CN110882688A - Preparation method of photodegradation catalyst for oilfield sewage - Google Patents
Preparation method of photodegradation catalyst for oilfield sewage Download PDFInfo
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- CN110882688A CN110882688A CN201911257392.9A CN201911257392A CN110882688A CN 110882688 A CN110882688 A CN 110882688A CN 201911257392 A CN201911257392 A CN 201911257392A CN 110882688 A CN110882688 A CN 110882688A
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- photodegradation catalyst
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- 239000003054 catalyst Substances 0.000 title claims abstract description 33
- 238000001782 photodegradation Methods 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 239000010865 sewage Substances 0.000 title claims abstract description 14
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 44
- 229910052681 coesite Inorganic materials 0.000 claims abstract description 34
- 229910052906 cristobalite Inorganic materials 0.000 claims abstract description 34
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 34
- 229910052682 stishovite Inorganic materials 0.000 claims abstract description 34
- 229910052905 tridymite Inorganic materials 0.000 claims abstract description 34
- 239000011941 photocatalyst Substances 0.000 claims abstract description 21
- 239000002077 nanosphere Substances 0.000 claims abstract description 17
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000002351 wastewater Substances 0.000 claims abstract description 11
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract 10
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 30
- 238000003756 stirring Methods 0.000 claims description 11
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 10
- 239000002253 acid Substances 0.000 claims description 10
- 238000000498 ball milling Methods 0.000 claims description 10
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 10
- 229910017604 nitric acid Inorganic materials 0.000 claims description 10
- 239000002243 precursor Substances 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- 239000002245 particle Substances 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 claims 1
- 230000001699 photocatalysis Effects 0.000 abstract description 14
- 229920013818 hydroxypropyl guar gum Polymers 0.000 abstract description 7
- 238000012360 testing method Methods 0.000 abstract description 7
- 230000003647 oxidation Effects 0.000 abstract description 6
- 238000007254 oxidation reaction Methods 0.000 abstract description 6
- 238000010521 absorption reaction Methods 0.000 abstract description 2
- 238000011065 in-situ storage Methods 0.000 abstract description 2
- 229910052751 metal Inorganic materials 0.000 abstract description 2
- 239000002184 metal Substances 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 14
- 239000000126 substance Substances 0.000 description 7
- 238000005516 engineering process Methods 0.000 description 5
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 229910052797 bismuth Inorganic materials 0.000 description 3
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 3
- 230000015556 catabolic process Effects 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 238000006731 degradation reaction Methods 0.000 description 3
- 229910052736 halogen Inorganic materials 0.000 description 3
- 150000002367 halogens Chemical class 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000007146 photocatalysis Methods 0.000 description 3
- 239000003642 reactive oxygen metabolite Substances 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 239000002957 persistent organic pollutant Substances 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 229920002907 Guar gum Polymers 0.000 description 1
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 150000001735 carboxylic acids Chemical class 0.000 description 1
- 239000013043 chemical agent Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000005189 flocculation Methods 0.000 description 1
- 230000016615 flocculation Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229960002154 guar gum Drugs 0.000 description 1
- 235000010417 guar gum Nutrition 0.000 description 1
- 239000000665 guar gum Substances 0.000 description 1
- 229910017053 inorganic salt Inorganic materials 0.000 description 1
- 239000010805 inorganic waste Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- VUZPPFZMUPKLLV-UHFFFAOYSA-N methane;hydrate Chemical compound C.O VUZPPFZMUPKLLV-UHFFFAOYSA-N 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 239000011435 rock Substances 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 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
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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/18—Arsenic, antimony or bismuth
-
- B01J35/23—
-
- B01J35/39—
-
- B01J35/51—
-
- B01J35/613—
-
- 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
- C02F2101/34—Organic compounds containing oxygen
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/10—Nature of the water, waste water, sewage or sludge to be treated from quarries or from mining activities
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2209/00—Controlling or monitoring parameters in water treatment
- C02F2209/08—Chemical Oxygen Demand [COD]; Biological Oxygen Demand [BOD]
-
- 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 discloses a preparation method of a photodegradation catalyst for oilfield sewage, which is characterized in that metal Bi is formed on the surface of a TiO2 nanosphere and SiO2/Bi is loaded in situ to prepare a novel SiO2/Bi photodegradation catalyst with excellent photocatalytic performance. Compared with the traditional SiO2/Bi photocatalyst, the photodegradation catalyst has the advantages that the specific surface area is obviously increased, the light forms spherical absorption, the utilization rate of light energy is obviously improved, and the photocatalytic performance is effectively promoted. The SiO2/Bi photodegradation catalyst provided by the invention can better remove hydroxypropyl guar gum in oil field wastewater by photocatalytic oxidation under visible light, and the COD removal rate can reach more than 95% after 1h under test conditions.
Description
Technical Field
The invention relates to the technical field of photodegradation catalysts, in particular to a preparation method of a photodegradation catalyst for oilfield sewage.
Background
Research on methods for treating oil field wastewater generated in the oil field production increasing process has achieved certain achievements at home and abroad, and most of inorganic wastes in the oil field wastewater, such as: rock debris, proppant, inorganic salt and the like can be effectively removed by a series of methods such as physical sedimentation, chemical flocculation and the like. But for polymers in which degradation is difficult, for example: high molecular polymers such as guar gum and the like need to consume a large amount of energy or a large variety of chemical agents for one-to-one degradation, and have the advantages of high treatment cost, large equipment investment, long treatment period and easiness in secondary pollution.
The photocatalysis technology is a new process for treating organic pollutants difficult to degrade developed in the later stage of the 20 th century, and is characterized in that Reactive Oxygen Species (ROS) with extremely strong activity is generated under the action of a semiconductor catalyst, and the ROS can almost indiscriminately oxidize and degrade the organic pollutants difficult to degrade in the wastewater into small molecular substances which are nontoxic or low in toxicity, and even directly mineralize the small molecular substances into carbon dioxide, water and other small molecular carboxylic acids, so that the aim of harmlessness is fulfilled. The technology has the advantages of no selectivity, strong oxidation capability, high reaction speed, high treatment efficiency, no secondary pollution and the like. The characteristics enable the photocatalysis technology to show great application space in the field of processing shale gas flow-back liquid. In the field of photocatalytic technology, the development of photocatalysts is one of the most central technologies. Bismuth oxyhalide has become a new favorite in the field of photocatalysis in recent years.
The Chinese invention patent CN108722445A discloses a bismuth oxyhalide ultrathin solid solution ultrathin bismuth oxyhalide photocatalyst, a preparation method and application thereof, the catalyst has higher specific surface area and is ultrathin, and hydroxypropyl guar gum in oil field wastewater can be better removed by photocatalytic oxidation under visible light, and the preparation method reduces the production cost and simplifies the production process. However, the catalyst contains various halogens, the damage of the halogens to the ozone layer is very serious, and obviously, the catalyst is not suitable for being used as an environment-friendly photodegradation catalyst, so that the invention researches a preparation method of the photodegradation catalyst which does not contain the halogens and can efficiently degrade hydroxypropyl guar gum in the oil field wastewater.
Disclosure of Invention
Based on the technical problems in the background art, the invention provides a preparation method of a photodegradation catalyst for oilfield sewage.
The technical scheme of the invention is as follows:
a preparation method of a photodegradation catalyst for oilfield sewage comprises the following steps:
A. adding Bi (NO)3)3·5H2Dissolving O in 1mol/L nitric acid, and stirring uniformly to obtain Bi (NO)3)3·5H2O acid solution;
B. adding ethylene glycol to the Bi (NO)3)3·5H2Adding into O acid solution, stirring, adding TiO2Nanospheres are uniformly stirred;
C. adding nano SiO2Heating to 50-70 ℃, ball-milling the solution for 30-50min by adopting a wet ball-milling mode, homogenizing at high speed to obtain SiO2A Bi photocatalyst precursor;
D. subjecting the SiO2Performing hydrothermal reaction on the/Bi photocatalyst precursor, centrifuging, washing and drying to obtain SiO2a/Bi photocatalyst.
Preferably, in the step A, Bi (NO) is used3)3·5H2The concentration of O is 0.1-0.3 mol/L.
Preferably, in the step B, the TiO is2The diameter of the nanosphere is 300-600 nm.
Preferably, in the step B, the addition amount of the ethylene glycol is 3-8 times (V/V) of that of the nitric acid, and the TiO is added2The adding amount of the nanospheres is 0.03-0.1 mol/L.
Preferably, in the step C, the nano SiO2Has a particle diameter of 10-30nm and is made of nano SiO2Is added in combination with Bi (NO)3)3·5H2The mass ratio of O is (20-50): 1.
preferably, in the step D, the temperature of the hydrothermal reaction is 180 ℃ and 250 ℃, and the time is 8-15 h.
The invention has the advantages that: the invention provides a preparation method of a photodegradation catalyst for oilfield sewage, which is prepared from TiO2In-situ loaded SiO on metal Bi formed on the surface of nanosphere2Bi to produce novel SiO with excellent photocatalytic properties2a/Bi photodegradation catalyst. Compared with the traditional SiO, the photodegradation catalyst2The specific surface area of the/Bi photocatalyst is obviously increased, and spherical absorption is formed for light, so that the specific surface area is obviously improvedThe utilization rate of light energy effectively promotes the photocatalytic performance. The SiO provided by the invention2the/Bi photodegradation catalyst can better remove hydroxypropyl guar gum in the oil field wastewater by photocatalytic oxidation under visible light, and the COD removal rate can reach more than 95% after 1 hour under the test condition.
Detailed Description
Example 1
A preparation method of a photodegradation catalyst for oilfield sewage comprises the following steps:
A. adding Bi (NO)3)3·5H2Dissolving O in 1L of nitric acid of 1mol/L, and uniformly stirring to obtain Bi (NO)3)3·5H2O acid solution;
B. adding ethylene glycol to the Bi (NO)3)3·5H2Adding into O acid solution, stirring, adding TiO2Nanospheres are uniformly stirred;
C. adding nano SiO2Heating to 65 ℃, ball-milling the solution for 45min by adopting a wet ball-milling mode, and homogenizing at high speed to obtain SiO2A Bi photocatalyst precursor;
D. subjecting the SiO2Performing hydrothermal reaction on the/Bi photocatalyst precursor, centrifuging, washing and drying to obtain SiO2a/Bi photocatalyst.
In the step A, the Bi (NO)3)3·5H2The concentration of O was 0.15 mol/L.
In the step B, the TiO2The diameter of the nanosphere is 300-600 nm.
In the step B, the addition amount of the ethylene glycol is 6 times (V/V) of that of the nitric acid, and the TiO is2The adding amount of the nanospheres is 0.08 mol/L.
In the step C, the nano SiO2Has a particle diameter of 10-30nm and is made of nano SiO2Is added in combination with Bi (NO)3)3·5H2The mass ratio of O is 35: 1.
in the step D, the temperature of the hydrothermal reaction is 220 ℃ and the time is 12 hours.
Example 2
A preparation method of a photodegradation catalyst for oilfield sewage comprises the following steps:
A. adding Bi (NO)3)3·5H2Dissolving O in 1L of nitric acid of 1mol/L, and uniformly stirring to obtain Bi (NO)3)3·5H2O acid solution;
B. adding ethylene glycol to the Bi (NO)3)3·5H2Adding into O acid solution, stirring, adding TiO2Nanospheres are uniformly stirred;
C. adding nano SiO2Heating to 70 ℃, ball-milling the solution for 30min by adopting a wet ball-milling mode, and homogenizing at high speed to obtain SiO2A Bi photocatalyst precursor;
D. subjecting the SiO2Performing hydrothermal reaction on the/Bi photocatalyst precursor, centrifuging, washing and drying to obtain SiO2a/Bi photocatalyst.
In the step A, the Bi (NO)3)3·5H2The concentration of O was 0.1 mol/L.
In the step B, the TiO2The diameter of the nanosphere is 300-600 nm.
In the step B, the addition amount of the ethylene glycol is 8 times (V/V) of that of the nitric acid, and the TiO is2The adding amount of the nanospheres is 0.03 mol/L.
In the step C, the nano SiO2Has a particle diameter of 10-30nm and is made of nano SiO2Is added in combination with Bi (NO)3)3·5H2The mass ratio of O is 50: 1.
in the step D, the temperature of the hydrothermal reaction is 180 ℃ and the time is 15 h.
Example 3
A preparation method of a photodegradation catalyst for oilfield sewage comprises the following steps:
A. adding Bi (NO)3)3·5H2Dissolving O in 1L of nitric acid of 1mol/L, and uniformly stirring to obtain Bi (NO)3)3·5H2O acid solution;
B. adding ethylene glycol to the Bi (NO)3)3·5H2Adding into O acid solution, stirring, adding TiO2Nanospheres are uniformly stirred;
C. adding nano SiO2Heating to 50 ℃, ball-milling the solution for 50min by adopting a wet ball-milling mode, and homogenizing at high speed to obtain SiO2A Bi photocatalyst precursor;
D. subjecting the SiO2Performing hydrothermal reaction on the/Bi photocatalyst precursor, centrifuging, washing and drying to obtain SiO2a/Bi photocatalyst.
In the step A, the Bi (NO)3)3·5H2The concentration of O was 0.3 mol/L.
In the step B, the TiO2The diameter of the nanosphere is 300-600 nm.
In the step B, the addition amount of the ethylene glycol is 3 times (V/V) of that of the nitric acid, and the TiO is2The adding amount of the nanospheres is 0.1 mol/L.
In the step C, the nano SiO2Has a particle diameter of 10-30nm and is made of nano SiO2Is added in combination with Bi (NO)3)3·5H2The mass ratio of O is 20: 1.
in the step D, the temperature of the hydrothermal reaction is 250 ℃ and the time is 8 h.
Comparative example 1
The photocatalyst prepared in example 1 of the Chinese patent CN 108722445A.
Comparative example 2
The photocatalyst prepared in example 1 of the Chinese patent CN 106000389A.
Photocatalytic activity test:
the photocatalytic activity test is characterized by removing hydroxypropyl guar gum in the oil field wastewater through oxidation under visible light, wherein a 500W xenon lamp is used as a light source, visible light in the range of 420-780nm is obtained through an optical filter, the dosage of a catalyst is 0.05g each time, the original COD of a hydroxypropyl guar gum solution is controlled to be 200mg/L, the COD after catalytic oxidation is measured by a water quality analyzer, the sampling amount is 1mL, and specific test data are shown in Table 1.
Wherein, COD is chemical oxygen demand (chemical oxygen demand), and is used for measuring the amount of reducing substances needing to be oxidized in a water sample by a chemical method.
Water quality Analyzer model No. DR6100A was obtained from Seisan Pop Biotech Co., Ltd.
Table 1: photocatalytic activity test results of the catalyst samples prepared in examples 1 to 3 and comparative example 1;
the test data show that the photodegradation catalyst prepared by the preparation method of the photodegradation catalyst for oilfield sewage has a very good catalytic degradation effect on hydroxypropyl guar gum.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (6)
1. A preparation method of a photodegradation catalyst for oilfield sewage is characterized by comprising the following steps:
A. dissolving Bi (NO3) 3.5H 2O in 1mol/L nitric acid, and uniformly stirring to obtain a Bi (NO3) 3.5H 2O acid solution;
B. adding ethylene glycol into the acid solution of Bi (NO3) 3.5H 2O, uniformly stirring, adding TiO2 nanospheres, and uniformly stirring;
C. adding nano SiO2, heating to 50-70 ℃, ball-milling the solution for 30-50min by adopting a wet ball-milling mode, and homogenizing at high speed to obtain a SiO2/Bi photocatalyst precursor;
D. and carrying out hydrothermal reaction on the SiO2/Bi photocatalyst precursor, centrifuging, washing and drying to obtain the SiO2/Bi photocatalyst.
2. The method for preparing the photodegradation catalyst for oilfield wastewater of claim 1, wherein in the step A, the concentration of Bi (NO3) 3.5H 2O is 0.1-0.3 mol/L.
3. The method for preparing the photodegradation catalyst for oilfield sewage as claimed in claim 1, wherein in the step B, the TiO2 nanospheres are titanium dioxide nanospheres with a diameter of 300-600 nm.
4. The method for preparing the photodegradation catalyst for oilfield sewage of claim 1, wherein in the step B, the addition amount of the ethylene glycol is 3-8 times (V/V) of the nitric acid, and the addition amount of the TiO2 nanospheres is 0.03-0.1 mol/L.
5. The method for preparing the photodegradation catalyst for oilfield wastewater as claimed in claim 1, wherein in the step C, the particle size of the nano SiO2 is 10-30nm, and the mass ratio of the added amount of the nano SiO2 to the Bi (NO3) 3.5H 2O is (20-50): 1.
6. the method for preparing the photodegradation catalyst for oilfield wastewater as claimed in claim 1, wherein in the step D, the temperature of the hydrothermal reaction is 180-250 ℃ and the time is 8-15 h.
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| CN201911257392.9A CN110882688A (en) | 2019-12-10 | 2019-12-10 | Preparation method of photodegradation catalyst for oilfield sewage |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114011407A (en) * | 2022-01-04 | 2022-02-08 | 天津市职业大学 | Photocatalytic material for treating oil field wastewater and preparation method and application thereof |
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| CN106000389A (en) * | 2016-07-13 | 2016-10-12 | 重庆工商大学 | Photocatalyst and preparation method thereof |
| CN107469804A (en) * | 2016-06-08 | 2017-12-15 | 中国科学院金属研究所 | A kind of titania-based composite photocatalyst material of nano particle bismuth load and its preparation method and application |
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2019
- 2019-12-10 CN CN201911257392.9A patent/CN110882688A/en active Pending
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| US20110266136A1 (en) * | 2010-04-30 | 2011-11-03 | Varma Rajender S | Doped titanium dioxide as a visible and sun light photo catalyst |
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Application publication date: 20200317 |