cMOF Evidence Base

Synthesis evidence

Synthesis and structure of anhydrous Zn2EDTA metal-organic framework

Starodubtseva A.A., Kan T.V., Marshenya S.N. et al. · Polyhedron · 2024 · 116750

2 structured synthesis routes

Completeness describes how fully the route could be reconstructed from the main article and supporting information.

Complete recipeSource: Main

Route 1: Other

p003 / journal page 3 · Experimental

Metal precursorsZn2EDTA powder
SolventsN-methylpyrrolidone
AdditivesTIMCAL SUPER C45 conductive additive; PVDF binder
Atmospherevacuum oven for final drying
Temperature70 then 120
Time1 then 24
Substrate orientationgraphite foil; Doctor Blade 100 micrometre
Work-upGrind slurry in agate mortar, apply thin layer by Doctor Blade onto graphite foil, dry at 70 degC for 1 h, then vacuum dry at 120 degC for 24 h.
ActivationVacuum drying at 120 degC for 24 h before electrochemical testing.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
OtherZn2(EDTA)70 wt% of solids ratiop003 / journal page 3 · Experimental
AdditiveTIMCAL SUPER C45 conductive additive20 wt% of solids ratiop003 / journal page 3 · Experimental
Additivepolyvinylidene fluoride (PVDF)10 wt% of solids ratio · 3 wt% in N-methylpyrrolidonep003 / journal page 3 · Experimental
SolventN-methylpyrrolidoneNot specifiedp003 / journal page 3 · Experimental
Complete recipeSource: Main

Route 2: Hydrothermal

p002 / journal page 2 · Experimental

Metal precursorsZnCl2 solution (Aldrich, 99%), approximately 0.5 M; 6-8 mL aliquot depending on established Zn2+ concentration
Linker precursorsNa2H2EDTA.2H2O powder (Aldrich, 99%), 0.675 g
Solvents25 mL deionised water
Additives10 M KOH solution added dropwise to dissolve mixture and adjust pH to 2.5-4; pure Zn2EDTA optimum at pH 2.7
Atmospherenot specified
Temperature180
Time24
Work-upCool autoclave to room temperature; separate crystalline product from mother liquor by repeated decantation-washing with water; dry at 120 degC for 4 h in oven.
ActivationNo separate activation reported beyond drying at 120 degC for 4 h.
Scalability contextNo scale-up test; authors motivate EDTA and zinc as inexpensive resources.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal Sourcezinc chloride ZnCl2 (Aldrich, 99%) solution6-8 ml aliquot · approximately 0.5 M; exact concentration established by titrationp002 / journal page 2 · Experimental
LinkerNa2H2EDTA.2H2O (Aldrich, 99%) powder0.675 gp002 / journal page 2 · Experimental
Solventdeionized water25 mlp002 / journal page 2 · Experimental
Basepotassium hydroxide KOH (Aldrich, 99%) solutionadded dropwise until dissolved and required pH reached · 10 Mp002 / journal page 2 · Experimental