CN111408377A - NiTi nano-flower hydrotalcite photocatalyst and preparation method and application thereof - Google Patents
NiTi nano-flower hydrotalcite photocatalyst and preparation method and application thereof Download PDFInfo
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- CN111408377A CN111408377A CN201911156814.3A CN201911156814A CN111408377A CN 111408377 A CN111408377 A CN 111408377A CN 201911156814 A CN201911156814 A CN 201911156814A CN 111408377 A CN111408377 A CN 111408377A
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- nickel
- hydrotalcite
- photocatalyst
- titanium
- salt
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- 239000011941 photocatalyst Substances 0.000 title claims abstract description 74
- 229960001545 hydrotalcite Drugs 0.000 title claims abstract description 71
- 229910001701 hydrotalcite Inorganic materials 0.000 title claims abstract description 71
- GDVKFRBCXAPAQJ-UHFFFAOYSA-A dialuminum;hexamagnesium;carbonate;hexadecahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Al+3].[Al+3].[O-]C([O-])=O GDVKFRBCXAPAQJ-UHFFFAOYSA-A 0.000 title claims abstract description 68
- 229910001000 nickel titanium Inorganic materials 0.000 title claims abstract description 68
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- 239000002057 nanoflower Substances 0.000 title claims description 55
- SRBFZHDQGSBBOR-IOVATXLUSA-N D-xylopyranose Chemical compound O[C@@H]1COC(O)[C@H](O)[C@H]1O SRBFZHDQGSBBOR-IOVATXLUSA-N 0.000 claims abstract description 62
- HZEWFHLRYVTOIW-UHFFFAOYSA-N [Ti].[Ni] Chemical compound [Ti].[Ni] HZEWFHLRYVTOIW-UHFFFAOYSA-N 0.000 claims abstract description 55
- 238000006243 chemical reaction Methods 0.000 claims abstract description 52
- 238000010438 heat treatment Methods 0.000 claims abstract description 39
- QXKAIJAYHKCRRA-UHFFFAOYSA-N D-lyxonic acid Natural products OCC(O)C(O)C(O)C(O)=O QXKAIJAYHKCRRA-UHFFFAOYSA-N 0.000 claims abstract description 33
- QXKAIJAYHKCRRA-FLRLBIABSA-N D-xylonic acid Chemical compound OC[C@@H](O)[C@H](O)[C@@H](O)C(O)=O QXKAIJAYHKCRRA-FLRLBIABSA-N 0.000 claims abstract description 33
- PYMYPHUHKUWMLA-UHFFFAOYSA-N arabinose Natural products OCC(O)C(O)C(O)C=O PYMYPHUHKUWMLA-UHFFFAOYSA-N 0.000 claims abstract description 31
- SRBFZHDQGSBBOR-UHFFFAOYSA-N beta-D-Pyranose-Lyxose Natural products OC1COC(O)C(O)C1O SRBFZHDQGSBBOR-UHFFFAOYSA-N 0.000 claims abstract description 31
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 26
- 238000000034 method Methods 0.000 claims abstract description 23
- VKYKSIONXSXAKP-UHFFFAOYSA-N hexamethylenetetramine Chemical compound C1N(C2)CN3CN1CN2C3 VKYKSIONXSXAKP-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000000047 product Substances 0.000 claims abstract description 19
- 238000001816 cooling Methods 0.000 claims abstract description 16
- 238000001035 drying Methods 0.000 claims abstract description 16
- 150000002815 nickel Chemical class 0.000 claims abstract description 12
- 150000003608 titanium Chemical class 0.000 claims abstract description 12
- 230000003197 catalytic effect Effects 0.000 claims abstract description 11
- 238000003756 stirring Methods 0.000 claims abstract description 4
- 239000000243 solution Substances 0.000 claims description 43
- 239000002244 precipitate Substances 0.000 claims description 26
- 239000011259 mixed solution Substances 0.000 claims description 13
- DCKVFVYPWDKYDN-UHFFFAOYSA-L oxygen(2-);titanium(4+);sulfate Chemical compound [O-2].[Ti+4].[O-]S([O-])(=O)=O DCKVFVYPWDKYDN-UHFFFAOYSA-L 0.000 claims description 13
- 229910000348 titanium sulfate Inorganic materials 0.000 claims description 13
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- 239000012670 alkaline solution Substances 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 9
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 4
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims description 4
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 4
- 239000002135 nanosheet Substances 0.000 claims description 3
- 229910052759 nickel Inorganic materials 0.000 claims description 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 2
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 claims description 2
- SMWCOYAMRBMIII-UHFFFAOYSA-N O.O.O.O.O.[N+](=O)([O-])[O-].[Ni+2].[N+](=O)([O-])[O-] Chemical compound O.O.O.O.O.[N+](=O)([O-])[O-].[Ni+2].[N+](=O)([O-])[O-] SMWCOYAMRBMIII-UHFFFAOYSA-N 0.000 claims description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 2
- 238000001914 filtration Methods 0.000 claims description 2
- 235000010299 hexamethylene tetramine Nutrition 0.000 claims description 2
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 claims description 2
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 claims description 2
- UQPSGBZICXWIAG-UHFFFAOYSA-L nickel(2+);dibromide;trihydrate Chemical compound O.O.O.Br[Ni]Br UQPSGBZICXWIAG-UHFFFAOYSA-L 0.000 claims description 2
- KERTUBUCQCSNJU-UHFFFAOYSA-L nickel(2+);disulfamate Chemical compound [Ni+2].NS([O-])(=O)=O.NS([O-])(=O)=O KERTUBUCQCSNJU-UHFFFAOYSA-L 0.000 claims description 2
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 claims description 2
- BFDHFSHZJLFAMC-UHFFFAOYSA-L nickel(ii) hydroxide Chemical compound [OH-].[OH-].[Ni+2] BFDHFSHZJLFAMC-UHFFFAOYSA-L 0.000 claims description 2
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims description 2
- 235000017557 sodium bicarbonate Nutrition 0.000 claims description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 2
- LLZRNZOLAXHGLL-UHFFFAOYSA-J titanic acid Chemical compound O[Ti](O)(O)O LLZRNZOLAXHGLL-UHFFFAOYSA-J 0.000 claims description 2
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 claims description 2
- YONPGGFAJWQGJC-UHFFFAOYSA-K titanium(iii) chloride Chemical compound Cl[Ti](Cl)Cl YONPGGFAJWQGJC-UHFFFAOYSA-K 0.000 claims description 2
- 239000003054 catalyst Substances 0.000 abstract description 31
- 238000006555 catalytic reaction Methods 0.000 abstract description 7
- 239000006227 byproduct Substances 0.000 abstract description 5
- 230000015572 biosynthetic process Effects 0.000 abstract 1
- 238000003786 synthesis reaction Methods 0.000 abstract 1
- -1 polytetrafluoroethylene Polymers 0.000 description 33
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 33
- 239000004810 polytetrafluoroethylene Substances 0.000 description 33
- 239000011521 glass Substances 0.000 description 13
- 239000008367 deionised water Substances 0.000 description 11
- 229910021641 deionized water Inorganic materials 0.000 description 11
- AOPCKOPZYFFEDA-UHFFFAOYSA-N nickel(2+);dinitrate;hexahydrate Chemical compound O.O.O.O.O.O.[Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O AOPCKOPZYFFEDA-UHFFFAOYSA-N 0.000 description 11
- 238000000967 suction filtration Methods 0.000 description 11
- 230000003647 oxidation Effects 0.000 description 8
- 238000007254 oxidation reaction Methods 0.000 description 8
- 229910021642 ultra pure water Inorganic materials 0.000 description 8
- 239000012498 ultrapure water Substances 0.000 description 8
- 229910052724 xenon Inorganic materials 0.000 description 6
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 6
- 239000000126 substance Substances 0.000 description 5
- 238000005303 weighing Methods 0.000 description 5
- 239000012295 chemical reaction liquid Substances 0.000 description 4
- 238000007865 diluting Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 3
- 239000000835 fiber Substances 0.000 description 3
- 238000001027 hydrothermal synthesis Methods 0.000 description 3
- 238000005286 illumination Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000013032 photocatalytic reaction Methods 0.000 description 3
- 239000002028 Biomass Substances 0.000 description 2
- 229920002488 Hemicellulose Polymers 0.000 description 2
- 239000002585 base Substances 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 239000001913 cellulose Substances 0.000 description 2
- 229920002678 cellulose Polymers 0.000 description 2
- 230000003247 decreasing effect Effects 0.000 description 2
- 238000000855 fermentation Methods 0.000 description 2
- 230000004151 fermentation Effects 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 235000000346 sugar Nutrition 0.000 description 2
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 description 2
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 1
- 238000003917 TEM image Methods 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 150000001323 aldoses Chemical class 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000008103 glucose Substances 0.000 description 1
- 239000004312 hexamethylene tetramine Substances 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 239000008104 plant cellulose Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012552 review Methods 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 150000008163 sugars Chemical class 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
Images
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
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/74—Iron group metals
- B01J23/755—Nickel
-
- B01J35/39—
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/10—Heat treatment in the presence of water, e.g. steam
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/16—Preparation of carboxylic acids or their salts, halides or anhydrides by oxidation
- C07C51/295—Preparation of carboxylic acids or their salts, halides or anhydrides by oxidation with inorganic bases, e.g. by alkali fusion
Abstract
The invention discloses a NiTi hydrotalcite photocatalyst and a preparation method and application thereof. The catalyst is three-dimensional NiTi nano-meter, and the diameter of the nano-meter flower is 6-7 μm. The preparation method comprises the following steps: dissolving titanium salt, nickel salt and urotropine in water, and stirring the solution to be transparent; heating the reaction system for reaction; and cooling and drying the heated product to obtain the nickel-titanium nano-hydrotalcite photocatalyst, wherein the nickel-titanium nano-hydrotalcite photocatalyst can be used for catalyzing xylose to be converted into xylonic acid. The invention has simple synthesis in the aspect of preparing the catalyst, high-temperature heating is not needed, and the synthesized catalyst can be directly used for catalytic reaction without subsequent treatment. The catalyst provided by the invention has the potential of industrialization, the cost of the catalytic process is low, the catalyst is different from the traditional thermal catalysis, the process is green and environment-friendly, and no harmful by-product is generated.
Description
Technical Field
The invention belongs to the cross technical field of catalytic materials, photocatalysis and conversion of biomass into chemicals, and particularly relates to a NiTi hydrotalcite photocatalyst as well as a preparation method and application thereof.
Background
The sugars available in plant cellulose resources are mainly cellulose and hemicellulose, and among them, the glucose fermentation industry, which uses cellulose as a raw material, is relatively mature. However, the hemicellulose mainly containing xylose in plant fiber accounts for about 20% -35%, and its high efficiency transformation and utilization become one of the key technical bottlenecks of the whole biorefinery system. In recent years, xylonic acid has a wide industrial application potential as an emerging product for efficient bioconversion and utilization of plant fiber resource xylose, and is determined by the U.S. department of energy as one of 30 target products or chemical basic building block units with the greatest development prospect in refining plant fiber resource biomass.
Based on the research significance, it is very important to find a green and efficient catalyst to catalytically convert xylose into xylonic acid through a green reaction way. The preparation of sugar acids from aldoses is mainly carried out by biological oxidation, homogeneous catalytic oxidation, electrolytic oxidation and heterogeneous catalytic oxidation. The biological oxidation method has mild production conditions and is environment-friendly, but has strict requirements on experimental conditions, long period and difficult separation of byproducts, thereby influencing the purity of products. The intermediate steps in the homogeneous catalytic oxidation process are complex, the number of byproducts is large, the products are difficult to separate, the catalyst is difficult to recycle, and the wastes cause great harm to the environment. The electrolytic oxidation method solves the defects of more byproducts, complicated steps and the like of a biological fermentation method and a homogeneous chemical oxidation method, but has large energy consumption and difficult control of conditions in industrial production. Recently emerging photocatalysts have made better use of solar, green conversion substrates.
Hydrotalcite, as a heterogeneous basic catalyst, is replacing conventional basic catalysts such as NaOH and KOH in many reactions. Because isopoly and heteropolyanion pillared hydrotalcite has unique properties, such as adjustable pore channel structure, stronger shape-selective catalysis and acid-base properties, people pay more attention to the performance. The existing synthetic methods include low saturation coprecipitation method, hydrothermal synthesis method, ion exchange method, microwave crystallization method, etc. (Journal of the Chemical Society Reviews 43.20(2014): 7040-.
Disclosure of Invention
In order to solve the problems, the invention provides a NiTi hydrotalcite photocatalyst and a preparation method and application thereof. The method specifically comprises a novel method for synthesizing a nickel-titanium hydrotalcite photocatalyst by hydrolyzing nickel salt and titanium salt in an alkaline medium urotropine (hexamethylenetetramine) aqueous solution by a hydrothermal method and a method for catalyzing xylose to convert xylonic acid by using the hydrotalcite catalyst.
The purpose of the invention is realized by at least one of the following technical solutions.
The invention provides a preparation method of a nickel-titanium nano-flower hydrotalcite photocatalyst, which comprises the following steps:
(1) adding titanium salt, nickel salt and urotropine into water, and stirring uniformly to dissolve all substances to obtain a mixed solution (transparent);
(2) heating the mixed solution obtained in the step (1) for heating reaction, cooling to room temperature to obtain a heated product, and filtering to obtain a precipitate;
(3) and (3) drying the precipitate obtained in the step (2) to obtain the nickel-titanium nano-flower hydrotalcite photocatalyst.
Further, the titanium salt in the step (1) is more than one of titanic acid, titanium tetrachloride, titanium trichloride and titanium sulfate; the nickel salt is more than one of nickel sulfate, nickel chloride, nickel sulfamate, nickel bromide, nickel hydroxide, nickel carbonyl and nickel nitrate pentahydrate; the molar ratio of the nickel salt to the titanium salt is 1-5: 1.
further, the ratio of the total mole number of the titanium salt and the nickel salt to the mole number of the urotropine in the step (1) is 2-10: 1.
further, the ratio of the mole number of the water in the step (1) to the total mole number of the titanium salt and the nickel salt is 200-: 1.
further, the temperature of the heating reaction in the step (2) is 100-.
Further, the drying temperature in the step (3) is 60-100 ℃.
The invention provides a nickel-titanium nano-flower hydrotalcite photocatalyst prepared by the preparation method, which has a three-dimensional nano-flower structure, is formed by crossing nano-sheets and has the diameter of 6-7 mu m.
The nickel-titanium nano-flower hydrotalcite photocatalyst provided by the invention can be mixed with xylose, water and alkali liquor, and then is subjected to catalytic reaction under the irradiation of visible light to obtain xylonic acid.
The nickel-titanium nano-flower hydrotalcite photocatalyst provided by the invention can be applied to the reaction of catalyzing and converting xylose to generate xylonic acid.
The application of the nickel-titanium nano-flower hydrotalcite photocatalyst in catalytic conversion of xylose to generate xylonic acid comprises the following steps:
A. adding xylose and the nickel-titanium nano-flower hydrotalcite photocatalyst into water, uniformly mixing, adding an alkaline solution, and uniformly mixing to obtain a mixed solution;
B. and C, heating the mixed solution obtained in the step A under the irradiation of visible light, and cooling to room temperature to obtain the xylonic acid.
Further, the application of the nickel-titanium nano-flower hydrotalcite photocatalyst in catalytic conversion of xylose to generate xylonic acid is that in the mixed solution in the step A, the concentration of the xylose is 10-100mg/m L, the concentration of the nickel-titanium nano-flower hydrotalcite photocatalyst is 1-10mg/m L, the alkaline solution in the step A is one of KOH solution, NaOH solution, sodium carbonate solution, sodium bicarbonate solution and ammonia water, the concentration of the alkaline solution is 0.1-1.0mol/m L, the volume ratio of the water to the alkaline solution in the step A is 1-9:1, the heating treatment temperature in the step B is 20-80 ℃, and the heating treatment time is 30-300 min.
In the preparation method provided by the invention, the adopted nickel and titanium have good photoresponse, the urotropine (urea and thiourea) provides a weak alkaline environment in the hydrothermal process to form the nickel-titanium nano-flower hydrotalcite catalyst, the special structure of the catalyst can be utilized to carry out photocatalytic reaction, and the selectivity of the reaction can be further improved in the future industrial production process.
The method for preparing the catalyst is simple, high-temperature heating is not needed, and the synthesized catalyst can be directly used for catalytic reaction without subsequent treatment. The catalyst provided by the invention has the potential of industrialization, the cost of the catalytic process is low, the catalyst is different from the traditional thermal catalysis, the process is green and environment-friendly, and no harmful by-product is generated.
Compared with the prior art, the invention has the following advantages and beneficial effects:
(1) the nickel-titanium nanoflower hydrotalcite photocatalyst synthesized by the method has a special nanoflower structure, can effectively utilize light energy on the surface of the nanoflower, improves apparent quantum efficiency, and is a good photocatalyst;
(2) the application of the nickel-titanium nano-flower hydrotalcite photocatalyst in catalyzing xylose to generate xylonic acid is a photocatalytic reaction way, the reaction process is green and environment-friendly, the requirement on reaction conditions is not high, a xenon lamp can be used as a light source (simulating solar illumination), and the photocatalyst has a commercialized application prospect and is green and environment-friendly;
(3) the preparation method provided by the invention is simple, high-temperature heating is not required, and the synthesized catalyst can be directly used for catalytic reaction without subsequent treatment.
Drawings
FIG. 1 is an SEM image of a NiTi hydrotalcite photocatalyst prepared in example 2;
FIG. 2 is a TEM image of the NiTitania hydrotalcite photocatalyst prepared in example 2;
FIG. 3 is a graph of the yield of xylose converted to xylonic acid in example 12 at various catalyst loadings;
FIG. 4 is a graph of the yield of xylose-converted xylonic acid catalyzed by example 13 at different reaction times;
FIG. 5 is a graph of the yield of xylose-converted xylonic acid catalyzed by example 14 under different reaction temperature conditions;
FIG. 6 is a graph of the yield of xylose-converted xylonic acid catalyzed by example 15 under different base concentrations.
Detailed Description
The following examples are presented to further illustrate the practice of the invention, but the practice and protection of the invention is not limited thereto. It is noted that the processes described below, if not specifically described in detail, are all realizable or understandable by those skilled in the art with reference to the prior art. The reagents or apparatus used are not indicated to the manufacturer, and are considered to be conventional products available by commercial purchase.
Example 1
A preparation method of a nickel-titanium nanometer hydrotalcite photocatalyst comprises the following steps:
(1) dissolving 0.29g of nickel nitrate hexahydrate, 0.237g of titanium sulfate and 2.8g of urotropine into 50m L deionized water, and uniformly stirring to obtain a transparent solution;
(2) transferring the transparent solution obtained in the step (1) into a polytetrafluoroethylene lining, heating the polytetrafluoroethylene lining in a muffle furnace for heating reaction at the temperature of 140 ℃ for 9 hours, cooling the polytetrafluoroethylene lining to room temperature to obtain a heated product, and performing suction filtration to obtain a precipitate;
(3) and (3) drying the precipitate obtained in the step (2) at the temperature of 30 ℃ to obtain the nickel-titanium nano-flower hydrotalcite photocatalyst.
Example 2
A preparation method of a nickel-titanium nanometer hydrotalcite photocatalyst comprises the following steps:
(1) 0.8721g of nickel nitrate hexahydrate, 0.237g of titanium sulfate and 2.8g of urotropine are dissolved in 50m L of deionized water and are uniformly stirred to obtain a transparent solution;
(2) transferring the transparent solution obtained in the step (1) into a polytetrafluoroethylene lining, heating the polytetrafluoroethylene lining in a muffle furnace for heating reaction at the temperature of 140 ℃ for 9 hours, cooling the polytetrafluoroethylene lining to room temperature to obtain a heated product, and performing suction filtration to obtain a precipitate;
(3) and (3) drying the precipitate obtained in the step (2) at the temperature of 60 ℃ to obtain the nickel-titanium nano-flower hydrotalcite photocatalyst.
The effect of the nickel titanium nano-flower hydrotalcite photocatalyst prepared in example 2 observed under a scanning electron microscope is shown in fig. 1, and it can be known from fig. 1 that the nickel titanium nano-flower hydrotalcite photocatalyst prepared in example 2 has a nano-flower structure; the effect of the nickel titanium nano-flower hydrotalcite photocatalyst prepared in example 2 observed under a transmission electron microscope is shown in fig. 2, and it can be seen from fig. 2 that the nano-flower structure of the nickel titanium nano-flower hydrotalcite photocatalyst prepared in example 2 is composed of nano-sheets under a high power transmission microscope. The effect of the nickel titanium nano-flower hydrotalcite photocatalyst prepared in other examples observed under an electron microscope is similar to that of example 2, and the photocatalyst also has a nano-flower structure, and reference can be made to fig. 1 and 2.
Example 3
A preparation method of a nickel-titanium nanometer hydrotalcite photocatalyst comprises the following steps:
(1) 1.45g of nickel nitrate hexahydrate, 0.237g of titanium sulfate and 2.8g of urotropine are dissolved in 50m L deionized water and are uniformly stirred to obtain a transparent solution;
(2) transferring the transparent solution obtained in the step (1) into a polytetrafluoroethylene lining, heating the polytetrafluoroethylene lining in a muffle furnace for heating reaction at the temperature of 140 ℃ for 9 hours, cooling the polytetrafluoroethylene lining to room temperature to obtain a heated product, and performing suction filtration to obtain a precipitate;
(3) and (3) drying the precipitate obtained in the step (2) at the temperature of 100 ℃ to obtain the nickel-titanium nano-flower hydrotalcite photocatalyst.
Example 4
A preparation method of a nickel-titanium nanometer hydrotalcite photocatalyst comprises the following steps:
(1) 0.8721g of nickel nitrate hexahydrate, 0.237g of titanium sulfate and 1.1214g of urotropine are dissolved in 50m L of deionized water and are uniformly stirred to obtain a transparent solution;
(2) transferring the transparent solution obtained in the step (1) into a polytetrafluoroethylene lining, heating the polytetrafluoroethylene lining in a muffle furnace for heating reaction at the temperature of 140 ℃ for 9 hours, cooling the polytetrafluoroethylene lining to room temperature to obtain a heated product, and performing suction filtration to obtain a precipitate;
(3) and (3) drying the precipitate obtained in the step (2) at the temperature of 60 ℃ to obtain the nickel-titanium nano-flower hydrotalcite photocatalyst.
Example 5
A preparation method of a nickel-titanium nanometer hydrotalcite photocatalyst comprises the following steps:
(1) 0.8721g of nickel nitrate hexahydrate, 0.237g of titanium sulfate and 5.6g of urotropine are dissolved in 50m L of deionized water and are uniformly stirred to obtain a transparent solution;
(2) transferring the transparent solution obtained in the step (1) into a polytetrafluoroethylene lining, heating the polytetrafluoroethylene lining in a muffle furnace for heating reaction at the temperature of 140 ℃ for 9 hours, cooling the polytetrafluoroethylene lining to room temperature to obtain a heated product, and performing suction filtration to obtain a precipitate;
(3) and (3) drying the precipitate obtained in the step (2) at the temperature of 60 ℃ to obtain the nickel-titanium nano-flower hydrotalcite photocatalyst.
Example 6
A preparation method of a nickel-titanium nanometer hydrotalcite photocatalyst comprises the following steps:
(1) 0.8721g of nickel nitrate hexahydrate, 0.237g of titanium sulfate and 5.6g of urotropine are dissolved in 25m L of deionized water and are uniformly stirred to obtain a transparent solution;
(2) transferring the transparent solution obtained in the step (1) into a polytetrafluoroethylene lining, heating the polytetrafluoroethylene lining in a muffle furnace for heating reaction at the temperature of 140 ℃ for 9 hours, cooling the polytetrafluoroethylene lining to room temperature to obtain a heated product, and performing suction filtration to obtain a precipitate;
(3) and (3) drying the precipitate obtained in the step (2) at the temperature of 60 ℃ to obtain the nickel-titanium nano-flower hydrotalcite photocatalyst.
Example 7
A preparation method of a nickel-titanium nanometer hydrotalcite photocatalyst comprises the following steps:
(1) 0.8721g of nickel nitrate hexahydrate, 0.237g of titanium sulfate and 5.6g of urotropine are dissolved in 72m of L deionized water and are uniformly stirred to obtain a transparent solution;
(2) transferring the transparent solution obtained in the step (1) into a polytetrafluoroethylene lining, heating the polytetrafluoroethylene lining in a muffle furnace for heating reaction at the temperature of 140 ℃ for 9 hours, cooling the polytetrafluoroethylene lining to room temperature to obtain a heated product, and performing suction filtration to obtain a precipitate;
(3) and (3) drying the precipitate obtained in the step (2) at the temperature of 60 ℃ to obtain the nickel-titanium nano-flower hydrotalcite photocatalyst.
Example 8
A preparation method of a nickel-titanium nanometer hydrotalcite photocatalyst comprises the following steps:
(1) 0.8721g of nickel nitrate hexahydrate, 0.237g of titanium sulfate and 2.8g of urotropine are dissolved in 50m L of deionized water and are uniformly stirred to obtain a transparent solution;
(2) transferring the transparent solution obtained in the step (1) into a polytetrafluoroethylene lining, heating the polytetrafluoroethylene lining in a muffle furnace for heating reaction at the temperature of 100 ℃ for 9 hours, cooling the polytetrafluoroethylene lining to room temperature to obtain a heated product, and performing suction filtration to obtain a precipitate;
(3) and (3) drying the precipitate obtained in the step (2) at 70 ℃ to obtain the nickel-titanium nano-flower hydrotalcite photocatalyst.
Example 9
A preparation method of a nickel-titanium nanometer hydrotalcite photocatalyst comprises the following steps:
(1) 0.8721g of nickel nitrate hexahydrate, 0.237g of titanium sulfate and 2.8g of urotropine are dissolved in 50m L of deionized water and are uniformly stirred to obtain a transparent solution;
(2) transferring the transparent solution obtained in the step (1) into a polytetrafluoroethylene lining, heating the polytetrafluoroethylene lining in a muffle furnace for heating reaction at the temperature of 300 ℃ for 9 hours, cooling the polytetrafluoroethylene lining to room temperature to obtain a heated product, and performing suction filtration to obtain a precipitate;
(3) and (3) drying the precipitate obtained in the step (2) at the temperature of 100 ℃ to obtain the nickel-titanium nano-flower hydrotalcite photocatalyst.
Example 10
A preparation method of a nickel-titanium nanometer hydrotalcite photocatalyst comprises the following steps:
(1) 0.8721g of nickel nitrate hexahydrate, 0.237g of titanium sulfate and 2.8g of urotropine are dissolved in 50m L of deionized water and are uniformly stirred to obtain a transparent solution;
(2) transferring the transparent solution obtained in the step (1) into a polytetrafluoroethylene lining, heating the polytetrafluoroethylene lining in a muffle furnace for heating reaction at the temperature of 300 ℃ for 6 hours, cooling the polytetrafluoroethylene lining to room temperature to obtain a heated product, and performing suction filtration to obtain a precipitate;
(3) and (3) drying the precipitate obtained in the step (2) at the temperature of 60 ℃ to obtain the nickel-titanium nano-flower hydrotalcite photocatalyst.
Example 11
A preparation method of a nickel-titanium nanometer hydrotalcite photocatalyst comprises the following steps:
(1) 0.8721g of nickel nitrate hexahydrate, 0.237g of titanium sulfate and 2.8g of urotropine are dissolved in 50m L of deionized water and are uniformly stirred to obtain a transparent solution;
(2) transferring the transparent solution obtained in the step (1) into a polytetrafluoroethylene lining, heating the polytetrafluoroethylene lining in a muffle furnace for heating reaction at the temperature of 300 ℃ for 20 hours, cooling the polytetrafluoroethylene lining to room temperature to obtain a heated product, and performing suction filtration to obtain a precipitate;
(3) and (3) drying the precipitate obtained in the step (2) at the temperature of 60 ℃ to obtain the nickel-titanium nano-flower hydrotalcite photocatalyst.
Example 12
(1) Weighing 5 parts of xylose with the mass of 0.1g, respectively adding the xylose into 5 glass reactors, respectively adding 1 part of 9 m L ultra-pure water with the volume of 1m L and KOH solution with the concentration of 0.5 mol/L into the 5 glass reactors, respectively adding only 1 part of xylose, ultra-pure water and KOH solution into each glass reactor, and uniformly mixing to obtain 5 parts of the same mixed solution;
(2) respectively weighing 10mg, 20 mg, 30mg, 40 mg and 50 mg of nickel-titanium nano-flower hydrotalcite photocatalyst (the catalyst is prepared in example 2) and adding the catalyst into 5 parts of mixed liquor obtained in the step (1), wherein the catalyst is added into each part of mixed liquor only once and is uniformly stirred to obtain 5 parts of reaction system;
(3) placing the 5 parts of reaction system in a water bath condition at 40 ℃, and reacting for 1h under the irradiation of a xenon lamp to obtain 5 parts of reaction liquid;
(4) and (4) diluting the 5 parts of reaction solution obtained in the step (3) by one time respectively, and measuring the content of the xylonic acid by using a high performance liquid chromatograph.
The yield of xylonic acid was determined to be 14.53%, 16.93%, 20.98%, 18.78% and 18.18% with the catalyst amounts of 10mg, 20 mg, 30mg, 40 mg and 50 mg, respectively. The above results are shown in FIG. 3. It can be seen from this that, in fig. 3, as the amount of the catalyst used increases, the yield gradually increases, reaching a maximum at a catalyst amount of 30mg (the nickel titanium nano-flower hydrotalcite photocatalyst prepared in example 2), and then as the amount of the catalyst increases, the yield of the xylonic acid tends to decrease.
Example 13
(1) Weighing 6 parts of xylose with the mass of 0.1g and 6 parts of nickel-titanium nano-hydrotalcite photocatalyst (prepared in example 2) with the mass of 30mg, respectively adding the xylose and the catalyst into 6 glass reactors, adding 1 part of xylose into each glass reactor, adding 1 part of ultrapure water with the volume of 9 m L and 1 part of KOH solution with the volume of 1m L and the concentration of 0.5 mol/L into the 6 glass reactors, respectively, only adding 1 part of ultrapure water and 1 part of KOH solution into each glass reactor, and uniformly mixing to obtain 6 parts of a reaction system;
(2) placing the 6 parts of reaction system in a water bath condition at 40 ℃, reacting for 30min, 60min, 90min, 120min, 150min and 180min respectively, and obtaining 6 parts of reaction liquid under the irradiation of a xenon lamp;
(3) diluting the 6 parts of reaction solution in the step (2) by one time, and then measuring the content of the xylonic acid by using a high performance liquid chromatograph.
The yield of the xylonic acid is determined to be 21.26%, 24.2%, 25.73%, 24.4%, 22.96% and 22.43% under the conditions of reaction for 30min, 60min, 90min, 120min, 150min and 180 min. The above results are shown in FIG. 4. It can be seen from this that, in fig. 4, the yield gradually increased with the increase of the reaction time, reached the maximum value at the time of reaction for 90min, and then the yield of xylonic acid tended to decrease with the increase of the amount of the catalyst used.
Example 14
(1) Respectively weighing 5 parts by mass of 0.1g xylose and 30mg nickel-titanium nano-flower hydrotalcite photocatalyst (prepared in example 2) and adding the weighed materials into 5 glass reactors, respectively adding 1 part by volume of 9 m L ultrapure water and 1 part by volume of 1m L KOH solution with the concentration of 0.5 mol/L into the 5 glass reactors, uniformly mixing, and only adding 1 part by volume of xylose, the catalyst, the ultrapure water and the KOH solution into each glass reactor to obtain 5 parts of a reaction system;
(2) placing the 5 parts of reaction system in water bath conditions of 20 ℃, 30 ℃, 40 ℃, 50 ℃ and 60 ℃ respectively, reacting for 90min, and obtaining 5 parts of reaction liquid under the irradiation of a xenon lamp;
(3) diluting the 5 parts of reaction solution in the step (2) by one time, and then measuring the content of the xylonic acid by using a high performance liquid chromatograph.
The test shows that the yield of the xylonic acid is 26.15%, 27.98%, 28.4%, 26.78% and 20.81% under the water bath conditions of the reaction temperature of 20 ℃, 30 ℃, 40 ℃, 50 ℃ and 60 ℃. The above results are shown in FIG. 5. It can be seen from this that, in fig. 5, the yield gradually increased with the increase of the reaction temperature, reached the maximum value at the reaction temperature of 40 ℃, and then the yield of xylonic acid decreased with the increase of the amount of the catalyst.
Example 15
(1) Respectively weighing 7 parts by mass of 0.1g of xylose and 7 parts by mass of 30mg of nickel-titanium nano-flower hydrotalcite photocatalyst (prepared in example 2), adding the weighed materials into 7 parts of glass reactors, respectively adding 1 part by volume of 9 m L ultrapure water into the 7 glass reactors, only adding 1 part by volume of xylose, the catalyst and the ultrapure water into one glass reactor, and uniformly mixing to obtain 7 parts of mixed solution;
(2) adding KOH solutions with the concentration of 10 mmol/L, 20 mmol/L, 30 mmol/L, 40 mmol/L, 50 mmol/L, 60 mmol/L and 70 mmol/L of 1m L into the 7 parts of mixed solution in the step (1) respectively, uniformly mixing to obtain 7 parts of reaction system, placing the 7 parts of reaction system in a water bath condition at 40 ℃, and reacting for 90min under the irradiation of a xenon lamp to obtain 7 parts of reaction liquid;
(3) and (3) diluting the 7 parts of reaction solution in the step (2) by one time respectively, and then measuring the content of the xylonic acid by using a high performance liquid chromatograph.
It was determined that the yields of xylonic acid were 22.93%, 33.41%, 35.71%, 42.21%, 51.1%, 53.68% and 50.37% at alkaline solution (KOH solution) concentrations of 10 mmol/L, 20 mmol/L, 30 mmol/L, 40 mmol/L, 50 mmol/L, 60 mmol/L and 70 mmol/L, respectively, as shown in fig. 6, it can be seen that in fig. 6, the yield gradually increased with increasing alkaline concentration, reaching a maximum at an alkaline concentration of 60 mol/L, and thereafter, the yield of xylonic acid decreased with increasing catalyst usage.
The results of the above examples show that the nickel titanium nano-flower hydrotalcite photocatalyst synthesized in example 2 has a special nano-flower structure, can effectively utilize light energy on the surface of the nano-flower, improves apparent quantum efficiency, and is a good photocatalyst; the application of the nickel-titanium nanoflower hydrotalcite photocatalyst provided by the embodiment 2 in catalyzing xylose to generate xylonic acid is a photocatalytic reaction approach, the reaction process is green and environment-friendly, the requirement on reaction conditions is not high, a xenon lamp can be used as a light source (simulating solar illumination), and the photocatalyst has a commercialized application prospect and is green and environment-friendly;
other embodiments can effectively utilize light energy and improve apparent quantum efficiency, are good photocatalysts, can catalyze xylose to generate xylonic acid under the condition of illumination, have low requirements on reaction conditions, and can catalyze the application effect of xylose to generate xylonic acid in other embodiments, and refer to fig. 3, fig. 4, fig. 5 and fig. 6.
The above examples are only preferred embodiments of the present invention, which are intended to be illustrative and not limiting, and those skilled in the art should understand that they can make various changes, substitutions and alterations without departing from the spirit and scope of the invention.
Claims (10)
1. A preparation method of a nickel titanium nanometer hydrotalcite photocatalyst is characterized by comprising the following steps:
(1) adding titanium salt, nickel salt and urotropine into water, and uniformly stirring to obtain a mixed solution;
(2) heating the mixed solution obtained in the step (1) for heating reaction, cooling to room temperature to obtain a heated product, and filtering to obtain a precipitate;
(3) and (3) drying the precipitate obtained in the step (2) to obtain the nickel-titanium nano-flower hydrotalcite photocatalyst.
2. The method for preparing the nickel titanium nanoflower hydrotalcite photocatalyst according to claim 1, wherein the titanium salt in step (1) is one or more of titanic acid, titanium tetrachloride, titanium trichloride and titanium sulfate; the nickel salt is more than one of nickel sulfate, nickel chloride, nickel sulfamate, nickel bromide, nickel hydroxide, nickel carbonyl and nickel nitrate pentahydrate; the molar ratio of the nickel salt to the titanium salt is 1-5: 1.
3. the method for preparing the NiTi nanofloral hydrotalcite photocatalyst as claimed in claim 1, wherein the ratio of the total moles of the titanium salt and the nickel salt to the moles of the urotropin in step (1) is 2 to 10: 1.
4. the method for preparing NiTi nanoflower hydrotalcite photocatalyst as claimed in claim 1, wherein the ratio of the mole number of water in step (1) to the total mole number of the titanium salt and the nickel salt is 200-1000: 1.
5. the method for preparing the NiTi nanoflower hydrotalcite photocatalyst as claimed in claim 1, wherein the temperature of the heating reaction in step (2) is 100-300 ℃, and the time of the heating reaction is 6-20 h.
6. The method of claim 1, wherein the drying temperature in step (3) is 60-100 ℃.
7. The NiTi nanoflower hydrotalcite photocatalyst prepared by the preparation method of any one of claims 1 to 6, has a three-dimensional nanoflower structure, is formed by crossing nanosheets, and has a diameter of 6-7 μm.
8. Use of the nickel titanium nanoflower hydrotalcite photocatalyst of claim 7 for the catalytic conversion of xylose to xylonic acid.
9. The use of the nickel titanium nanoflower hydrotalcite photocatalyst of claim 8 in the catalytic conversion of xylose to xylonic acid comprising the steps of:
A. adding xylose and the nickel-titanium nano-flower hydrotalcite photocatalyst into water, uniformly mixing, adding an alkaline solution, and uniformly mixing to obtain a mixed solution;
B. and C, heating the mixed solution obtained in the step A under the irradiation of visible light, and cooling to room temperature to obtain the xylonic acid.
10. The application of the NiTi nanoflower hydrotalcite photocatalyst in catalytic conversion of xylose to xylonic acid according to claim 9 is characterized in that in the mixed solution in the step A, the concentration of xylose is 10-100mg/m L, the concentration of the NiTi nanoflower hydrotalcite photocatalyst is 1-10mg/m L, the alkaline solution in the step A is one of KOH solution, NaOH solution, sodium carbonate solution, sodium bicarbonate solution and ammonia water, the concentration of the alkaline solution is 0.1-1.0mol/m L, the volume ratio of water to the alkaline solution in the step A is 1-9:1, the heating treatment temperature in the step B is 20-80 ℃, and the heating treatment time is 30-300 min.
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| CN113856741A (en) * | 2021-11-19 | 2021-12-31 | 陕西科技大学 | Hydrotalcite solid base, preparation method thereof and application of hydrotalcite solid base in efficient catalysis of cyclopentanone trimerization |
| CN114956141A (en) * | 2022-03-30 | 2022-08-30 | 润和科华催化剂(上海)有限公司 | Flower-like hydrotalcite microspheres and preparation method and application thereof |
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Cited By (4)
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| CN113856741A (en) * | 2021-11-19 | 2021-12-31 | 陕西科技大学 | Hydrotalcite solid base, preparation method thereof and application of hydrotalcite solid base in efficient catalysis of cyclopentanone trimerization |
| CN113856741B (en) * | 2021-11-19 | 2023-06-20 | 陕西科技大学 | Hydrotalcite solid base, preparation method thereof and application of hydrotalcite solid base in efficient catalysis of cyclopentanone trimerization |
| CN114956141A (en) * | 2022-03-30 | 2022-08-30 | 润和科华催化剂(上海)有限公司 | Flower-like hydrotalcite microspheres and preparation method and application thereof |
| CN114956141B (en) * | 2022-03-30 | 2023-05-16 | 润和科华催化剂(上海)有限公司 | Flower-shaped hydrotalcite microsphere and preparation method and application thereof |
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