CN107321375A - A kind of SiO2/ZnO/g‑C3N4Nano material and its application in reduction of hexavalent chromium - Google Patents
A kind of SiO2/ZnO/g‑C3N4Nano material and its application in reduction of hexavalent chromium Download PDFInfo
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- CN107321375A CN107321375A CN201710572468.1A CN201710572468A CN107321375A CN 107321375 A CN107321375 A CN 107321375A CN 201710572468 A CN201710572468 A CN 201710572468A CN 107321375 A CN107321375 A CN 107321375A
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 29
- 229910052681 coesite Inorganic materials 0.000 title claims abstract description 15
- 229910052906 cristobalite Inorganic materials 0.000 title claims abstract description 15
- 239000000377 silicon dioxide Substances 0.000 title claims abstract description 15
- 229910052682 stishovite Inorganic materials 0.000 title claims abstract description 15
- 229910052905 tridymite Inorganic materials 0.000 title claims abstract description 15
- 235000012239 silicon dioxide Nutrition 0.000 title claims description 3
- JOPOVCBBYLSVDA-UHFFFAOYSA-N chromium(6+) Chemical compound [Cr+6] JOPOVCBBYLSVDA-UHFFFAOYSA-N 0.000 title abstract description 9
- 239000000463 material Substances 0.000 title description 5
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 28
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 claims abstract description 28
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 25
- 238000001556 precipitation Methods 0.000 claims abstract description 25
- 239000002086 nanomaterial Substances 0.000 claims abstract description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000008367 deionised water Substances 0.000 claims abstract description 17
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 17
- 238000003756 stirring Methods 0.000 claims abstract description 17
- 238000010438 heat treatment Methods 0.000 claims abstract description 16
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229920000877 Melamine resin Polymers 0.000 claims abstract description 13
- 238000005119 centrifugation Methods 0.000 claims abstract description 13
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000006243 chemical reaction Methods 0.000 claims abstract description 10
- 238000009413 insulation Methods 0.000 claims abstract description 8
- 239000004570 mortar (masonry) Substances 0.000 claims abstract description 8
- 238000002360 preparation method Methods 0.000 claims abstract description 8
- 238000002791 soaking Methods 0.000 claims abstract description 8
- 238000010531 catalytic reduction reaction Methods 0.000 claims description 5
- 230000001699 photocatalysis Effects 0.000 claims description 5
- 238000002242 deionisation method Methods 0.000 claims description 3
- 239000003643 water by type Substances 0.000 claims description 3
- XZMCDFZZKTWFGF-UHFFFAOYSA-N Cyanamide Chemical compound NC#N XZMCDFZZKTWFGF-UHFFFAOYSA-N 0.000 claims 1
- 150000002148 esters Chemical class 0.000 claims 1
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims 1
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 34
- 239000011787 zinc oxide Substances 0.000 description 17
- 239000000047 product Substances 0.000 description 16
- 239000011651 chromium Substances 0.000 description 9
- 239000000243 solution Substances 0.000 description 9
- 238000006722 reduction reaction Methods 0.000 description 7
- 230000000694 effects Effects 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- -1 microballoon Substances 0.000 description 3
- 239000002244 precipitate Substances 0.000 description 3
- 230000003595 spectral effect Effects 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- XYIBRDXRRQCHLP-UHFFFAOYSA-N ethyl acetoacetate Chemical compound CCOC(=O)CC(C)=O XYIBRDXRRQCHLP-UHFFFAOYSA-N 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000004070 electrodeposition Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 239000002071 nanotube Substances 0.000 description 1
- 239000002070 nanowire Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 238000006068 polycondensation reaction Methods 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000010532 solid phase synthesis reaction Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000012086 standard solution Substances 0.000 description 1
- 239000012808 vapor phase Substances 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
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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
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/24—Nitrogen compounds
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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
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/06—Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
- B01J21/08—Silica
-
- 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
- B01J23/06—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of zinc, cadmium or mercury
-
- 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
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- Engineering & Computer Science (AREA)
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- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Nanotechnology (AREA)
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- Condensed Matter Physics & Semiconductors (AREA)
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Abstract
The present invention relates to a kind of SiO2/ZnO/g‑C3N4Nano material and its application in reduction of hexavalent chromium, and in particular to a kind of SiO2/ZnO/g‑C3N4Nano material, its preparation method comprises the following steps:(1) zinc nitrate is dissolved in appropriate deionized water, adds ammoniacal liquor, stirring reaction is after 12 hours at room temperature, centrifugation must be precipitated;(2) the precipitation ultrasonic disperse for obtaining step (1) adds appropriate ammoniacal liquor, tetraethyl orthosilicate (TEOS) in ethanol, and stirring at room temperature is added 34 hours, and centrifugation must be precipitated;(3) precipitation and melamine obtained step (2), with mortar grinder it is uniform after, be put into Muffle furnace, temperature is set as 510 DEG C, 10 DEG C/min of heating rate, soaking time 120 minutes, after insulation terminates, stop heating and naturally cool to room temperature, obtain the SiO2/ZnO/g‑C3N4Nano material.
Description
Technical field
The invention belongs to technical field of material chemistry, it is related to a kind of SiO2/ZnO/g-C3N4Nano material and its in reduction of hexavalent chromium
In application.
Background technology
g-C3N4Preparation method have vapor phase method, hot solvent method, solid-phase synthesis, electrochemical deposition method, high temperature and high pressure method
Deng it is to prepare g-C using polycondensation organic matter precursor to study in recent years more3N4.In addition, people have also synthesized different morphologies
Carbonitride, including nano wire, nanotube, microballoon, fiber and hollow ball etc..
g-C3N4With raw material resources is abundant, cheap economy, environmental protection the features such as.With it is micro-/receive porous g-
C3N4Structure for it is micro-/receive porous and while have photo-catalysis capability, and the ability being combined with other metal materials.Nanometer g-
C3N4Also higher surface-active, is preferable catalyst material, so relevant g-C3N4Research all extremely people always
Concern.But the g-C with micro-/nano porous structure of current most of preparations3N4With nanometer g-C3N4There is specific surface area small, living
The low shortcoming of property, composite is not too much more, thus limits its popularizing in practice.Feelings in view of the above
Condition, the present invention prepares new SiO using pyrolysismethod2/ZnO/g-C3N4Nano material, it has, and specific surface area is big, photo catalytic reduction
The features such as effect is good.
The content of the invention
The present invention provides a kind of SiO2/ZnO/g-C3N4Nano material, it is characterised in that the preparation method bag of the nano material
Include following steps:
(1) zinc nitrate is dissolved in appropriate deionized water, adds ammoniacal liquor, at room temperature after stirring reaction 1-2 hours, from
The heart, must be precipitated;
(2) the precipitation ultrasonic disperse for obtaining step (1) adds appropriate ammoniacal liquor, tetraethyl orthosilicate (TEOS) in ethanol,
Stirring is added 3-4 hours at room temperature, centrifugation, must be precipitated;
(3) precipitation and melamine obtained step (2), with mortar grinder it is uniform after, be put into Muffle furnace, temperature is set
It is set to 510 DEG C, 10 DEG C/min of heating rate, soaking time 120 minutes after insulation terminates, stops heating and naturally cools to room temperature,
Obtain the SiO2/ZnO/g-C3N4Nano material.
In above-mentioned preparation method, the precipitation that step (1) or (2) are obtained is preferred to use deionization and washed 2-3 times;Step (1)
Middle zinc nitrate, deionized water, the consumption of ammoniacal liquor use 5-10mL deionized waters, 2-3mL ammoniacal liquor for every gram of zinc nitrate;Step (2)
Middle ethanol, ammoniacal liquor, the consumption of tetraethyl orthosilicate use 8-12mL ethanol, 1-2mL ammoniacal liquor, the positive silicon of 0.8-1.6mL for every gram of precipitation
Acetoacetic ester;The consumption of melamine is that every gram of precipitation uses 10-100 grams of melamine in step (3).
Another embodiment of the present invention provides above-mentioned SiO2/ZnO/g-C3N4The preparation method of nano material, its feature exists
In comprising the following steps:
(1) zinc nitrate is dissolved in appropriate deionized water, adds ammoniacal liquor, at room temperature after stirring reaction 1-2 hours, from
The heart, must be precipitated;
(2) the precipitation ultrasonic disperse for obtaining step (1) adds appropriate ammoniacal liquor, tetraethyl orthosilicate (TEOS) in ethanol,
Stirring is added 3-4 hours at room temperature, centrifugation, must be precipitated;
(3) precipitation and melamine obtained step (2), with mortar grinder it is uniform after, be put into Muffle furnace, temperature is set
It is set to 510 DEG C, 10 DEG C/min of heating rate, soaking time 120 minutes after insulation terminates, stops heating and naturally cools to room temperature,
Obtain the SiO2/ZnO/g-C3N4Nano material.
In above-mentioned preparation method, the precipitation that step (1) or (2) are obtained is preferred to use deionization and washed 2-3 times;Step (1)
Middle zinc nitrate, deionized water, the consumption of ammoniacal liquor use 5-10mL deionized waters, 2-3mL ammoniacal liquor for every gram of zinc nitrate;Step (2)
Middle ethanol, ammoniacal liquor, the consumption of tetraethyl orthosilicate use 8-12mL ethanol, 1-2mL ammoniacal liquor, the positive silicon of 0.8-1.6mL for every gram of precipitation
Acetoacetic ester;The consumption of melamine is that every gram of precipitation uses 10-100 grams of melamine in step (3).
Another embodiment of the present invention provides above-mentioned SiO2/ZnO/g-C3N4Nano material is in photo catalytic reduction Cr VI
In application.
The ammoniacal liquor used in the present invention is the aqueous solution containing ammonia 25%~28%.
Compared with prior art the advantage of the invention is that:(1) SiO prepared by the present invention2/ZnO/g-C3N4Nano material,
It has specific surface area big, the features such as photo catalytic reduction effect is good;(2) SiO prepared by the present invention2/ZnO/g-C3N4Light irradiation
After 2.5 hours, the content of Cr VI is less than 10% in solution, better than g-C3N4And ZnO/g-C3N4Photo catalytic reduction effect (light
After irradiation 2.5 hours, the content of Cr VI is higher than 20%) in solution.
Brief description of the drawings
Fig. 1 schemes for product A SEM;
Fig. 2 schemes for product B SEM;
Fig. 3 schemes for the SEM of products C;
Fig. 4 schemes for product D SEM;
Fig. 5 is product A, B, C, D, zinc oxide, g-C3N4、SiO2To the reducing power of Cr VI, C0
For original Cr in solution6+Concentration, Ct be different time points Cr6+Concentration;
Fig. 6 is the spectral absorption figure that product A is catalyzed reduction of hexavalent chromium solution;
Fig. 7 is the spectral absorption figure that product B is catalyzed reduction of hexavalent chromium solution;
Specific embodiment
For the ease of a further understanding of the present invention, examples provided below has done more detailed description to it.But
It is that these embodiments only are not used for limiting the scope of the present invention or implementation principle, reality of the invention for being better understood from invention
The mode of applying is not limited to herein below.
Embodiment 1
(1) weigh zinc nitrate (1.0g) to be dissolved in appropriate deionized water (5mL), add ammoniacal liquor (2mL), stir at room temperature
After reaction 1-2 hours, centrifugation must be precipitated, is washed with deionized water 2-3 times;
(2) precipitation ultrasonic disperse that 0.8g steps (1) obtain is weighed in ethanol (6.4mL), adds appropriate ammoniacal liquor
(0.8mL), tetraethyl orthosilicate (0.64mL), at room temperature stirring is added 3-4 hours, and centrifugation must precipitate, 2-3 is washed with deionized water
It is secondary;
(3) precipitation and melamine (10g) that 1.0g steps (2) obtain are weighed, with mortar grinder it is uniform after, be put into Muffle
In stove, temperature is set as 510 DEG C, and 10 DEG C/min of heating rate, soaking time 120 minutes after insulation terminates, stops heating nature
Room temperature is cooled to, SiO is obtained2/ZnO/g-C3N4Nano material (hereinafter referred to as product A, Fig. 1).
Embodiment 2
(1) weigh zinc nitrate (1.0g) to be dissolved in appropriate deionized water (10mL), add ammoniacal liquor (3mL), stir at room temperature
After mixing reaction 1-2 hours, centrifugation must be precipitated, is washed with deionized water 2-3 times;
(2) precipitation ultrasonic disperse that 0.8g steps (1) obtain is weighed in ethanol (9.6mL), adds appropriate ammoniacal liquor
(1.6mL), tetraethyl orthosilicate (1.28mL), at room temperature stirring is added 3-4 hours, and centrifugation must precipitate, 2-3 is washed with deionized water
It is secondary;
(3) precipitation and melamine (100g) that 1.0g steps (2) obtain are weighed, with mortar grinder it is uniform after, be put into horse
Not in stove, temperature is set as 510 DEG C, and 10 DEG C/min of heating rate, soaking time 120 minutes after insulation terminates, stops heating certainly
Room temperature so is cooled to, SiO is obtained2/ZnO/g-C3N4Nano material (hereinafter referred to as product B, Fig. 2).
Embodiment 3
(1) weigh zinc nitrate (1.0g) to be dissolved in appropriate deionized water (5mL), add ammoniacal liquor (2mL), stir at room temperature
After reaction 1-2 hours, centrifugation must be precipitated, is washed with deionized water 2-3 times;
(2) precipitation and melamine (10g) that 1.0g steps (1) obtain are weighed, with mortar grinder it is uniform after, be put into Muffle
In stove, temperature is set as 510 DEG C, and 10 DEG C/min of heating rate, soaking time 120 minutes after insulation terminates, stops heating nature
Room temperature is cooled to, ZnO/g-C is obtained3N4Material (hereinafter referred to as products C, Fig. 3).
Embodiment 4
(1) weigh zinc nitrate (1.0g) to be dissolved in appropriate deionized water (10mL), add ammoniacal liquor (3mL), stir at room temperature
After mixing reaction 1-2 hours, centrifugation must be precipitated, is washed with deionized water 2-3 times;
(2) precipitation ultrasonic disperse that 0.8g steps (1) obtain is weighed in ethanol (9.6mL), adds appropriate ammoniacal liquor
(1.6mL), tetraethyl orthosilicate (1.28mL), at room temperature stirring is added 3-4 hours, and centrifugation must precipitate, 2-3 is washed with deionized water
It is secondary;
(3) precipitation and melamine (200g) that 1.0g steps (2) obtain are weighed, with mortar grinder it is uniform after, be put into horse
Not in stove, temperature is set as 510 DEG C, and 10 DEG C/min of heating rate, soaking time 120 minutes after insulation terminates, stops heating certainly
Room temperature so is cooled to, SiO is obtained2/ZnO/g-C3N4Nano material (hereinafter referred to as product D, Fig. 4).
Embodiment 5 is catalyzed reduction of hexavalent chromium
Take 200ml sexavalences chromium standard solution, 1 milliliter of citric acid solution, be separately added into 0.2g products A, B, C, D, zinc oxide,
g-C3N4、SiO2, using 500W xenon lamps and 420nm optical filters as visible light source, first each stirring reaction 1 hour in dark room conditions,
Stirring reaction of turning on light again 3.5 hours;Test result indicates that product A, B of the present invention are better than products C, D to the reduction effect of Cr VI
And g-C3N4, when light irradiation 2.5 is small after, in solution the content of Cr VI less than 10%, especially product A when light irradiation 2.5 it is small
The content of Cr VI is less than 3% (result is shown in Fig. 5) in Shi Hou, solution.Product A, B are catalyzed the spectral absorption of reduction of hexavalent chromium solution
Figure is (see Fig. 6,7).
Claims (6)
1. a kind of SiO2/ZnO/g-C3N4Nano material, it is characterised in that the preparation method of the nano material comprises the following steps:
(1) zinc nitrate is dissolved in appropriate deionized water, adds ammoniacal liquor, at room temperature after stirring reaction 1-2 hours, centrifugation is obtained
Precipitation;
(2) the precipitation ultrasonic disperse for obtaining step (1) adds appropriate ammoniacal liquor, tetraethyl orthosilicate (TEOS), room temperature in ethanol
Lower stirring is added 3-4 hours, and centrifugation must be precipitated;
(3) precipitation and melamine obtained step (2), with mortar grinder it is uniform after, be put into Muffle furnace, temperature is set as
510 DEG C, 10 DEG C/min of heating rate, soaking time 120 minutes after insulation terminates, stops heating and naturally cools to room temperature, obtain
The SiO2/ZnO/g-C3N4Nano material.
2. the SiO described in claim 12/ZnO/g-C3N4Nano material, it is characterised in that what the step (1) or (2) were obtained
Precipitation is preferred to use deionization and washed 2-3 times.
3. the SiO described in claim 12/ZnO/g-C3N4Nano material, it is characterised in that zinc nitrate in the step (1), go
Ionized water, the consumption of ammoniacal liquor use 5-10mL deionized waters, 2-3mL ammoniacal liquor for every gram of zinc nitrate.
4. the SiO described in claim any one of 1-32/ZnO/g-C3N4Nano material, it is characterised in that second in the step (2)
Alcohol, ammoniacal liquor, the consumption of tetraethyl orthosilicate use 8-12mL ethanol, 1-2mL ammoniacal liquor, the positive silicic acid second of 0.8-1.6mL for every gram of precipitation
Ester.
5. the SiO described in claim any one of 1-42/ZnO/g-C3N4Nano material, it is characterised in that three in the step (3)
The consumption of poly cyanamid is that every gram of precipitation uses 10-100 grams of melamine.
6. the SiO described in claim any one of 1-52/ZnO/g-C3N4Nano material answering in photo catalytic reduction Cr VI
With.
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