solid suspension, heavy metal, radioactive substance, pathogen etc., cause body eutrophication, destroy the ecological body in water
System；If the fish in edible sewage, it will serious damage is caused to human body, consequence allows of no optimist；Also contain in sewage simultaneously
There are a large amount of toxicants, immeasurable destruction is brought, therefore the water pollution in environment is handled for agricultural, forestry etc.
It is extremely urgent.
Polychlorinated biphenyls (PCBs) is one of typical persistence organic pollutant of Convention of Stockholm priority acccess control, due to
It has higher bio-toxicity, bioconcentration and anti-degradability, can be concentrated by food chain, cause the potential danger to human body
Evil, building up property poisoning, seriously affects human health.Chlorophenol (CPs) usually as chemicals intermediate, timber preservative,
Herbicide, insecticide and fungicide etc. are widely used in chemical industry, forestry and woodworking, are widely present in industrial wastewater.
Since CPs is toxic, mutagenesis and carcinogen, the death of animal and plant can be led to, people increasingly worry CPs to ring
Border and the influence of human health.The pollution getting worse that PCBs and CPs are brought in environment, researcher are dedicated to carrying out them
Quantitative analysis measures, but its concentration is low in the sample, there are many interfering substance and matrix complex, therefore before must being carried out to sample
Processing rear can measure.The present invention has chosen after Polychlorinated biphenyls and chlorophenol carry out it efficient pre-treatment and carries out quantitative measurment.
At present, Polychlorinated biphenyls and the common pre-treating method of chlorophenol have liquid-liquid extraction, liquid-phase micro-extraction, solid phase microextraction,
Superfluid extraction etc..Solid Phase Extraction can complete example enrichment and purification, but there is consumption simultaneously as a kind of novel abstraction technique
Duration, extraction column easily block, consume the problems such as a large amount of organic solvents.Magnetic solid phase extraction is that one kind is easy to operate, is easily isolated, is honest and clean
The novel solid phase extraction techniques of valency, when handling complex sample, there is no the columns encountered in Solid Phase Extraction to block up magnetic solid phase extraction
The problems such as plug.Wherein, the key for being selected to magnetic solid phase extraction technology of magnetic material.In carbonitride race, graphite-phase nitrogen
Change carbon (g-C3N4) it is most stable of allotrope, it is stable at up to 500 DEG C, it is only by common Elements C, N and H
Composition has higher acid resistance and alkali resistance, is widely used in pollutant photocatalytic degradation.However traditional g-C3N4Because than
Surface area is smaller, and the treatment effeciency of pollutant is had certain limitations, and the present invention has synthesized a kind of synthesis and simply, with larger compared table
The V-g-C of area3N4Nano material, the more common g-C of adsorption efficiency3N4Higher, and by fixing Fe on surface3O4With magnetic
Property, increase specific surface area, and Fe3O4Nano-particle is easy to fixed, will not adsorption analysis object.
Invention content
In view of the above-mentioned deficiencies in the prior art, it is an object of the present invention to disclose the velvet-like height of magnetic swan
The preparation method of dispersed carbonitride.
Technical solution
A kind of preparation method of the velvet-like polymolecularity carbonitride of magnetism swan, comprises the following steps：
A. a concentration of 0.5~1.0g/mL aqueous solution of urea is added in alumina crucible, be put into 350 in Muffle furnace~
450 DEG C of 1~2h of heating, 450~500 DEG C are heated 4~7h, are collected product and are simultaneously dried at room temperature for, obtain V-g-C3N4；
~100 DEG C b.60 at, by FeCl3·6H2O and FeCl2·4H2O presses 1~3:1：The molal volume of 150~250mL
Than being added in distilled water, stir evenly；
C. ammonium hydroxide is added dropwise, reacts 2~4h, obtained Fe is then washed with water and ethyl alcohol3O4Nano particle, in sky
It is dry in gas, wherein the volume ratio of the ammonium hydroxide and distilled water described in step b is 1~4：15~25；
D. by step a V-g-C3N4With in step c Fe3O4Nano particle is dispersed in distilled water, at ultrasound
0.2~0.8h is managed, wherein, the V-g-C3N4、Fe3O4Quality, volume ratio with distilled water are 1~3:1:40~100mL；
E. mixture at 40~80 DEG C is stirred into 8~14h, cooled down, filtered and wash 3~5 with deionized water and ethyl alcohol
Secondary, 40~80 DEG C of drying are to get the velvet-like polymolecularity carbonitride of magnetic swan.
In the more excellent disclosed example of the present invention, 400 DEG C of heating 1h, 450 DEG C of heating 5h in Muffle furnace are put into described in step a.
In the more excellent disclosed example of the present invention, described in step b 85 DEG C by FeCl3·6H2O and FeCl2·4H2O presses 2:1:200mL
Molal volume ratio be added in distilled water.
In the more excellent disclosed example of the present invention, ammoniacal liquor mass concentration described in step c is 25~28%.
In the more excellent disclosed example of the present invention, mixture is stirred into 10h at 60 DEG C described in step e.
Another object of the present invention is to disclose according to the velvet-like polymolecularity of magnetic swan made from the above method
Application of the carbonitride in Polychlorinated biphenyls or chlorophenol processing, i.e., by the velvet-like polymolecularity carbonitride (V-g-C of magnetic swan3N4/
Fe3O4) be added in Polychlorinated biphenyls or chlorophenol solution and adsorbed, it can also parachlorphenol progress photocatalytic degradation.
Specifically, the application includes the following steps：
(1) mixed liquor for preparing 1.0 μ g/mL PCBs mixed liquors and CPs respectively is stored in vial, for use；
(2) and then by the velvet-like polymolecularity carbonitride (V-g-C of magnetic swan3N4/Fe3O4) (1.0mg) be added to what is prepared
In PCBs the CPs aqueous solutions of 1.0mL；
(3) by mixture ultrasound, until the concentration of target compound stops declining, and obtain equilibrium adsorption, with magnet pair
It carries out separation of solid and liquid, and the liquid of gained is measured with HPLC；
(4) 1.0mL ethyl alcohol is added in into sorbent material, and is ultrasonically treated 1.0min, at this point, the PCBs of absorption is by ethyl alcohol
Elution, ibid reuses magnet and carries out separation of solid and liquid to it, then drying nano composite material adsorbent and reuses；
(5) it by the amount of subtraction absorption PCBs on the sorbent and CPs, operates above in triplicate；
(6) solution after the standard specimen to three kinds of CPs solution of 1 μ g/mL and degradation respectively, carries out real-time mass spectrum (DART)
Analysis finds that three kinds of CPs are complete by photocatalytic degradation, and degradation rate is about 100%.
The principle of this method：g-C3N4With two-sided fragrant supporting structure, there is big pi-electron structure, so as to make its absorption
Mechanism mainly includes hydrophobic effect, π-pi-conjugated and electrostatic interaction, so it is to food, drug, in organism and pollutant
Aromatic compound have strong affinity effect.In addition, g-C3N4It is typically to have without metal-containing polymer semi-conducting material
The band gap of 2.7eV, visible light absorbing are widely used in contaminant degradation.The velvet-like graphite-phase nitrogen of swan prepared by the present invention
Change carbon (V-g-C3N4/Fe3O4) specific surface area bigger, favorable dispersibility, adsorption efficiency are high in water.And Fe3O4With magnetism, than
Surface area is larger, easily fixes in V-g-C3N4, be conducive to the absorption degradation to PCBs and CPs.
Advantageous effect
V-g-C is made through one step thermal condensation of high temperature in aqueous solution of urea by the present invention3N4, then ultrasonic disperse, by chemistry altogether
The precipitation method fix Fe on its surface3O4With magnetism, the synthetic operation is simple.The present invention is also by the velvet-like high score of magnetic swan
Dissipate property carbonitride (V-g-C3N4/Fe3O4) be added in Polychlorinated biphenyls or chlorophenol solution and carry out adsorption treatment, there is pre-treatment behaviour
Make the convenient, rate of adsorption fast (30s), be easily isolated, reusable advantage, in sample handling processes, need not move through centrifugation
Or filtering, reduce the loss of sample.Can degradation treatment be carried out with parachlorphenol.The pre-treating method that this method is established, for processing
Other nonpolar pollutant samples for containing carbon-based ring structure provide new thinking and technology.
Description of the drawings
Fig. 1 (a) Fe3O4,V-g-C3N4And V-g-C3N4/Fe3O4TGA curves；(b)V-g-C3N4,Fe3O4And V-g-
C3N4/Fe3O4XRD diagram；(c)V-g-C3N4,Fe3O4And V-g-C3N4/Fe3O4FT-IR figure；(d)V-g-C3N4And V-g-
C3N4/Fe3O4N2N2 adsorption-desorption；
(a) V-g-C of Fig. 2 different times synthesis3N4and(b)V-g-C3N4/Fe3O4TEM figure；
Fig. 3 .V-g-C3N4/Fe3O4To PCBs or CPs adsorption treatment process schematics；
Fig. 4 .V-g-C3N4/Fe3O4Adsorption treatment PCBs influence factors：(a) initial concentration of PCBs；(b) adsorption time；
(c) solution salinity；(d) pH value of solution；(e) solution temperature；
Fig. 5 .V-g-C3N4/Fe3O4Adsorption treatment CPs influence factors：(a) initial concentration of CPs；(b) adsorption time；(c)
Solution salinity；(d) pH value of solution；(e) solution temperature；
Fig. 6 utilize the measure of tri- kinds of CPs standard specimens of DART, (a) 2,4,6-TCP, (b) 2,3,4,6-TCP, (c) PCP.
Specific embodiment
The following describes the present invention in detail with reference to examples, so that those skilled in the art more fully understand this hair
It is bright, but the invention is not limited in following embodiments.
Embodiment 1
V-g-C3N4/Fe3O4To the adsorption treatment of Polychlorinated biphenyls
(1)V-g-C3N4/Fe3O4Synthesis
A concentration of 0.5~1.0g/mL aqueous solution of urea is added in into alumina crucible, is put into Muffle furnace, 350~450
1~2h is heated at DEG C, 4~7h is then heated at 450~500 DEG C, finally collect product and is dried at room temperature for, obtains V-g-
C3N4.At 60~100 DEG C, by FeCl3·6H2O and FeCl2·4H2O presses 1:1~3:1 molar ratio is added to 150~250mL steamings
In distilled water, 5min is stirred, is uniformly distributed it, be then gradually added into 10~40ml ammonium hydroxide (25~28%), react 2~4h, most
Afterwards obtained Fe is washed using water and ethyl alcohol3O4Then nano particle is dried in air.It is prepared by chemical coprecipitation
V-g-C3N4/Fe3O4Mass ratio is 1 first by nanocomposite:1~3:1 V-g-C3N4And Fe3O4It is dispersed in 40~
In the distilled water of 100mL, it is ultrasonically treated 0.2~0.8 hour at room temperature.Secondly, gained mixture is stirred at 40~80 DEG C
It mixes 8~14 hours.Then, reaction mixture is cooled down and is washed 3~5 times with deionized water and ethyl alcohol.Finally, receiving synthesis
Nano composite material is dried in 40~80 DEG C of baking ovens.
(2)V-g-C3N4/Fe3O4Characterization
First, determination of elemental analysis is carried out to determine V-g-C3N4/Fe3O4The component of sample.V-g-C3N4The H of middle trace and
O may be due to its NH2The CO of/NH groups absorption2, O2And H2Caused by O.Chemical formula is expressed as [C6N7(NH2) (NH)] n,
With the V-g-C of preparation3N4Chemical composition C2.76N3.57H2.34Unanimously.
In order to determine V-g-C3N4/Fe3O4V-g-C in composite material3N4Amount, in air, from 40-800 DEG C carry out heat
Weight analysis (TGA) (Fig. 1 (a)).At 120 DEG C, the weight loss of beginning is due to the evaporation of water in sample, from 400 DEG C to 700
DEG C, observe Fe3O4, C3N4And V-g-C3N4/Fe3O4Mass loss respectively may be about 0.36%, 91.16% and 23.81%, this
Show that a large amount of weight loss occurs between 400 DEG C and 600 DEG C, be due to V-g-C3N4Aerial oxidation and decomposition.Cause
This, V-g-C3N4/Fe3O4About contain 23wt%V-g-C in nanocomposite3N4。
XRD and FT-IR is used to determine the structure of sample.From V-g-C3N4It can be seen that in the XRD spectrum (Fig. 1 (b)) of sample,
Comprising two peaks at about 13.1 ° and 27.2 °, with V-g-C3N4(1 0 0) and (0 0 2) crystal face match.Work as V-g-
C3N4With Fe3O4During mixing, V-g-C3N4And Fe3O4Diffraction maximum than pure V-g-C3N4With pure Fe3O4Diffraction maximum it is weak, show V-g-
C3N4/Fe3O4It is by V-g-C3N4And Fe3O4Two phase compositions.Fig. 1 (c) shows V-g-C3N4, Fe3O4And V-g-C3N4/Fe3O4's
FT-IR spectrum.1200 and 1650cm-1Between bands of a spectrum correspond to CN heterocycles Typical tensile absorption peak, in V-g-C3N4Spectrogram
In, it can be seen that in 808cm-1There are one absorption peaks at place, are 5-triazine units (C6N7) characteristic absorption peak, show synthesis be V-g-
C3N4。3100-3300cm-1The wide absorption band at place, is caused by the stretching of N-H group keys or the stretching vibration of O-H.Fe3O4With
V-g-C3N4/Fe3O4Nanocomposite is in 570cm-1The absorption band at place is due to Fe3O4In Fe-O caused by.In short, FT-
IR spectrum show to successfully synthesize V-g-C3N4, Fe3O4And V-g-C3N4/Fe3O4Nanocomposite.
It in order to measure the specific surface area of these materials, is measured using N2 adsorption-desorption, V-g-C is found in Fig. 1 (d)3N4With
V-g-C3N4/Fe3O4Specific surface area be respectively 151.5 and 126.6m2/ g, the results showed that successfully synthesize big specific surface area
Material, and (V-g-C3N4/Fe3O4) surface area reduction be due to Fe3O4In V-g-C3N4On deposition cause.
In order to confirm Fe3O4It is deposited on V-g-C3N4On, understand V-g-C3N4And V-g-C3N4/Fe3O4Pattern, pass through TEM
It has been analyzed and characterized both solids.As shown in Fig. 2, pure V-g-C3N4It is made of transparent filament, and in V-g-C3N4/
Fe3O4In, the Fe of black3O4Nanoparticle deposition is in V-g-C3N4Surface.Under the similarity condition, phenetic analysis multi-stage synthesis
Nano material, to prove the reproducibility of synthetic method, from TEM it can be seen from the figure thats, the appearance of each synthetic material is consistent.
(3) preparation of standard reserving solution
Single sample standard solution of the 100 μ g/mL of 10 kinds of PCBs is prepared with methanol respectively, and is stored in 4.0 DEG C of environment.It is logical
After daily with distilled water dilution standard stock solution come preparation work solution.
(4) influence of PCBs initial concentrations
The initial concentration of PCBs can influence V-g-C3N4/Fe3O4Nanocomposite is to the practical adsorbance of PCBs.In order to
The suitable PCBs concentration of interaction and selection studied between PCBs and nanocomposite is used for the follow-up excellent of processing
Change, the present invention has studied influence of the Polychlorinated biphenyls initial concentration to target analytes adsorption rate, and concentration range is 0.1~1.0 μ g/
ML, as a result as shown in Fig. 4 (a), it can be seen that with the increase of concentration, V-g-C3N4/Fe3O4The adsorbance of PCBs is gradually increased
Add.In order to further study influence of the other conditions to absorption behavior, the present invention uses the PCBs of 0.5 μ g/mL.
(5) influence of adsorption time
The present invention has studied influence of the adsorption time to adsorption rate, and access time range is 30s~420s, and experimental result is such as
Shown in Fig. 4 (b), according to it can be seen from the figure that, the time has little effect the absorption of target compound, illustrates, adsorption equilibrium
It has been rapidly reached within 30 seconds.The reason of causing this quick adsorption is V-g-C3N4/Fe3O4Good dispersion and receive
The strong interaction of nano composite material and target compound.
(6) influence of salinity
In 0~25.0% concentration range, influence of the research salinity to PCBs adsorption effects.By in Fig. 4 (c) it is found that
The adsorbance of PCBs with add in NaCl amount from 0% increase to 10.0% when increase, then as add in NaCl amount increasing
Add and reduce.The addition of salt can improve the adsorption efficiency of target compound, but can reduce the solubility (salting-out effect) of PCBs
With the increase for leading to solution viscosity, this can reduce the quality transfering rate and extraction efficiency of PCBs.
(7) influence of pH
Influence of the pH value of solution to absorption is studied by adding in 1M HCl or the 1M NaOH of proper volume, the pH of selection exists
In the range of 1.0~11.0.The pH of solution can influence the state of charge of target compound and its interaction with adsorbent.Such as
Shown in Fig. 4 (d), the influence very little of the pH of solution to absorption.The reason of causing this phenomenon is during PCBs is under household condition
Property molecule, by pH value of solution variation influenced.
(8) influence of temperature
The present invention is investigated the influence of temperature, because raising temperature can reduce solution viscosity to realize solution diffusivity
Increase, to improve adsorption efficiency, but higher temperature reduces the interaction between target compound and adsorbent, instead
And adsorbance can be caused to reduce.The adsorbance of PCBs is as temperature when rising to 30.0 DEG C for 15.0 DEG C from increasing as shown in Fig. 4 (e),
Along with the raising of temperature, adsorbance reduces instead.
(9) reuse of magnetic Nano material
Magnetic nanometer composite material is reused in PCBs adsorption processes, to study the recyclable utilization of adsorbent
Property.Before re-use, they with water and ethyl alcohol are washed for several times successively, then dried.After five times are reused, analyte
The rate of recovery is not substantially reduced or increases.Wherein material to the adsorption rate of PCBs 90~100%, the results showed that V-g-C3N4/
Fe3O4It is stable, and does not have the carrying of PCBs in adsorption process, it is good reusable shows that material has
Property.
Embodiment 2
V-g-C3N4/Fe3O4The adsorption treatment of parachlorphenol
(1)V-g-C3N4/Fe3O4Synthesis
(2) preparation of standard reserving solution
The standard solution of the 100 μ g/mL of three kinds of CPs is prepared with methanol respectively, and is stored in 4.0 DEG C of environment, by every
It is with distilled water dilution standard stock solution come preparation work solution.
(3) influence of CPs initial concentrations
The initial concentration of CPs determines that theoretically nanocomposite can be with the maximum of adsorbed target compound in water sample
Amount, and V-g-C can be influenced3N4/Fe3O4On practical adsorbance.This experimental study chlorophenol initial concentration is to target analysis
The influence of object adsorption rate, concentration range are 0.1~1.0ug/mL, as a result as shown in Fig. 5 (a), it can be seen that with the increasing of concentration
Add, V-g-C3N4/Fe3O4The adsorbance of CPs is gradually increased.In order to further study influence of the other conditions to absorption behavior,
The present invention uses 0.5ug/mL.
(4) influence of adsorption time
The present invention has studied influence of the adsorption time to adsorption rate, and access time range is 30s~420s, and experimental result is such as
Shown in Fig. 5 (b), according to it can be seen from the figure that, the time has little effect the absorption of target compound, shows adsorption equilibrium
It has been rapidly reached within 30 seconds.The reason of causing this quick adsorption is V-g-C3N4/Fe3O4Good dispersion and receive
The strong interaction of nano composite material and target compound.
(5) influence of salinity
In the concentration range of 0~30.0%NaCl (w/v), influence of the research salinity to adsorption effect.By in figure it is found that
The adsorbance of CPs with add in NaCl amount from 0% increase to 25.0% when increase, then as add in NaCl amount continuation
Increase reduces (Fig. 5 (c)) instead.The addition of salt can improve the adsorption efficiency of target compound, but can reduce the solubility of CPs
(salting-out effect) and the increase for leading to solution viscosity can reduce the quality transfering rate and extraction efficiency of CPs.Therefore, it is of the invention
The NaCl for adding in 25.0% is used for subsequent condition optimizing.
(6) influence of pH
Under normal conditions, the pH of solution is the important factor in order in CPs adsorption processes, is because pH can not only change
The existing forms and state of charge of analyte, and the interaction between CPs and nanocomposite can be changed.Therefore,
Influence of the pH value of solution (1.0~11.0) to absorption is studied by adding in 1M HCl or the 1M NaOH of proper volume.Such as Fig. 5 (d)
Shown, the pH of solution has a great impact to the process of material absorption CPs, and nanocomposite will to the adsorption rate of three kinds of CPs
100.00%, and when pH increases to 3.0 from 1.0, the adsorption rate of three kinds of CPs increases, and pH increases to 11.0 from 3.0
When, the adsorption rate of three kinds of CPs reduces.It is CPs is acidic molecular or in neutral and alkaline environment the reason of this phenomenon occur
Caused by a large amount of dissociation of middle CPs, therefore, the present invention selects pH as 3.0.
(7) influence of temperature
The present invention has studied the influence of temperature, because raising temperature can reduce solution viscosity to realize that solution is diffusible
Increase, to improve adsorption efficiency, but higher temperature reduces the interaction between target compound and adsorbent, instead
Adsorbance can be caused to reduce.Fig. 5 (e) shows that the adsorbance of chlorophenol is as temperature when rising to 25.0 DEG C for 15.0 DEG C from increasing, then
With the raising of temperature, adsorbance reduces instead.
(8) reuse of magnetic Nano material
Magnetic nanometer composite material is reused in CPs adsorption processes, to study the reusing of adsorbent.Five
After secondary reuse, the analyte rate of recovery is not substantially reduced or increases.Wherein material to the adsorption rate of PCBs 90~
100%, the results showed that V-g-C3N4/Fe3O4It is stable, and does not have the carrying of CPs in adsorption process, shows material
Material has good reusability.
Embodiment 3
V-g-C3N4/Fe3O4The photocatalytic degradation of parachlorphenol
(1) preparation of standard reserving solution
In methyl alcohol, the standard solution of the 100 μ g/mL of 2,4,6-TCP, 2,3,4,6-TCP and PCP is prepared respectively, and is stored up
There are in 4.0 DEG C of environment.By daily with distilled water dilution standard stock solution come preparation work solution.
(2) Photocatalytic Degradation Process
In aqueous solution, by assessing prepared receive to the degradation of 2,4,6-TCP, 2,3,4,6-TCP and PCP respectively
The photocatalytic activity of rice material.Under simulated solar irradiation, lamp radiated wavelength range is 400~800nm, and it is real to carry out photocatalytic degradation
It tests.Due to absorption ratio faster, so before exposure, respectively by 2,4,6-TCP containing nano material, 2,3,4,6-TCP
60 seconds are adsorbed with PCP solution to reach absorption-desorption balance.Then, according to experiment needs, by one timing of turbid liquid irradiation
Between, carry out fully degraded.
Respectively the standard specimen (Fig. 6) of 2,4,6-TCP, 2,3,4,6-TCP and PCP solution to 1 μ g/mL and degradation after it is molten
Real-time mass spectrum (DART) analysis of liquid, by finding that three kinds of CPs are complete by photocatalytic degradation in figure, degradation rate is close to 100%.
(3) reuse of magnetic Nano material
V-g-C3N4/Fe3O4It is reused after light degradation experiment, to study the recycling of magnetic nanometer composite material
Property.After five times recycle, the degradation percentage of three kinds of analytes is not substantially reduced or increases, magnetic 96~100%
The good repeatability of nanocomposite shows that it is kind of a stable and permanent nano material, in addition, photochemical catalyst is sharp again
The pollution of nano material can be protected the environment against with property.
The foregoing is merely the embodiment of the present invention, are not intended to limit the scope of the invention, every to utilize this hair
The equivalent structure or equivalent flow shift that bright specification is made directly or indirectly is used in other related technical areas,
Similarly it is included within the scope of the present invention.
Claims (8)
1. the preparation method of the velvet-like polymolecularity carbonitride of a kind of magnetism swan, which is characterized in that comprise the following steps：
A. a concentration of 0.5~1.0g/mL aqueous solution of urea is added in alumina crucible, is put into Muffle furnace 350~450 DEG C
1~2h is heated, 450~500 DEG C of 4~7h of heating collect product and are dried at room temperature for, obtain V-g-C3N4；
~100 DEG C b.60 at, by FeCl3·6H2O and FeCl2·4H2O presses 1~3:1：The molal volume of 150~250mL is than adding in
Into distilled water, stir evenly；
C. ammonium hydroxide is added dropwise, reacts 2~4h, obtained Fe is then washed with water and ethyl alcohol3O4Nano particle, in air
It is dry, wherein the volume ratio of the ammonium hydroxide and distilled water described in step b is 1~4：15~25；
D. by step a V-g-C3N4With in step c Fe3O4Nano particle is dispersed in distilled water, is ultrasonically treated 0.2
~0.8h, wherein, the V-g-C3N4、Fe3O4Quality, volume ratio with distilled water are 1~3:1:40~100mL；
E. mixture at 40~80 DEG C is stirred into 8~14h, cooled down, filtered and wash 3~5 times with deionized water and ethyl alcohol, 40
~80 DEG C of drying are to get the velvet-like polymolecularity carbonitride of magnetic swan.
2. the preparation method of the velvet-like polymolecularity carbonitride of magnetic swan according to claim 1, it is characterised in that：Step a
It is described to be put into 400 DEG C of heating 1h, 450 DEG C of heating 5h in Muffle furnace.
3. the preparation method of the velvet-like polymolecularity carbonitride of magnetic swan according to claim 1, it is characterised in that：Step b
Described 85 DEG C by FeCl3·6H2O and FeCl2·4H2O presses 2:1:The molal volume ratio of 200mL is added in distilled water.
4. the preparation method of the velvet-like polymolecularity carbonitride of magnetic swan according to claim 1, it is characterised in that：Step c
The ammoniacal liquor mass concentration is 25~28%.
5. the preparation method of the velvet-like polymolecularity carbonitride of magnetic swan according to claim 1, it is characterised in that：Step e
It is described that mixture is stirred into 10h at 60 DEG C.
6. the velvet-like polymolecularity carbonitride of magnetic swan according to made from claim 1-5 any claim the methods.
7. a kind of application of the velvet-like polymolecularity carbonitride of magnetic swan described in claim 6, it is characterised in that：By the magnetism
The velvet-like polymolecularity carbonitride of swan, which is added in Polychlorinated biphenyls or chlorophenol solution, to be adsorbed.
8. a kind of application of the velvet-like polymolecularity carbonitride of magnetic swan described in claim 6, it is characterised in that：By the magnetism
The velvet-like polymolecularity carbonitride of swan, which is added in chlorophenol solution, carries out photocatalytic degradation.
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Application publication date: 20180619 |