LO and all the reagents used for the chemical modification of the triglyceride structure and product purification were purchased from Sigma-Aldrich (Merck KGaA, Darmstadt, Germany). The components of the curing process: citric acid monohydrate (99.5+%) acquired from Alfa Aesar (Thermo Fisher Scientific, Waltham, Massachusetts, United States), anhydrous THF (≥99.9%, inhibitor-free) from Sigma-Aldrich (Merck KGaA, Darmstadt, Germany) and Jeffamine D230, kindly supplied by Huntsman (Texas, United States), were used as received, without any purification.
Anhydrous thf
Manufactured by Merck Group
Sourced in United States
Anhydrous THF is a colorless, volatile, and highly flammable liquid. It is commonly used as a solvent in organic synthesis and various laboratory applications. Anhydrous THF has a low boiling point and is typically stored and handled under inert atmospheric conditions to prevent contamination and degradation.
Automatically generated - may contain errors
Lab products found in correlation
Jeffamine d230, by Merck Group (1 mentions)
Tatato, by Merck Group (1 mentions)
Anhydrous dcm, by Merck Group (1 mentions)
Palladium acetate, by Merck Group (1 mentions)
Anhydrous methanol, by Merck Group (1 mentions)
Dmso d6, by Merck Group (1 mentions)
Ammonium hydroxide, by Thermo Fisher Scientific (1 mentions)
Cd3od, by Merck Group (1 mentions)
Cdcl3, by Merck Group (1 mentions)
Ch2cl2, by Merck Group (1 mentions)
Cd2cl2, by Merck Group (1 mentions)
Copper 2 acetate, by Merck Group (1 mentions)
Anhydrous dmf, by Merck Group (1 mentions)
3 picoline, by Avantor (1 mentions)
Diisopropyl azodicarboxylate, by Merck Group (1 mentions)
Benzotrifluoride, by Merck Group (1 mentions)
2 2 azobisisobutyronitrile aibn, by Junsei (1 mentions)
Citric acid monohydrate, by Thermo Fisher Scientific (1 mentions)
Sncl2, by Thermo Fisher Scientific (1 mentions)
Pdcl2, by Thermo Fisher Scientific (1 mentions)
8 protocols using anhydrous thf
1
Triglyceride Modification and Purification
2
Synthesis of Diacrylate LC Monomers
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Diacrylate LC monomers RM257 and RM82 were purchased from Wilshire Technologies. EDDT, TATATO, TPO, radical inhibitor butylated hydroxytoluene (BHT), anhydrous DCM, and anhydrous THF were purchased from Sigma-Aldrich. All reagents and solvents were used as received without further purification.
3
Synthesis of Palladium-Containing Precursor
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All of the synthesis reactions were carried out according to our recently reported method [18 (link),35 (link)] as follows. First, 10 g of Durazane 1800 (dur Xtreme Gmbh, Ulm, Germany) was dissolved in anhydrous THF (50 mL) and then added into a dropping funnel. Then, 4 g of Palladium acetate (≥99.9, Sigma-Aldrich, Burlington, MA, USA) was dispersed in 50 mL of anhydrous THF (≥99.9, Sigma-Aldrich, Burlington, MA, USA) and added into a round flask. The flask and dropping funnel were first assembled in the glovebox, and the reaction vessel was immediately removed from the glovebox and submerged in the ice bath (−6 °C) and connected to Schlenk lines. The synthesis process was continued under stirring and argon flow in the ice bath for 2 h and followed by 24 h at room temperature until the end of gas liberation (Figure S1 ). Finally, the THF was removed under vacuum for at least 5 h, and the synthesized Pd-containing precursor was collected in the glovebox. The synthesized Pd-containing precursor is denoted as Du1800-Pd.
4
Anhydrous Solvent Preparation for Polymer Solutions
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Inhibitor-free anhydrous THF ( ≥ 99.9%) and anhydrous methanol (99.8%) were purchased from Sigma-Aldrich and used without further purification. Predetermined quantities of PSS:Im-b-PMB (or PSS:Im), ZImS, and neutral Im were dissolved into 80/20 vol.% methanol/THF mixtures to prepare ca. 5 wt% solutions using the balance (Mettler Toledo, ME 204) inside the argon-filled glove box. Under argon atmosphere, solvents were slowly evaporated at room temperature for 2 days and were further exposed to vacuum at 70 °C for 7 days.
5
Synthesis of Organometallic Complexes
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Chemicals were obtained from the following suppliers: diisopropylamine, 2.5 M n-butyl lithium in hexanes (Acros); EDTA, AgOTf, 4,4′-dimethyl-2,2′-bipyridine, sodium sulfide, celite 512 medium, Et3N, 2-chloro-methylpyridinium iodide, triethanolamine, anhydrous DMF, methyl chloroformate, copper(ii ) acetate (Aldrich); 3-picoline (BDH Chemicals); CO2 – CP-grade with 5% CH4 (or 1% CH4) (BOC); Na2SO4, Na2CO3, NaHCO3, NaOH, HCl, KOH, ammonium hydroxide (Fisher); Zn(OAc)2·H2O, CH3CO2Na (Fisons).
Solvents for general use were obtained from Fisher. Solvents were dried by refluxing over sodium wire (C6H6, THF, toluene) or over CaH2 (CH2Cl2). DMF was dried using a Pure Solv 400-3-MD (Innovative Technology). For TRIR experiments, CH2Cl2 (99.9%, Merck) was distilled under an inert atmosphere of Ar from calcium hydride and anhydrous THF (≥99.9%, inhibitor-free, Sigma Aldrich) was used as supplied and stored in a glove box.
CD2Cl2, CD3OD, DMSO-d6 and CDCl3 were used as obtained (Aldrich) and THF-d8 was dried over potassium. Diisopropylamine was distilled from sodium hydroxide. Methyl chloroformate was distilled prior to use. n-BuLi was titrated against n-benzylbenzamide prior to use. Routine separation of porphyrins by flash chromatography was performed on a CombiFlash Rf system using 24 g RediSep Rf silica columns (Teledyne Isco), and dry-loading the samples on silica (Fluka).
Solvents for general use were obtained from Fisher. Solvents were dried by refluxing over sodium wire (C6H6, THF, toluene) or over CaH2 (CH2Cl2). DMF was dried using a Pure Solv 400-3-MD (Innovative Technology). For TRIR experiments, CH2Cl2 (99.9%, Merck) was distilled under an inert atmosphere of Ar from calcium hydride and anhydrous THF (≥99.9%, inhibitor-free, Sigma Aldrich) was used as supplied and stored in a glove box.
CD2Cl2, CD3OD, DMSO-d6 and CDCl3 were used as obtained (Aldrich) and THF-d8 was dried over potassium. Diisopropylamine was distilled from sodium hydroxide. Methyl chloroformate was distilled prior to use. n-BuLi was titrated against n-benzylbenzamide prior to use. Routine separation of porphyrins by flash chromatography was performed on a CombiFlash Rf system using 24 g RediSep Rf silica columns (Teledyne Isco), and dry-loading the samples on silica (Fluka).
6
Fluorine-Containing Polymer Synthesis
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Benzotrifluoride, diisopropyl azodicarboxylate, maleimide, and anhydrous THF were purchased from Sigma-Aldrich and used as received. 1,1,1,2,3,3-Hexafluoro-4-(1,1,2,3,3,3-hexafluoropropoxy)pentane (PF-7600) was bought from 3 M Korea and used without further purification. 2,2-Azobisisobutyronitrile (AIBN) was obtained from Junsei Chemical and used after recrystallization from a mixed solvent of MeOH and CHCl3. 4-Cyano-4-[(dodecylsulfanylthiocarbonyl)sulfanyl]pentanoic acid (CDSTSP),48 (link) 5,5,6,6,7,7,8,8,9,9,10,10,11,11,12,12,12-heptadecafluorododecan-1-ol,49 (link) and 5,5,6,6,7,7,8,8,9,9,10,10,11,11,12,12,12-heptadecafluorododecan-1-amine50 (link) were prepared according to the literature.
7
Biobased Epoxy Matrix Crosslinking
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The GO structures were synthesized by our team through a modified
Hummers method and reported elsewhere. Methanol and acetone were purchased
from Sigma-Aldrich. Polyetheramine Jeffamine D230 was kindly provided
by Huntsman. Natural sodium montmorillonite (MMT) Nanofil 116 with
a cation exchange capacity (CEC) of 116 mequiv/100 g of clay was purchased
from Southern Clay Products. The epoxidized linseed oil (ELO) used
in this study was previously synthesized and characterized by Balanuca
et al.28 To cross-link the biobased epoxy
matrix, citric acid monohydrate (>99.5%) from Alfa Aesar was used
in the presence of anhydrous THF (≥99.9%, inhibitor-free) from
Sigma-Aldrich.
Hummers method and reported elsewhere. Methanol and acetone were purchased
from Sigma-Aldrich. Polyetheramine Jeffamine D230 was kindly provided
by Huntsman. Natural sodium montmorillonite (MMT) Nanofil 116 with
a cation exchange capacity (CEC) of 116 mequiv/100 g of clay was purchased
from Southern Clay Products. The epoxidized linseed oil (ELO) used
in this study was previously synthesized and characterized by Balanuca
et al.28 To cross-link the biobased epoxy
matrix, citric acid monohydrate (>99.5%) from Alfa Aesar was used
in the presence of anhydrous THF (≥99.9%, inhibitor-free) from
Sigma-Aldrich.
8
Synthesis and Catalytic Assessment of Nanoparticles
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All chemicals were dried in vacuum for 3 h prior to use. Metal salt precursors (PdCl2, Pd(ac)2, Sn(ac)2, and SnCl2) were purchased from Acros, Fluka, Strem, and Sigma Aldrich, respectively. 1 M KBEt3H in THF was purchased from Sigma Aldrich. Anhydrous THF was purchased from Sigma Aldrich and stored over molecular sieve (3 Å). Trioctylmethylammonium bromide was purchased from Sigma Aldrich and dried using the following procedure: (1) RT for 16–32 h, 10−3 mbar and (2) 70 °C for 0.5–1 h, 10−3 mbar. Methyltrioctylammonium bis(trifluoromethylsulfonyl)imide ([OMA][NTf2]) was obtained from IoLiTec (H2O content <100 ppm; halide content <100 ppm) and dried in vacuum prior to use (10−3 mbar, 70 °C, 3 h; 10−4 mbar, RT, 16 h). All manipulations for NP synthesis and catalytic testing were carried out using common Schlenk techniques and the anoxic glove box under argon atmosphere and anhydrous solvents.
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