CN108311140A - A kind of preparation method of the optic catalytic composite material of palladium modification - Google Patents
A kind of preparation method of the optic catalytic composite material of palladium modification Download PDFInfo
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- CN108311140A CN108311140A CN201810234281.5A CN201810234281A CN108311140A CN 108311140 A CN108311140 A CN 108311140A CN 201810234281 A CN201810234281 A CN 201810234281A CN 108311140 A CN108311140 A CN 108311140A
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- Prior art keywords
- palladium
- composite material
- pdcl
- preparation
- rgo
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- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 title claims abstract description 52
- 229910052763 palladium Inorganic materials 0.000 title claims abstract description 18
- 239000002131 composite material Substances 0.000 title claims abstract description 17
- 230000004048 modification Effects 0.000 title claims abstract description 15
- 238000012986 modification Methods 0.000 title claims abstract description 15
- 230000003197 catalytic effect Effects 0.000 title claims abstract description 14
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims abstract description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000000843 powder Substances 0.000 claims abstract description 9
- 229910002666 PdCl2 Inorganic materials 0.000 claims abstract description 8
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 6
- 239000007864 aqueous solution Substances 0.000 claims abstract description 5
- 229960005070 ascorbic acid Drugs 0.000 claims abstract description 5
- 235000010323 ascorbic acid Nutrition 0.000 claims abstract description 5
- 239000011668 ascorbic acid Substances 0.000 claims abstract description 5
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000002904 solvent Substances 0.000 claims abstract description 4
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 3
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 3
- 239000010439 graphite Substances 0.000 claims abstract description 3
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 3
- -1 palladium modified titanic oxide Chemical class 0.000 claims abstract description 3
- PIBWKRNGBLPSSY-UHFFFAOYSA-L palladium(II) chloride Chemical compound Cl[Pd]Cl PIBWKRNGBLPSSY-UHFFFAOYSA-L 0.000 claims abstract description 3
- 238000007789 sealing Methods 0.000 claims abstract 2
- 239000000243 solution Substances 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 5
- 238000001291 vacuum drying Methods 0.000 claims description 5
- 101150003085 Pdcl gene Proteins 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims description 2
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 2
- 239000010936 titanium Substances 0.000 claims 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims 1
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 claims 1
- 239000003795 chemical substances by application Substances 0.000 claims 1
- 239000008367 deionised water Substances 0.000 claims 1
- 229910021641 deionized water Inorganic materials 0.000 claims 1
- 229910052719 titanium Inorganic materials 0.000 claims 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims 1
- 238000013019 agitation Methods 0.000 abstract description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000003643 water by type Substances 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000005416 organic matter Substances 0.000 description 2
- 238000007146 photocatalysis Methods 0.000 description 2
- 230000001699 photocatalysis Effects 0.000 description 2
- 229910052723 transition metal Inorganic materials 0.000 description 2
- 150000003624 transition metals Chemical class 0.000 description 2
- 239000012855 volatile organic compound Substances 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 229910020692 Pd-TiO2 Inorganic materials 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000002604 ultrasonography Methods 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
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/40—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals of the platinum group metals
- B01J23/44—Palladium
-
- B01J35/39—
Abstract
The present invention devises a kind of preparation method of the optic catalytic composite material of palladium modification.With palladium chloride (PdCl2) source as palladium (Pd), by PdCl2It is mixed with graphite oxide (GO) aqueous solution, ascorbic acid is as reducing agent, pyroreaction after sealing, obtains palladium modification reduced graphene powder (RGO/Pd)；Using butyl titanate as presoma, using neopelex (DBS) as solvent, RGO/Pd powder, neopelex (DBS), butyl titanate are mixed, magnetic agitation, a kind of simple, green hydrothermal method is finally used, palladium modified titanic oxide/graphene composite material (Pd TiO are obtained2/GO)。
Description
Technical field
The present invention relates to a kind of preparation methods of the optic catalytic composite material of palladium modification, belong to photocatalysis technology field.
Background technology
VOCs (volatile organic compounds) volatile organic matter, is often referred to readily volatilized at normal temperatures
Organic matter is one of the main source of environment in recent years pollution, and administering organic pollution problem using photochemical catalyst becomes research
One of hot spot.Common transition metal modification catalysis material has certain catalytic effect, but there are easy oxygen for transition metal
The shortcomings that change, particle are easily reunited, limit its application.And precious metal palladium (Pd) catalytic performance is excellent, chemical property is stablized, and is repaiied with Pd
Catalysis material is adornd, the performance of catalyst can be improved, thus there is very high application value.
In order to overcome the difficulty of above-mentioned technical aspect, present invention uses a kind of simple, green hydrothermal methods, are prepared for
A kind of optic catalytic composite material of Pd modification, improve the specific surface area of composite photo-catalyst, reduce electron-hole pair in conjunction with
Rate, and then improve photocatalysis efficiency.
Invention content
The present invention is a kind of preparation method of the optic catalytic composite material of palladium modification, intends to solve and exists in above-mentioned background technology
The problem of.
1. as a preferred embodiment, with palladium chloride (PdCl2) source as Pd, take the PdCl of 0.5~2g2Dissolving
Afterwards, it is mixed into graphite oxide (GO) aqueous solution of a concentration of 0.3~1.0g/L of 50~100mL, 5~10g ascorbic acid conducts
Reducing agent is dissolved into above-mentioned solution, forms PdCl2With the mixed liquor of GO.
2. as a preferred embodiment, by PdCl2It is sealed in beaker with the mixed liquor of GO, under the conditions of 100~200 DEG C
5~10h is reacted, centrifuges and washs, dry 10~20h in vacuum drying chamber obtains palladium modification reduced graphene powder (RGO/
Pd)。
3. as a preferred embodiment, using neopelex (DBS) as solvent, using butyl titanate before
Body is driven, according to molal weight n (DBS):The ratio of n (Ti)=0.3~1, is put into the beaker for filling 100~200mL deionized waters
In, 1~2h of magnetic agitation, then RGO/Pd powder is added in beaker, continue 1~2h of magnetic agitation, solution in beaker is moved to
In reaction kettle, 10~20h is kept the temperature at a temperature of 150~200 DEG C.After reaction, it by solution centrifuge washing, vacuum drying, obtains
Palladium modified titanic oxide/graphene composite material (Pd-TiO2/RGO)。
Description of the drawings
Fig. 1：The structural schematic diagram of the optic catalytic composite material of Pd modifications
Specific implementation mode
By 1g PdCl2Ultrasound in 30mL deionized waters is added to be transferred in beaker, pipette later to being completely dissolved
The GO aqueous solutions of a concentration of 0.5g/L of 50mL are slowly dropped in beaker；It is another weigh 5g ascorbic acid ultrasonic dissolution in 30mL go from
In sub- water, it is used in combination the NaOH of a concentration of 5mol/L to adjust solution ph and is slowly dropped in beaker to 8, then by the solution, sealed
Beaker reacts 5h under the conditions of 100 DEG C, after cooling, centrifuge and washs, and dry 10h, obtains RGO/Pd powder in vacuum drying chamber
End.
Using DBS as solvent, using butyl titanate as presoma, according to molal weight n (DBS):N's (Ti)=0.3
Ratio is put into the beaker for filling 100mL deionized waters, magnetic agitation 1h, then RGO/Pd powder is added in beaker, continues magnetic
Power stirs 1h, and solution in beaker is moved in reaction kettle, 10h is kept the temperature at a temperature of 180 DEG C.After reaction, by solution centrifugation point
From washing, dry 10h, obtains Pd-TiO in vacuum drying chamber2/RGO。
Claims (5)
1. a kind of preparation method of the optic catalytic composite material of palladium modification, feature are：With palladium chloride (PdCl2) it is used as palladium
(Pd) source is mixed with graphite oxide (GO) aqueous solution, and as reducing agent, pyroreaction after sealing obtains ascorbic acid
Pd modifies reduced graphene powder (RGO/Pd)；Using butyl titanate as presoma, made with neopelex (DBS)
Palladium modified titanic oxide/graphene composite material (Pd-TiO is obtained using one step hydro thermal method for solvent2/RGO)。
2. a kind of preparation method of the optic catalytic composite material of palladium modification according to claim 1, feature are：With
PdCl2As the source of Pd, PdCl2Dosage be 0.5~2g.
3. the preparation method of the optic catalytic composite material of a kind of palladium modification according to claim 1, by the PdCl of 0.5~2g2
It is mixed into GO aqueous solutions, the dosage of GO is 50~100mL, a concentration of 0.3~1.0g/L；5~10g ascorbic acid is as reduction
Agent is dissolved into above-mentioned solution, obtains PdCl2With the mixed liquor of GO.
4. a kind of preparation method of the optic catalytic composite material of palladium modification according to claim 1, feature are：It will
PdCl25~10h is reacted under the conditions of 100~200 DEG C with the mixed liquor of GO, is centrifuged and is washed, it is dry in vacuum drying chamber,
Obtain RGO/Pd powder.
5. a kind of preparation method of the optic catalytic composite material of palladium modification according to claim 1, feature are：With titanium
Sour four butyl esters are as presoma, according to molal weight n (DBS):The ratio of n (Ti)=0.3~1, is dissolved into deionized water, magnetic
Power stirs 1~2h, and RGO/Pd powder is added, moves in reaction kettle, and 10~20h is kept the temperature at a temperature of 150~200 DEG C, obtains Pd-
TiO2/ RGO composite materials.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810234281.5A CN108311140A (en) | 2018-03-21 | 2018-03-21 | A kind of preparation method of the optic catalytic composite material of palladium modification |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810234281.5A CN108311140A (en) | 2018-03-21 | 2018-03-21 | A kind of preparation method of the optic catalytic composite material of palladium modification |
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| Publication Number | Publication Date |
|---|---|
| CN108311140A true CN108311140A (en) | 2018-07-24 |
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Cited By (3)
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| CN109806765A (en) * | 2019-03-26 | 2019-05-28 | 中国建筑材料科学研究总院有限公司 | Composite material for air cleaning and preparation method thereof |
| CN111799478A (en) * | 2020-07-17 | 2020-10-20 | 西南大学 | Graphene-supported palladium nanoparticle composite material and preparation method and application thereof |
| CN112774732A (en) * | 2021-01-29 | 2021-05-11 | 胡国强 | Ti-MOF/Rh-Al2O3Preparation method of composite catalyst |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109806765A (en) * | 2019-03-26 | 2019-05-28 | 中国建筑材料科学研究总院有限公司 | Composite material for air cleaning and preparation method thereof |
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| CN111799478A (en) * | 2020-07-17 | 2020-10-20 | 西南大学 | Graphene-supported palladium nanoparticle composite material and preparation method and application thereof |
| CN111799478B (en) * | 2020-07-17 | 2022-04-15 | 西南大学 | Graphene-supported palladium nanoparticle composite material and preparation method and application thereof |
| CN112774732A (en) * | 2021-01-29 | 2021-05-11 | 胡国强 | Ti-MOF/Rh-Al2O3Preparation method of composite catalyst |
| CN112774732B (en) * | 2021-01-29 | 2023-04-11 | 江西新节氢能源科技有限公司 | Ti-MOF/Rh-Al 2 O 3 Preparation method of composite catalyst |
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Application publication date: 20180724 |