CN110102327A - A kind of defect carbonitride coupling pucherite catalysis material and preparation method thereof and purposes - Google Patents
A kind of defect carbonitride coupling pucherite catalysis material and preparation method thereof and purposes Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 36
- 230000007547 defect Effects 0.000 title claims abstract description 32
- 238000006555 catalytic reaction Methods 0.000 title claims abstract description 27
- 230000008878 coupling Effects 0.000 title claims abstract description 22
- 238000010168 coupling process Methods 0.000 title claims abstract description 22
- 238000005859 coupling reaction Methods 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 239000002351 wastewater Substances 0.000 claims abstract description 15
- 230000001699 photocatalysis Effects 0.000 claims abstract description 14
- 238000007146 photocatalysis Methods 0.000 claims abstract description 10
- 229910002915 BiVO4 Inorganic materials 0.000 claims abstract description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 4
- 229920000877 Melamine resin Polymers 0.000 claims abstract description 4
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000004202 carbamide Substances 0.000 claims abstract description 4
- 229960000935 dehydrated alcohol Drugs 0.000 claims abstract description 4
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims abstract description 4
- JOPOVCBBYLSVDA-UHFFFAOYSA-N chromium(6+) Chemical compound [Cr+6] JOPOVCBBYLSVDA-UHFFFAOYSA-N 0.000 claims description 8
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 5
- 150000001875 compounds Chemical class 0.000 claims description 5
- 229910017604 nitric acid Inorganic materials 0.000 claims description 5
- 239000011651 chromium Substances 0.000 claims description 4
- 239000002131 composite material Substances 0.000 claims description 4
- 238000005286 illumination Methods 0.000 claims description 4
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 claims description 4
- 238000005070 sampling Methods 0.000 claims description 4
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 3
- 239000004809 Teflon Substances 0.000 claims description 3
- 229920006362 Teflon® Polymers 0.000 claims description 3
- 239000000654 additive Substances 0.000 claims description 3
- 230000000996 additive effect Effects 0.000 claims description 3
- 239000000908 ammonium hydroxide Substances 0.000 claims description 3
- 230000003197 catalytic effect Effects 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 230000001376 precipitating effect Effects 0.000 claims description 3
- 229910001220 stainless steel Inorganic materials 0.000 claims description 3
- 239000010935 stainless steel Substances 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 238000010792 warming Methods 0.000 claims description 3
- 238000003760 magnetic stirring Methods 0.000 claims description 2
- 239000000047 product Substances 0.000 claims description 2
- 239000006228 supernatant Substances 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims description 2
- 238000005375 photometry Methods 0.000 claims 1
- 238000000870 ultraviolet spectroscopy Methods 0.000 claims 1
- 239000002023 wood Substances 0.000 claims 1
- 229910001385 heavy metal Inorganic materials 0.000 abstract description 7
- 231100000252 nontoxic Toxicity 0.000 abstract description 2
- 230000003000 nontoxic effect Effects 0.000 abstract description 2
- 238000004064 recycling Methods 0.000 abstract description 2
- 238000001354 calcination Methods 0.000 abstract 1
- 238000001027 hydrothermal synthesis Methods 0.000 abstract 1
- 238000000034 method Methods 0.000 description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 7
- 238000004519 manufacturing process Methods 0.000 description 5
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- 238000006243 chemical reaction Methods 0.000 description 3
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- 238000010521 absorption reaction Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052797 bismuth Inorganic materials 0.000 description 1
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000010531 catalytic reduction reaction Methods 0.000 description 1
- 238000009388 chemical precipitation Methods 0.000 description 1
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- 229910002804 graphite Inorganic materials 0.000 description 1
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- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
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- 239000008204 material by function Substances 0.000 description 1
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
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- 238000003786 synthesis reaction Methods 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 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
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/24—Nitrogen compounds
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
- B01J35/61—Surface area
-
- 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
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
- C02F2101/22—Chromium or chromium compounds, e.g. chromates
-
- 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
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Hydrology & Water Resources (AREA)
- Water Supply & Treatment (AREA)
- Environmental & Geological Engineering (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Toxicology (AREA)
- Catalysts (AREA)
- Treatment Of Water By Oxidation Or Reduction (AREA)
Abstract
The present invention relates to a kind of defect carbonitride coupling pucherite catalysis material and preparation method thereof and purposes.Catalysis material preparation comprises the concrete steps that: hydro-thermal method prepares monoclinic phase BiVO4, it is dissolved in dehydrated alcohol with melamine, urea, defect carbonitride coupling pucherite catalysis material is obtained after Muffle furnace calcining.The catalysis material is easy to get, photocatalysis efficiency is high, nontoxic, recycling is simple.The material can efficiently in reducing waste water Cr VI.The heavy metal wastewater therebies of plant emissions such as the present invention can be used for being electroplated, electronics are effectively treated.
Description
Technical field
The invention belongs to environment functional materials and water process new technical field, and in particular to a kind of defect carbonitride coupling vanadium
Sour bismuth catalysis material and preparation method thereof and purposes.
Background technique
Currently, a large amount of heavy metal contaminants discharge by various modes since China's industrial or agricultural and science and technology are grown rapidly
To water body.Cr VI causes great influence to human production life, easily causes since its is easy to migrate, easy absorbed property
The damage of human kidney, liver leads to various burst diseases.Therefore it is badly in need of finding what efficient and economic technology discharged enterprise
Waste water is handled.Ion exchange, absorption, redox, electro-deposition, filtering, chemical precipitation, infiltration etc. are conventional treatment skills
Art.And in recent years, photocatalytic method because its have the advantages that normal temperature and pressure, Non-toxic, rapidly and efficiently, selectivity it is good, energy consumption it is low, and
The attention being subject to is growing day by day.In this regard, research and development are novel with high efficiency and cheap practical photochemical catalyst, then become into
The critical problem of the development of one step and application photocatalytic method.
Graphite phase carbon nitride (g-C3N4) it is to have unique electronic band structure and excellent physical and chemical stability, right
Visible light has the polymer semiconductor responded strongly.Because its preparation cost is cheap, in the pollution-free substance release of reaction process, stabilization
Mildly and without good characteristics such as heavy metal element components, and it is widely used in visible light catalytic, such as the drop of organic pollutant
Solution, selective light synthesis and photodissociation aquatic products hydrogen produce oxygen etc..But one pack system g-C3N4Exciton binding energy with photo-generated carrier is high,
Photo-generate electron-hole is compound seriously, specific surface area is small, forbidden bandwidth is big, is unfavorable for separation of solid and liquid and catalyst after the completion of catalysis
Recycling the disadvantages of, limit its popularization in actual production and life.By regulating and controlling g-C3N4Pattern and coherent condition mention
High visible photocatalysis performance, such as building defect g-C3N4, defect g-C3N4There are more holes and active site in surface, no
It is only capable of increasing specific surface area, moreover it is possible to widen visible absorption range and enhancing electron-hole pair separative efficiency.BiVO4With pole
High visible light-responded performance is, it can be achieved that decompose water and degradation of organic substances under visible light.The photocatalysis material of unoccupied orbital will be can provide
Material list monoclinic phase BiVO4With defect g-C3N4It is compound, it restrained effectively the compound of photo-generated carrier, improve the efficiency of light quantum,
To improve the separating capacity of light induced electron and hole, the photocatalysis efficiency of material.Therefore by composite material prepared by the present invention
For the Cr VI in photo catalytic reduction water, effective technological borrowing can be provided for the processing of heavy metal wastewater thereby.
Summary of the invention
The technical problems to be solved by the present invention are: the treatment effeciency for being directed to existing photochemical catalyst is not high, is difficult to quantify to give birth to
The problems such as production, develops a kind of stronger and more efficient functionality two that can be used for photocatalysis treatment heavy metal ion of catalytic performance
First composite material.
The present invention proposes a kind of preparation method of defect carbonitride coupling pucherite catalysis material, by BiVO4With defect
g-C3N4It is compound, improve the photocatalytic activity of material, the specific steps are as follows:
(1) 10~40g NH is weighed4VO3, 50~120g Bi (NO3)3·5H2O is dissolved in the nitric acid of 300~1000mL
(the nitric acid molar concentration is 1~6mol/L), pH value of solution is 1~5 after adjusting mixing with ammonium hydroxide, and 20~60min of stirring is simultaneously quiet
It sets two hours or more, the precipitating of solution bottom is transferred in 20~100mL Teflon inner liner stainless steel autoclave, volume accounting
50%~70%, autoclave is put into baking oven and is heated to 150~270 DEG C, and is kept for 8~16 hours, is cooled to room temperature, is washed
Pucherite is obtained after drying；
(2) 10~50g melamine, 30~150g urea are weighed, and weigh pucherite 1 obtained in step (1)~
10g is dissolved in 300~1000mL dehydrated alcohol, is stirred 20~80min in 20~80 DEG C of water-bath, and it is extra to outwell
Surplus solution is dispensed into crucible by supernatant, is put into Muffle furnace after closeing the lid, and 2~6 are kept under the conditions of 300~500 DEG C
Hour is warming up to 500~700 DEG C again and is kept for 2~5 hours, is ground up, sieved to obtain the defect carbonitride coupling pucherite after cooling
Composite material.
In addition to this, the present invention also provides a kind of above-mentioned defect carbonitride coupling pucherite catalysis materials to be applied to go
The method of heavy metal ion in water removal, the described method comprises the following steps:
A certain amount of hexavalent chromium wastewater is taken, the hexavalent chromium concentration of the waste water is 0.001~0.1g/L, and adjusting pH value is 1
~12, a certain amount of defect carbonitride coupling pucherite catalysis material is added in waste water, the additive amount in every liter of waste water
It is calculated as 0.05~3g with defect carbonitride coupling pucherite catalysis material weight, is stirred in the magnetic force that revolving speed is 500~1500rpm
It mixes and is reacted 0~8 hour on device, after some time plus illumination is reacted, and sampling is primary at regular intervals, every to take twice
Sample time interval is identical, completes the removal to Cr VI in waste water.
Compared with the prior art, the advantages of the present invention are as follows:
1. raw material sources used in defect carbonitride coupling pucherite catalysis material preparation process of the invention extensively,
It inexpensively and is easy to get, and preparation process is easy, short preparation period, it is easy to accomplish the factorial production.
2. surface defect makes carbonitride have bigger surface area, more light reaction sites are exposed,
Improve the physical adsorption property and light-catalyzed reaction activity of defect carbonitride coupling pucherite catalysis material.
It is environmentally friendly friendly material 3. material of the present invention causes evil effect without intoxicating to human body and environment, it can
It is put into production application with large batch of.
Detailed description of the invention
Fig. 1 is the pictorial diagram of the defect carbonitride coupling pucherite catalysis material of the embodiment of the present invention 1, is in grayish green toner
Last shape.
Specific embodiment
The present invention is described in further details below with reference to Figure of description and specific embodiment.
Embodiment 1:
A kind of preparation method of defect carbonitride coupling pucherite catalysis material of the present invention:
(1) NH of 4.212g is weighed4VO3, the Bi (NO of 17.46g3)3·5H2O is dissolved in the nitric acid of 150mL 2mol/L,
PH value of solution is 2 after adjusting mixing with ammonium hydroxide, and stirring 30min stands two hours or more, and the precipitating of solution bottom is transferred to 100mL
In Teflon inner liner stainless steel autoclave, autoclave is put into baking oven and is heated to 200 DEG C, and keeps 12 by volume accounting 70%
Hour or so, it is cooled to room temperature, obtains pucherite after washing is dry；
(2) 9.25g melamine, 27.75g urea are weighed, and weighs pucherite 1.25g obtained in (1), is added
370mL dehydrated alcohol is mixed 30min in 60 DEG C of water-bath, surplus solution is poured into crucible, puts after closeing the lid
Enter Muffle furnace, 520 DEG C are warming up to after being kept for two hours under the conditions of 500 DEG C and continues to be kept for two hours, is ground up, sieved after cooling
Pucherite catalysis material is coupled to the defect carbonitride.
Defect carbonitride coupling pucherite catalysis material appearance obtained above is in celadon, and appearance is as shown in Figure 1.
Embodiment 2:
Defect carbonitride coupling pucherite catalysis material of the invention is used to go heavy metal ion in water removal, including following
Step:
Taking 200mL concentration is the hexavalent chromium wastewater of 5mg/L, and adjusting pH value of solution with perchloric acid is 2, will be made from embodiment 1
Defect carbonitride coupling pucherite catalysis material is added in wastewater sample, and the additive amount 2.5g in every liter of waste water will react
Device, which is placed on the magnetic stirring apparatus that revolving speed is 1000rpm, to be reacted, and every 30min sampling was primary, at unglazed magnetic agitation 1 hour
Later plus illumination is reacted, and reaction continues 3 hours altogether.The concentration of hexavalent chromium in sample uses ultraviolet spectrophotometry
It is measured, the removal rate of calculating the results are shown in Table 1.
The 1 photocatalysis time of table goes the influence of hexavalent chromium in water removal to defect carbonitride coupling pucherite catalysis material
| The photocatalysis time/min | 0 | 30 | 60 | 90 | 120 |
| Hexavalent chromium removal rate/% | 0 | 83 | 98 | 98 | 98 |
As shown in Table 1, defect carbonitride couples pucherite catalysis material to the removal rate of hexavalent chromium with illumination
Duration increase and increase, and photocatalysis 60min, removal rate can reach 98%, illustrate the material with efficient photocatalysis
Performance.
The above is only the preferred embodiment of the present invention, protection scope of the present invention is not limited merely to above-described embodiment,
Various process programs with present inventive concept without substantial differences are in protection scope of the present invention.
Claims (3)
1. a kind of defect carbonitride couples pucherite catalysis material, by BiVO4With defect g-C3N4It is compound, improve the light of material
Catalytic activity.
2. a kind of preparation method of defect carbonitride coupling pucherite catalysis material as described in claim 1, including it is following
Step:
(1) 10~40g NH is weighed4VO3, 50~120g Bi (NO3)3·5H2O, the nitric acid for being dissolved in 300~1000mL are (described
Nitric acid molar concentration is 1~6mol/L), and pH value of solution is 1~5 after adjusting mixing with ammonium hydroxide, stirs 20~60min and standing two is small
When more than, the precipitating of solution bottom is transferred in 20~100mL Teflon inner liner stainless steel autoclave, volume accounting 50%~
70%, autoclave is put into baking oven and is heated to 150~270 DEG C, and is kept for 8~16 hours, is cooled to room temperature, after washing is dry
Obtain pucherite；
(2) 10~50g melamine, 30~150g urea are weighed, and weighs 1~10g of pucherite obtained in step (1), it is molten
In 300~1000mL dehydrated alcohol, it is stirred 20~80min in 20~80 DEG C of water-bath, outwells extra supernatant,
Surplus solution is dispensed into crucible, is put into Muffle furnace after closeing the lid, kept under the conditions of 300~500 DEG C 2~6 hours again
It is warming up to 500~700 DEG C to be kept for 2~5 hours, is ground up, sieved to obtain the defect carbonitride coupling pucherite composite wood after cooling
Material.
3. a kind of application of defect carbonitride coupling pucherite catalysis material as claimed in claim 2, by claim 2 institute
It is 0.001~0.1g/L's that the defect carbonitride coupling pucherite catalysis material stated, which is added to the mass concentration of 100~500mL,
In hexavalent chromium wastewater, adjusting pH with perchloric acid is 2, and the additive amount in every liter of waste water couples pucherite photocatalysis with defect carbonitride
Material weight is calculated as 0.05~3g, reacts 0~8 hour on the magnetic stirring apparatus that revolving speed is 500~1500rpm, in a timing
Between after plus illumination reacted, sampling is primary at regular intervals, and every two sub-samplings product time interval is identical, uses ultraviolet spectrometry
Photometry measures the surplus of Cr VI in waste water.
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| CN111036274A (en) * | 2019-12-31 | 2020-04-21 | 浙江大学 | Modified BiVO4Preparation method of nanosheet |
| CN111215116A (en) * | 2020-02-10 | 2020-06-02 | 中南林业科技大学 | 3D defect carbon nitride photocatalytic material and preparation method and application thereof |
| CN111364080A (en) * | 2020-03-05 | 2020-07-03 | 中国空间技术研究院 | C for photo-anodexNy/BiVO4Material, preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111036274A (en) * | 2019-12-31 | 2020-04-21 | 浙江大学 | Modified BiVO4Preparation method of nanosheet |
| CN111215116A (en) * | 2020-02-10 | 2020-06-02 | 中南林业科技大学 | 3D defect carbon nitride photocatalytic material and preparation method and application thereof |
| CN111364080A (en) * | 2020-03-05 | 2020-07-03 | 中国空间技术研究院 | C for photo-anodexNy/BiVO4Material, preparation method and application thereof |
| CN111364080B (en) * | 2020-03-05 | 2021-11-16 | 中国空间技术研究院 | C for photo-anodexNy/BiVO4Material, preparation method and application thereof |
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