CN110124665A - A kind of preparation method of shell multicore yolk shell catalyst Pd@HCS - Google Patents
A kind of preparation method of shell multicore yolk shell catalyst Pd@HCS Download PDFInfo
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- CN110124665A CN110124665A CN201910379790.1A CN201910379790A CN110124665A CN 110124665 A CN110124665 A CN 110124665A CN 201910379790 A CN201910379790 A CN 201910379790A CN 110124665 A CN110124665 A CN 110124665A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 54
- 239000003054 catalyst Substances 0.000 title claims abstract description 48
- 210000002969 egg yolk Anatomy 0.000 title claims abstract description 30
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 113
- 235000019441 ethanol Nutrition 0.000 claims abstract description 48
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 47
- 238000005406 washing Methods 0.000 claims abstract description 32
- 229910001868 water Inorganic materials 0.000 claims abstract description 24
- 239000008367 deionised water Substances 0.000 claims abstract description 23
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 23
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims abstract description 16
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229910052681 coesite Inorganic materials 0.000 claims abstract description 12
- 229910052906 cristobalite Inorganic materials 0.000 claims abstract description 12
- 229910052682 stishovite Inorganic materials 0.000 claims abstract description 12
- 229910052905 tridymite Inorganic materials 0.000 claims abstract description 12
- GHMLBKRAJCXXBS-UHFFFAOYSA-N resorcinol Chemical compound OC1=CC=CC(O)=C1 GHMLBKRAJCXXBS-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000006185 dispersion Substances 0.000 claims abstract description 7
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000012298 atmosphere Substances 0.000 claims abstract description 6
- 239000001257 hydrogen Substances 0.000 claims abstract description 6
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 6
- 230000003647 oxidation Effects 0.000 claims abstract description 6
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 6
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 5
- 238000005119 centrifugation Methods 0.000 claims abstract description 4
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims abstract description 3
- 239000000243 solution Substances 0.000 claims description 39
- 238000003756 stirring Methods 0.000 claims description 34
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims description 15
- 239000007788 liquid Substances 0.000 claims description 7
- 238000002604 ultrasonography Methods 0.000 claims description 7
- 238000003786 synthesis reaction Methods 0.000 claims description 6
- 239000011259 mixed solution Substances 0.000 claims description 5
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 5
- 238000000643 oven drying Methods 0.000 claims description 5
- 238000010992 reflux Methods 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 4
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 claims description 2
- 229910003603 H2PdCl4 Inorganic materials 0.000 claims description 2
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 2
- -1 reacts 20-40min Substances 0.000 claims description 2
- 239000012279 sodium borohydride Substances 0.000 claims description 2
- 229910000033 sodium borohydride Inorganic materials 0.000 claims description 2
- 230000003197 catalytic effect Effects 0.000 abstract description 8
- 239000002245 particle Substances 0.000 abstract description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 5
- 229910052799 carbon Inorganic materials 0.000 abstract description 5
- 238000001816 cooling Methods 0.000 abstract description 4
- 238000005530 etching Methods 0.000 abstract description 2
- 239000000377 silicon dioxide Substances 0.000 abstract description 2
- 238000001035 drying Methods 0.000 abstract 1
- XKZQKPRCPNGNFR-UHFFFAOYSA-N 2-(3-hydroxyphenyl)phenol Chemical compound OC1=CC=CC(C=2C(=CC=CC=2)O)=C1 XKZQKPRCPNGNFR-UHFFFAOYSA-N 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000011258 core-shell material Substances 0.000 description 2
- 239000012495 reaction gas Substances 0.000 description 2
- PYKYMHQGRFAEBM-UHFFFAOYSA-N anthraquinone Natural products CCC(=O)c1c(O)c2C(=O)C3C(C=CC=C3O)C(=O)c2cc1CC(=O)OC PYKYMHQGRFAEBM-UHFFFAOYSA-N 0.000 description 1
- 150000004056 anthraquinones Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000010189 synthetic method 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
-
- B01J35/396—
-
- B01J35/61—
Abstract
The invention discloses the preparation method of one shell multicore yolk shell catalyst Pd@HCS of one kind, include the following steps: that (1) prepares SiO2；(2) by the SiO of preparation2APTES is added in aqueous isopropanol in ultrasonic disperse, and product obtains SiO through ethyl alcohol centrifuge washing2‑NH2；(3) by SiO2‑NH2H is added in ethanol solution in ultrasonic disperse2PdCl4NaBH is added in solution4Solution, product obtain Pd/SiO through ethyl alcohol centrifuge washing2‑NH2；(4) by the Pd/SiO of preparation2‑NH2Dispersion in deionized water, is added ethanol solution, sequentially adds CTAB, resorcinol and NH3·H2Formalin is added in O, and cooling, product is dry after ethyl alcohol centrifuge washing, obtains Pd/SiO2‑NH2@RF；(5) Pd@SiO made from2‑NH2In deionized water, HF solution is added in@RF roasting dispersion, and room temperature etching restores under drying and roasting oxidation and hydrogen atmosphere after centrifugation and water washing, obtains one shell yolk shell structure catalyst Pd HCS of multicore.The characteristics of catalyst of the invention is a shell coenocytism, possesses multiple Pd particles in the same carbon shell, has catalytic contact area big, high catalytic efficiency.
Description
Technical field
The present invention relates to the preparation method of catalyst Pd@HCS a kind of, an especially a kind of shell multicore yolk shell catalyst
The preparation method of Pd@HCS.
Background technique
H2And O2Directly synthesize H2O2It the advantages that environmentally protective, Atom economy and simple process, is studied all the time
The extensive concern of person is expected to the anthraquinone synthesis H of substitution tradition2O2Synthetic method.However, H2O2Selectivity and yield still
It is very low, this is because other than main reaction (formula 1-1) occurs, while there is also three side reactions (formula 1-2,1-3 and 1-4), because
This reduces H2O2Selectivity and yield.
H2+O2→H2O2 △G0 298K=-120.4kJ/mol (1-1)
H2+1/2O2→H2O △G0 298K=-237.2kJ/mol (1-2)
H2O2→H2O+1/2O2 △G0 298K=-116.8kJ/mol (1-3)
H2O2+H2→2H2O △G0 298K=-354.0kJ/mol (1-4)
In order to improve H2O2Selectivity and yield, researcher have been devoted to catalyst research, Pd is normally used as activity
Component prepares Pd base catalyst for directly synthesizing H2O2.Currently, Pd base catalyst mainly has Pd base supported catalyst, however
Loaded catalyst active component Pd is easy to migrate to reunite and falls off.In consideration of it, researcher's design has synthesized a kind of novel yolk shell
Pd base catalyst.
But the H of existing current core-shell structure2O2Catalyst is one shell structure of a core, contains only one in a carbon shell
Pd particle, since really play catalytic action is internal Pd particle, mononuclear structure can inevitably reduce reaction gas and Pd
The contact area of particle, to reduce catalytic efficiency.Therefore, how improving the catalytic efficiency of the catalyst of core-shell structure, have very much must
It wants.
Summary of the invention
The object of the present invention is to provide the preparation methods of one shell multicore yolk shell catalyst Pd@HCS of one kind.The present invention
Catalyst be a shell coenocytism, possess multiple Pd particles in the same carbon shell, have catalytic contact area big, catalytic efficiency
High feature.
Technical solution of the present invention: the preparation method of one shell multicore yolk shell catalyst Pd@HCS of one kind, including walk as follows
It is rapid:
(1) SiO is prepared2: by ethyl alcohol, deionized water and NH3·H2O mixed solution stirs evenly at 20-30 DEG C, then
TEOS is added and reacts 1-3h, product obtains SiO through ethyl alcohol centrifuge washing2；
(2)SiO2-NH2Preparation: by the SiO of preparation2Ultrasonic disperse stirs at 70-90 DEG C in aqueous isopropanol
Uniformly, APTES is then added, and keeps temperature reflux 2-4h, then cools to room temperature, product is obtained through ethyl alcohol centrifuge washing
SiO2-NH2；
(3)Pd/SiO2-NH2Synthesis: firstly, by SiO2-NH2Ultrasonic disperse stirs in ethanol solution in 30-40 DEG C
Uniformly；Then H is added2PdCl4Solution stirs 1-3h；Finally, NaBH is added4Solution, react 20-40min, product through ethyl alcohol from
Heart washing, obtains Pd/SiO2-NH2；
(4)Pd/SiO2-NH2The preparation of@RF: firstly, by the Pd/SiO of preparation2-NH2Ultrasound is dispersed in deionized water
In, ethanol solution is then added, at 30-40 DEG C after mixing evenly, sequentially adds CTAB, resorcinol and NH3·H2O, stirring
To the uniform dispersion liquid of formation；Then formalin is added, is cooled to room temperature after reacting 12-20h, product is through ethyl alcohol centrifuge washing
Afterwards in 40-60 DEG C of oven drying 10-15h, Pd/SiO is obtained2-NH2@RF；
The preparation of (5) one shell multicore yolk shell catalyst Pd@HCS: Pd@SiO obtained2-NH2@RF is in a nitrogen atmosphere
1-3h is roasted at 550-650 DEG C obtains Pd@SiO2@C, by Pd@SiO2@C disperses in deionized water, HF solution, room temperature etching to be added
20-30h, through be centrifuged and water washing after at 70-90 DEG C of dry 10-15h, 200-300 DEG C roasting oxidation 1-3h and hydrogen atmosphere
Lower reductase 12-3h obtains one shell yolk shell structure catalyst Pd@HCS of multicore.
The preparation method of shell multicore yolk shell catalyst Pd@HCS above-mentioned is by 62ml second in the step (1)
Alcohol, 25ml deionized water and 1.5mlNH3·H2O mixing, is then added 4.5mlTEOS.
The preparation method of shell multicore yolk shell catalyst Pd@HCS above-mentioned in the step (2), will be prepared
SiO21.5mlAPTES is added in 180ml aqueous isopropanol in ultrasonic disperse after stirring.
The preparation method of shell multicore yolk shell catalyst Pd@HCS above-mentioned is first by SiO in the step (3)2-
NH21mlH is added in 100ml ethanol solution in ultrasonic disperse after stirring2PdCl4Solution, finally, 300 μ l NaBH are added4It is molten
Liquid.
The preparation method of shell multicore yolk shell catalyst Pd@HCS above-mentioned, the H2PdCl4The concentration of solution is
0.075M, NaBH4The concentration of solution is 10wt%.
The preparation method of shell multicore yolk shell catalyst Pd@HCS above-mentioned is first by preparation in the step (4)
Pd/SiO2-NH2Ultrasound is dispersed in 70ml deionized water, and 30ml ethanol solution is then added, after stirring, sequentially adds
2.0gCTAB, 0.35g resorcinol and 0.2mlNH3·H2O；Then 0.5ml formalin is added.
The preparation method of shell multicore yolk shell catalyst Pd@HCS above-mentioned is by Pd@SiO in the step (5)2@
C is dispersed in 35ml deionized water, and 5mlHF solution is added.
The preparation method of shell multicore yolk shell catalyst Pd@HCS above-mentioned, the step (1), (2), (3) and (4)
In ethyl alcohol centrifuge washing and the number of centrifugation and water washing in step (5) be 2-4 times.
Beneficial effects of the present invention
The present invention has produced the catalyst Pd@HCS with a shell coenocytism by above-mentioned technique, as shown in Figure 1,
Pd number of particles in carbon shell obviously increases, and therefore, the specific surface area of Pd particle in a carbon shell can be greatly increased, to mention
For more reaction gas reaction sites, catalytic efficiency is improved.
Detailed description of the invention
Attached drawing 1 is the synthetic route chart of catalyst of the present invention.
Specific embodiment
Below with reference to embodiment, the present invention is further illustrated, but is not intended as the foundation limited the present invention.
The embodiment of the present invention
Embodiment 1: the preparation method of one shell multicore yolk shell catalyst Pd@HCS of one kind, steps are as follows:
(1) SiO is prepared2: by 62ml ethyl alcohol, 25ml deionized water and 1.5mlNH3·H2O mixed solution stirs at 25 DEG C
Then 15min is added 4.5mlTEOS and reacts 2h, product obtains SiO through ethyl alcohol centrifuge washing 3 times2；
(2)SiO2-NH2Preparation: by the SiO of preparation2Ultrasonic disperse stirs at 80 DEG C in 180ml aqueous isopropanol
Then 1.5mlAPTES is added in 5min, and keep temperature reflux 3h, is cooled to room temperature, product through ethyl alcohol centrifuge washing 3 times,
Obtain SiO2-NH2；
(3)Pd/SiO2-NH2Synthesis: firstly, by SiO2-NH2Ultrasonic disperse stirs in 100ml ethanol solution in 35 DEG C
Mix 10min；Then 1mlH is added2PdCl4Solution (0.075M) stirs 2h；Finally, 300 μ l NaBH are added4Solution
(10wt%), reacts 30min, and product obtains Pd/SiO through ethyl alcohol centrifuge washing 3 times2-NH2；
(4)Pd/SiO2-NH2The preparation of@RF: firstly, by the Pd/SiO of preparation2-NH2Ultrasound is dispersed in deionized water
In (70ml), 30ml ethanol solution is then added, after stirring 10min at 35 DEG C, sequentially adds 2.0gCTAB, 0.35g isophthalic
Diphenol and 0.2mlNH3·H2O, stirring 1h form uniform dispersion liquid；Then 0.5ml formalin is added, reacts cooling after 16h
To room temperature, product, in 50 DEG C of oven drying 12h, obtains Pd/SiO after being centrifuged with ethanol washing 3 times2-NH2@RF；
The preparation of (5) one shell multicore yolk shell catalyst Pd@HCS: Pd@SiO obtained2-NH2@RF is in a nitrogen atmosphere
2h is roasted at 600 DEG C obtains Pd@SiO2@C, by Pd@SiO2@C is dispersed in 35ml deionized water, and 5mlHF solution is added, and room temperature is carved
Erosion for 24 hours, be centrifuged and water washing 3 times after at 80 DEG C of dry 12h, 250 DEG C reductase 12 .5h under roasting oxidation 2h and hydrogen atmosphere,
Obtain one shell yolk shell structure catalyst Pd@HCS of multicore.
Embodiment 2: the preparation method of one shell multicore yolk shell catalyst Pd@HCS of one kind, steps are as follows:
(1) SiO is prepared2: by 62ml ethyl alcohol, 25ml deionized water and 1.5mlNH3·H2O mixed solution stirs at 20 DEG C
Then 15min is added 4.5mlTEOS and reacts 1h, product obtains SiO through ethyl alcohol centrifuge washing 2 times2；
(2)SiO2-NH2Preparation: by the SiO of preparation2Ultrasonic disperse stirs at 70 DEG C in 180ml aqueous isopropanol
Then 1.5mlAPTES is added in 5min, and keep temperature reflux 2h, is cooled to room temperature, product through ethyl alcohol centrifuge washing 3 times,
Obtain SiO2-NH2；
(3)Pd/SiO2-NH2Synthesis: firstly, by SiO2-NH2Ultrasonic disperse stirs in 100ml ethanol solution in 30 DEG C
Mix 10min；Then 1mlH is added2PdCl4Solution (0.075M) stirs 1h；Finally, 300 μ l NaBH are added4Solution
(10wt%), reacts 20min, and product obtains Pd/SiO through ethyl alcohol centrifuge washing 2 times2-NH2；
(4)Pd/SiO2-NH2The preparation of@RF: firstly, by the Pd/SiO of preparation2-NH2Ultrasound is dispersed in deionized water
In (70ml), 30ml ethanol solution is then added, after stirring 10min at 30 DEG C, sequentially adds 2.0gCTAB, 0.35g isophthalic
Diphenol and 0.2mlNH3·H2O, stirring 1h form uniform dispersion liquid；Then 0.5ml formalin is added, reacts cooling after 12h
To room temperature, product, in 40 DEG C of oven drying 10h, obtains Pd/SiO after being centrifuged with ethanol washing 2 times2-NH2@RF；
The preparation of (5) one shell multicore yolk shell catalyst Pd@HCS: Pd@SiO obtained2-NH2@RF is in a nitrogen atmosphere
1h is roasted at 550 DEG C obtains Pd@SiO2@C, by Pd@SiO2@C is dispersed in 35ml deionized water, and 5mlHF solution is added, and room temperature is carved
Lose 20h, be centrifuged and water washing 2 times after at 70 DEG C of dry 10h, 200 DEG C reductase 12 h under roasting oxidation 1h and hydrogen atmosphere, obtain
To one shell yolk shell structure catalyst Pd@HCS of multicore.
Embodiment 3: the preparation method of one shell multicore yolk shell catalyst Pd@HCS of one kind, steps are as follows:
(1) SiO is prepared2: by 62ml ethyl alcohol, 25ml deionized water and 1.5mlNH3·H2O mixed solution stirs at 30 DEG C
Then 15min is added 4.5mlTEOS and reacts 3h, product obtains SiO through ethyl alcohol centrifuge washing 4 times2；
(2)SiO2-NH2Preparation: by the SiO of preparation2Ultrasonic disperse stirs at 90 DEG C in 180ml aqueous isopropanol
Then 1.5mlAPTES is added in 5min, and keep temperature reflux 4h, is cooled to room temperature, product through ethyl alcohol centrifuge washing 4 times,
Obtain SiO2-NH2；
(3)Pd/SiO2-NH2Synthesis: firstly, by SiO2-NH2Ultrasonic disperse stirs in 100ml ethanol solution in 40 DEG C
Mix 10min；Then 1mlH is added2PdCl4Solution (0.075M) stirs 3h；Finally, 300 μ l NaBH are added4Solution
(10wt%), reacts 40min, and product obtains Pd/SiO through ethyl alcohol centrifuge washing 3 times2-NH2；
(4)Pd/SiO2-NH2The preparation of@RF: firstly, by the Pd/SiO of preparation2-NH2Ultrasound is dispersed in deionized water
In (70ml), 30ml ethanol solution is then added, after stirring 10min at 40 DEG C, sequentially adds 2.0gCTAB, 0.35g isophthalic
Diphenol and 0.2mlNH3·H2O, stirring 1h form uniform dispersion liquid；Then 0.5ml formalin is added, reacts cooling after 20h
To room temperature, product, in 60 DEG C of oven drying 15h, obtains Pd/SiO after being centrifuged with ethanol washing 4 times2-NH2@RF；
The preparation of (5) one shell multicore yolk shell catalyst Pd@HCS: Pd@SiO obtained2-NH2@RF is in a nitrogen atmosphere
3h is roasted at 650 DEG C obtains Pd@SiO2@C, by Pd@SiO2@C is dispersed in 35ml deionized water, and 5mlHF solution is added, and room temperature is carved
30h is lost, 3h is restored under roasting oxidation 3h and hydrogen atmosphere at 90 DEG C of dry 15h, 300 DEG C after being centrifuged with water washing 4 times, obtains
To one shell yolk shell structure catalyst Pd@HCS of multicore.
Claims (8)
1. the preparation method of one shell multicore yolk shell catalyst Pd@HCS of one kind, which comprises the steps of:
(1) SiO is prepared2: by ethyl alcohol, deionized water and NH3·H2O mixed solution stirs evenly at 20-30 DEG C, is then added
TEOS simultaneously reacts 1-3h, and product obtains SiO through ethyl alcohol centrifuge washing2；
(2)SiO2-NH2Preparation: by the SiO of preparation2Ultrasonic disperse stirs evenly at 70-90 DEG C in aqueous isopropanol,
Then APTES is added, and keeps temperature reflux 2-4h, then cools to room temperature, product obtains SiO through ethyl alcohol centrifuge washing2-
NH2；
(3)Pd/SiO2-NH2Synthesis: firstly, by SiO2-NH2Ultrasonic disperse stirs evenly in ethanol solution in 30-40 DEG C；
Then H is added2PdCl4Solution stirs 1-3h；Finally, NaBH is added4Solution, reacts 20-40min, and product is washed through ethyl alcohol centrifugation
It washs, obtains Pd/SiO2-NH2；
(4)Pd/SiO2-NH2The preparation of@RF: firstly, by the Pd/SiO of preparation2-NH2Ultrasound is evenly dispersed in deionized water, with
After ethanol solution is added, at 30-40 DEG C after mixing evenly, sequentially add CTAB, resorcinol and NH3·H2O, stirring to shape
At uniform dispersion liquid；Then be added formalin, be cooled to room temperature after reacting 12-20h, product after ethyl alcohol centrifuge washing in
In 40-60 DEG C of oven drying 10-15h, Pd/SiO is obtained2-NH2@RF；
The preparation of (5) one shell multicore yolk shell catalyst Pd@HCS: Pd@SiO obtained2-NH2@RF 550- in a nitrogen atmosphere
1-3h is roasted at 650 DEG C obtains Pd@SiO2@C, by Pd@SiO2@C disperses in deionized water, HF solution to be added, and room temperature etches 20-
30h is centrifuged and is gone back under roasting oxidation 1-3h and hydrogen atmosphere at 70-90 DEG C of dry 10-15h, 200-300 DEG C after water washing
Former 2-3h obtains one shell yolk shell structure catalyst Pd@HCS of multicore.
2. the preparation method of shell multicore yolk shell catalyst Pd@HCS according to claim 1, it is characterised in that: described
It is by 62ml ethyl alcohol, 25ml deionized water and 1.5mlNH in step (1)3·H2O mixing, is then added 4.5mlTEOS.
3. the preparation method of shell multicore yolk shell catalyst Pd@HCS according to claim 1, it is characterised in that: described
It is the SiO that will be prepared in step (2)21.5mlAPTES is added in 180ml aqueous isopropanol in ultrasonic disperse after stirring.
4. the preparation method of shell multicore yolk shell catalyst Pd@HCS according to claim 1, it is characterised in that: described
It is first by SiO in step (3)2-NH21mlH is added in 100ml ethanol solution in ultrasonic disperse after stirring2PdCl4Solution, most
Afterwards, 300 μ lNaBH are added4Solution.
5. the preparation method of shell multicore yolk shell catalyst Pd@HCS according to claim 4, it is characterised in that: described
H2PdCl4The concentration of solution is 0.075M, NaBH4The concentration of solution is 10wt%.
6. the preparation method of shell multicore yolk shell catalyst Pd@HCS according to claim 1, it is characterised in that: described
It is the Pd/SiO first by preparation in step (4)2-NH2Ultrasound is dispersed in 70ml deionized water, and 30ml ethyl alcohol is then added
Solution after stirring, sequentially adds 2.0gCTAB, 0.35g resorcinol and 0.2mlNH3·H2O；Then it is molten that 0.5ml formaldehyde is added
Liquid.
7. the preparation method of shell multicore yolk shell catalyst Pd@HCS according to claim 1, it is characterised in that: described
It is by Pd@SiO in step (5)2@C is dispersed in 35ml deionized water, and 5mlHF solution is added.
8. the preparation method of shell multicore yolk shell catalyst Pd@HCS according to claim 1, it is characterised in that: described
Ethyl alcohol centrifuge washing in step (1), (2), (3) and (4) and the number of centrifugation and water washing in step (5) are 2-4
It is secondary.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111905763A (en) * | 2020-09-08 | 2020-11-10 | 中国科学技术大学 | Yolk-shell structure composite photocatalyst capable of efficiently producing hydrogen and preparation method and application thereof |
| CN112062919A (en) * | 2020-09-11 | 2020-12-11 | 华东理工大学 | Preparation method and application method of phenolic resin with hollow shell structure |
| CN113101974A (en) * | 2021-04-19 | 2021-07-13 | 宁夏德昊科技产业有限公司 | Method for preparing o-aminophenol by hydrogenation reduction catalysis |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107754826A (en) * | 2017-11-06 | 2018-03-06 | 贵州大学 | A kind of producing hydrogen peroxide by direct synthesis hollow core shell structure Pd catalyst and preparation method thereof |
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| CN112062919A (en) * | 2020-09-11 | 2020-12-11 | 华东理工大学 | Preparation method and application method of phenolic resin with hollow shell structure |
| CN112062919B (en) * | 2020-09-11 | 2022-08-30 | 华东理工大学 | Preparation method and application method of phenolic resin with hollow shell structure |
| CN113101974A (en) * | 2021-04-19 | 2021-07-13 | 宁夏德昊科技产业有限公司 | Method for preparing o-aminophenol by hydrogenation reduction catalysis |
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