Electrochemistry Application — Pd-Embedded Ti Metal–Organic Framework Nanostructures for Photocatalytic Reductive N-Formylation of Nitroarenes in Water

7 measurement groups · 51 results

Reported values remain attached to the sample, method, conditions, extraction quality and source location that produced them.

Photocatalytic N-formylation of substituted nitrobenzene derivatives

Pd1.5%/Ti-MOF · Powder

Reactant 0.3 mmol, HCOOH 8 equiv, Pd1.5%/Ti-MOF 30 mg, H2O 3 mL, 6 h, white LED 5 W x 4; data mean +/- SD, n=3.

Geometry: glass vessel
Context: target composite application scope
Measurement source: p008 / article p471 · Photocatalytic Activity · Table 2

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
4-amino N-formyl product selectivity	84 +/- 0.9 %	—	+/- 0.9	Table Exact Reported	p008 / article p471 · Photocatalytic Activity · Table 2
4-aminonitrobenzene conversionMarked as a best value within this paper	100 %	—	—	Table Exact Reported	p008 / article p471 · Photocatalytic Activity · Table 2
4-chloro N-formyl product selectivity	88 +/- 0.9 %	—	+/- 0.9	Table Exact Reported	p008 / article p471 · Photocatalytic Activity · Table 2
4-chloronitrobenzene conversion	96 +/- 1.6 %	—	+/- 1.6	Table Exact Reported	p008 / article p471 · Photocatalytic Activity · Table 2
4-hydroxy N-formyl product selectivity	79 +/- 0.6 %	—	+/- 0.6	Table Exact Reported	p008 / article p471 · Photocatalytic Activity · Table 2
4-hydroxynitrobenzene conversion	90 +/- 1.4 %	—	+/- 1.4	Table Exact Reported	p008 / article p471 · Photocatalytic Activity · Table 2
4-methoxy N-formyl product selectivity	88 +/- 0.9 %	—	+/- 0.9	Table Exact Reported	p008 / article p471 · Photocatalytic Activity · Table 2
4-methoxynitrobenzene conversion	86 +/- 1.8 %	—	+/- 1.8	Table Exact Reported	p008 / article p471 · Photocatalytic Activity · Table 2
4-methyl N-formyl product selectivity	89 +/- 1.0 %	—	+/- 1.0	Table Exact Reported	p008 / article p471 · Photocatalytic Activity · Table 2
4-methylnitrobenzene conversion	98 +/- 1.4 %	—	+/- 1.4	Table Exact Reported	p008 / article p471 · Photocatalytic Activity · Table 2

Photocatalytic N-formylation of nitrobenzene (GC-FID/GC-MS)

Pd1.5%/Ti-MOF · Powder

NB 0.3 mmol, HCOOH 8 equiv unless noted, catalyst 30 mg, solvent 3 mL, 6 h, white LED 5 W x 4 unless noted; data mean +/- SD, n=3.

Atmosphere: reaction vessel deaerated before photocatalysis
Geometry: glass vessel
Context: application table with pristine and Pd-loaded controls
Measurement source: p007 / article p470 · Photocatalytic Activity · Table 1

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
Pd1.5%/Ti-MOF N-formyl AN (1B) selectivity in H2O under LED	91 +/- 0.4 %	—	+/- 0.4	Table Exact Reported	p007 / article p470 · Photocatalytic Activity · Table 1
Pd1.5%/Ti-MOF 1B selectivity after 2 h	58 %	—	—	Text Exact Reported	p008 / article p471 · Photocatalytic Activity · Figure S7 referenced
Pd1.5%/Ti-MOF conversion after 2 h	29 %	—	—	Text Exact Reported	p008 / article p471 · Photocatalytic Activity · Figure S7 referenced
Pd1.5%/Ti-MOF conversion after 6 hMarked as a best value within this paper	complete NB conversion occurred in 6 h	—	—	Text Exact Reported	p008 / article p471 · Photocatalytic Activity · Figure S7 referenced
Pd1.5%/Ti-MOF N-formyl AN (1B) selectivity in acetonitrile	84 +/- 0.4 %	—	+/- 0.4	Table Exact Reported	p007 / article p470 · Photocatalytic Activity · Table 1
Pd1.5%/Ti-MOF NB conversion in acetonitrile	81 +/- 1.5 %	—	+/- 1.5	Table Exact Reported	p007 / article p470 · Photocatalytic Activity · Table 1
Pd1.5%/Ti-MOF NB conversion in H2O under LEDMarked as a best value within this paper	100 %	—	—	Table Exact Reported	p007 / article p470 · Photocatalytic Activity · Table 1
Pd1.5%/Ti-MOF 1B selectivity with 10 equiv HCOOHMarked as a best value within this paper	92 +/- 0.2 %	—	+/- 0.2	Table Exact Reported	p007-p008 / article pp470-471 · Photocatalytic Activity · Table 1
Pd1.5%/Ti-MOF 1B selectivity with 6 equiv HCOOH	84 +/- 1.4 %	—	+/- 1.4	Table Exact Reported	p007-p008 / article pp470-471 · Photocatalytic Activity · Table 1
Pd1.5%/Ti-MOF N-formyl AN (1B) selectivity under sunlight	88 +/- 0.4 %	—	+/- 0.4	Table Exact Reported	p007 / article p470 · Photocatalytic Activity · Table 1
Pd1.5%/Ti-MOF NB conversion under sunlight for 4 hMarked as a best value within this paper	100 %	—	—	Table Exact Reported	p007 / article p470 · Photocatalytic Activity · Table 1
Pd1.5%/Ti-MOF N-formyl AN (1B) selectivity in tolueneMarked as a best value within this paper	96 +/- 0.2 %	—	+/- 0.2	Table Exact Reported	p007-p008 / article pp470-471 · Photocatalytic Activity · Table 1
Pd1.5%/Ti-MOF NB conversion in toluene	88 +/- 1.8 %	—	+/- 1.8	Table Exact Reported	p007-p008 / article pp470-471 · Photocatalytic Activity · Table 1
Pd1%/Ti-MOF N-formyl AN (1B) selectivity	90 +/- 1.5 %	—	+/- 1.5	Table Exact Reported	p007 / article p470 · Photocatalytic Activity · Table 1
Pd1%/Ti-MOF NB conversion in H2O under LED	89 +/- 1.4 %	—	+/- 1.4	Table Exact Reported	p007 / article p470 · Photocatalytic Activity · Table 1
Pd2.5%/Ti-MOF N-formyl AN (1B) selectivityMarked as a best value within this paper	93 +/- 0.2 %	—	+/- 0.2	Table Exact Reported	p007 / article p470 · Photocatalytic Activity · Table 1
Pd2.5%/Ti-MOF NB conversion in H2O under LED	98 +/- 1.3 %	—	+/- 1.3	Table Exact Reported	p007 / article p470 · Photocatalytic Activity · Table 1
Pd2%/Ti-MOF N-formyl AN (1B) selectivity	92 +/- 0.4 %	—	+/- 0.4	Table Exact Reported	p007 / article p470 · Photocatalytic Activity · Table 1
Pd2%/Ti-MOF NB conversion in H2O under LEDMarked as a best value within this paper	100 %	—	—	Table Exact Reported	p007 / article p470 · Photocatalytic Activity · Table 1
Pd NP N-formyl AN (1B) selectivity	62 +/- 1.4 %	—	+/- 1.4	Table Exact Reported	p007 / article p470 · Photocatalytic Activity · Table 1
Pd NP NB conversion in H2O under LED	12 +/- 1.6 %	—	+/- 1.6	Table Exact Reported	p007 / article p470 · Photocatalytic Activity · Table 1
Ti-MOF N-formyl AN (1B) selectivity	45 +/- 1.2 %	—	+/- 1.2	Table Exact Reported	p007 / article p470 · Photocatalytic Activity · Table 1
Ti-MOF NB conversion in H2O under LED	8 +/- 1.2 %	—	+/- 1.2	Table Exact Reported	p007 / article p470 · Photocatalytic Activity · Table 1

Mechanistic control reactions

Pd1.5%/Ti-MOF · Powder

Control reactions with AN/HCOOH, NB or AN with CO2 + H2 gas mixture, CO2 only, and absence of HCOOH/light/catalyst.

Geometry: photocatalytic glass reactor for gas-mixture controls
Context: target composite mechanistic controls
Measurement source: p009-p010 / article pp472-473 · Mechanistic Study · Scheme 2 discussion

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
NB conversion without light, photocatalyst, or HCOOH	No NB conversion observed	—	—	Text Qualitative	p008 / article p471 · Photocatalytic Activity
AN + CO2/H2 gas mixture conversion	92 %	—	—	Text Exact Reported	p009-p010 / article pp472-473 · Mechanistic Study · Scheme 2 discussion
AN + CO2/H2 gas mixture N-formyl AN selectivityMarked as a best value within this paper	complete selectivity	—	—	Text Qualitative	p009-p010 / article pp472-473 · Mechanistic Study · Scheme 2 discussion
AN + HCOOH conversion over Pd1.5%/Ti-MOF	99 %	—	—	Text Exact Reported	p009-p010 / article pp472-473 · Mechanistic Study · Scheme 2 discussion
AN + HCOOH N-formyl AN selectivityMarked as a best value within this paper	100 %	—	—	Text Exact Reported	p009-p010 / article pp472-473 · Mechanistic Study · Scheme 2 discussion
CO2-only control N-formyl AN product	no N-formyl AN product detected	—	—	Text Qualitative	p010 / article p473 · Mechanistic Study · Scheme 2 discussion
NB + CO2/H2 gas mixture conversion	78 %	—	—	Text Exact Reported	p009-p010 / article pp472-473 · Mechanistic Study · Scheme 2 discussion
NB + CO2/H2 gas mixture N-formyl AN selectivity	68 %	—	—	Text Exact Reported	p009-p010 / article pp472-473 · Mechanistic Study · Scheme 2 discussion

GC-TCD chromatogram of HCOOH photodecomposition

Pd1.5%/Ti-MOF · Powder

Photochemical decomposition of HCOOH over Pd1.5%/Ti-MOF; embedded peak table in SI Figure S10 reports gas concentrations.

Context: target composite mechanistic gas analysis
Measurement source: p010 / SI pS10 · Figure S10 · Figure S10

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
CH4 concentration in GC-TCD report	20.762 PPM	—	—	Visual Estimate Approximate	p010 / SI pS10 · Figure S10 · Figure S10
CO2 concentration in HCOOH photodecomposition gasMarked as a best value within this paper	379833.410 PPM	—	—	Visual Estimate Approximate	p010 / SI pS10 · Figure S10 · Figure S10
H2 concentration in HCOOH photodecomposition gas	10.048 PPM	—	—	Visual Estimate Approximate	p010 / SI pS10 · Figure S10 · Figure S10
CO detected in HCOOH photodecomposition gas	no CO detected	—	—	Text Qualitative	p010 / SI pS10 · Figure S10 · Figure S10

Photocatalyst recycling test

Pd1.5%/Ti-MOF · Powder

Recycling in N-formylation of NB over Pd1.5%/Ti-MOF.

Context: target composite stability
Measurement source: p008-p009 / article pp471-472 · Photocatalytic Activity · Figure 7a

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
Pd1.5%/Ti-MOF fifth-cycle NB conversion	98 %	—	—	Text Exact Reported	p008 / article p471 · Photocatalytic Activity · Figure 7a

Electron- and hole-scavenging experiments

Pd1.5%/Ti-MOF · Powder

Electron trapping with ammonium persulfate; hole trapping with EDTA, TEOA, methanol, and citric acid.

Context: target composite mechanistic controls
Measurement source: p009-p010 / article pp472-473 · Mechanistic Study · Figure 7b,c

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
NB conversion with ammonium persulfate electron trap	8 %	—	—	Text Exact Reported	p010 / article p473 · Mechanistic Study · Figure 7b
NB conversion with citric acid hole scavenger	58 %	—	—	Text Exact Reported	p010 / article p473 · Mechanistic Study · Figure 7c
NB conversion with methanol hole scavenger	31 %	—	—	Text Exact Reported	p010 / article p473 · Mechanistic Study · Figure 7c

Comparative photocatalytic activity table

Pd1.5%/Ti-MOF · Powder

SI Table S3 compares Pd1.5%/Ti-MOF with reported photocatalysts; current catalyst conditions: NB 0.3 mmol, HCOOH 2.4 mmol, catalyst 30 mg, 6 h, water 3 mL, 20 W household white LED bulb.

Context: target composite comparative activity
Measurement source: p004 / SI pS4 · Table S3 · Table S3

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
Pd1.5%/Ti-MOF comparative N-formyl aniline yield	91 %	—	—	SI Table Exact Reported	p004 / SI pS4 · Table S3 · Table S3
Pd1.5%/Ti-MOF TOF in comparative tableMarked as a best value within this paper	11.6 h-1	—	—	SI Table Exact Reported	p004 / SI pS4 · Table S3 · Table S3