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40 protocols using dibutyltin dilaurate dbtdl

1

Synthesis of Polyurethane Foam

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ISB (molecular weight: 146.1 g/mol, hydroxyl value: 767.8 mg KOH/g) was obtained from Samyang Co., Ltd. (Dae-Jeon, Korea). Commercially available poly(propylene glycol) (PPG, TF-3000) with the number average molecular weight of 3000 g/mol and hydroxyl value of 56.1 mg KOH/g was obtained from SKC (Ul-San, Korea). Toluene diisocyanate (TDI-80, isomer ratio 2,4/2,6 = 8/2) was obtained from the OCI Company Ltd. (Gun-San, Korea). TDI-80 is one of popular diisocyanates in PU industries for beds and furniture. Silicone surfactant (Niax silicone L-580) was obtained from Momentive (Waterford, NY, USA). Both amine catalysts A-1 (70% bis[2-dimethylaminoethyl] ether in dipropylene glycol [DPG]) and 33-LV (33% triethylenediamine in DPG) were purchased from Aldrich (Yong-In, Korea). Dibutyltin dilaurate (DBTDL) from Aldrich was used to facilitate gelation. Distilled water was used as the blowing agent. PPG was dehydrated at 80 °C prior to use under vacuum. All chemicals were used as received.
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2

Enzymatic Cellulose Nanocrystals and Biobased Polyurethane Synthesis

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For enzymatically isolated cellulose nanocrystals with endoglucanase, denoted as EnCNC, Whatman® filter paper was used as a substrate. Cellulose nanocrystals produced by sulfuric acid treatment and purchased from Maine University in freeze dried form (0.94 wt% sulfur on sodium form) (Lot# 2014-FPL-CNC-065) were used for comparison and named as AcCNC.
For the synthesis of the biobased waterborne poly (urethane-urea) dispersion, a difunctional macrodiol derived from renewable sources, Priplast 3192® (Mw= 2000 g mol -1 ), purchased from Croda, was used as the soft segment. Isophorone diisocyanate (IPDI), kindly supplied by Covestro, 2,2-bis (hydroxymethyl) propionic acid (DMPA) as internal emulsifier and provided by Aldrich, and ethylenediamine (EDA) as chain extender and provided by Fluka, were used as hard segment. Triethylamine (TEA), supplied by Fluka, was employed to neutralize the carboxylic groups of the internal emulsifier, leading to ionic groups in the surface of the dispersed particles. Dibutyltin dilaurate (DBTDL), purchased from Aldrich, was used as a catalyst. Both the polyol and the DMPA were dried under vacuum at 60 °C for 4 hours before their use.
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3

Synthesis of PDMS-b-PPO Copolymer Membranes

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Poly(2,6-dimethyl-1,4-phenylene oxide) (PPO, 1.06 g/mL at 25 °C, “Sigma-Aldrich”, St. Petersburg, Russia) and polydimethylsiloxane (PDMS, hydroxy terminated, 0.94 g/mL at 25 °C, “Sigma-Aldrich”, St. Petersburg, Russia) were applied for synthesis of a PDMS-b-PPO copolymer, which was used as a membrane matrix. Graphene oxide (GO, “Fullerene Technologies”, St. Petersburg, Russia) [36 (link)] was used as a modifier of the PDMS-b-PPO membranes. 2,4-diisocyanatotoluene (TDI, 95 wt.%) used as a cross-linking agent and dibutyltin dilaurate (DBTDL, 95 wt.%) used as a catalyst were purchased from “Sigma-Aldrich” (St. Petersburg, Russia). Chloroform (CHCl3, 99.1 wt.%), chlorobenzene (C6H5Cl, 99.7 wt.%), methanol (MeOH, 99.5 wt.%) and ethanol (EtOH) purchased from “Vecton” (St. Petersburg, Russia) were used without additional treatment.
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4

Synthesis and Characterization of Bio-based Polyurethanes

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Polyetherol as polytertahydrofurane (PolyTHF 2000) with a molecular weight of ~ 2000 g/mol and a hydroxyl value of 56 mg KOH/g was purchased from BASF (Germany). Petrochemical aromatic diisocyanate—diphenylmethane diisocyanate (MDI) was provided by BorsodChem (Hungary). Petrochemical aliphatic diisocyanate—hexamethylene diisocyanate (HDI) with NCO content of 49.9 wt% and partially bio-based diisocyanate derived from palm oil—Tolonate™ X FLO 100 (coded FLO) with NCO content of 12.46 wt% were supplied by Vencorex Chemicals (France) [21 ]. As a chain extender bio-based 1,3-propanediol (Susterra® Propanediol, DuPont, USA) was used. Organotin catalyst—dibutyltin dilaurate (DBTDL) was provided by Sigma-Aldrich (Poland).
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5

Jatropha Oil Polyurethane Synthesis

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Reagent grade hydrogen peroxide 30% and methanol were supplied by Merck (Darmstadt, Germany). Isophrene diisocyanate (IPDI), dimethylol propionic acid (DMPA), n-methyl pyrollidone (NMP), hydroxyethyl methacrylate (HEMA), phtalic anhydride, and dibutyltin dilaurate (DBTDL) were supplied by Sigma Aldrich (Milwaukee, WI, USA). Ethyl methyl ketone (MEK), triethylamine (TEA), formic acid, magnesium sulphate anhydrous, pyridine, and sodium hydroxide were reagent grade, supplied by Classic Chemicals (Shah Alam, Malaysia). The crude jatropha oil was supplied by Biofuel Bionas Sdn Bhd, Kuala Lumpur, Malaysia. It is a non-food grade material and was used as received. All chemicals were used without further purification.
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6

Synthesis and Characterization of Polypropylene Glycol Biomaterials

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Polypropylene glycol (PPG,
M.W. 2000 kDa), hexamethylene diisocyanate (HDI), triethylene glycol
(TEG), glycerol, CA, trans PCA, FA, chloroform, dimethylformamide
(DMF), phosphate-buffered saline (PBS), Dulbecco’s modified
Eagle’s medium (DMEM), penicillin–streptomycin (P/S),
fetal bovine serum (FBS), and crystal violet (CV) were purchased from
Fisher Scientific (Waltham, Massachusetts, USA) and used as received.
Ethyl-3-(3-(dimethylamino)propyl)carbodiimide (EDC), 4-(N,N-dimethylamino)pyridine (DMAP), and dibutyltin
dilaurate (DBTDL) were purchased from Sigma-Aldrich (St. Louis, Missouri,
USA). Escherichia coli (E. coli, 397E strain), Staphylococcus
aureus
(S. aureus,
Wichita strain), and Swiss mouse 3T3 fibroblasts were purchased from
ATCC (Manassas, Virginia, USA), and glutaraldehyde was purchased from
Electron Microscopy Sciences (Hatfield, Pennsylvania, USA). PPG, TEG,
EDC, DMAP, CA, PCA, FA, and glycerol were all dehydrated under a vacuum
overnight to remove trace moisture before use. All solvents were dried
over sieves before use.
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7

Synthesis and Characterization of WBPUU Inks

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WBPUU inks were synthesized with a soft segment (SS) composed by two di-functional polyols, polycaprolactone (PCL) (CAS: 24980-41-4) and poly (ethylene glycol) (PEG) (CAS: 25322-68-3) (Mn = 2000 and 1000 g mol−1, respectively), both provided by Sigma-Aldrich. On the contrary, 2,2-bis(hydroxymethyl) propionic acid (DMPA, 98% purity, CAS: 4767-03-7) and ethylene diamine (EDA, 99% purity, CAS: 107-15-3), which were used as an internal emulsifier and a chain extender, respectively, also provided by Sigma-Aldrich, and isophorone diisocyanate (IPDI, 99.5% purity, CAS: 4098-71-9), supplied from Covestro, were used as components of the hard segment (HS). Dibutyltin dilaurate (DBTDL, CAS: 77-58-7), provided by Sigma-Aldrich, was used as a catalyst. The polyols and the DMPA were dried under a vacuum at 60 °C for 4 h prior to their use. Butanone (supplied by Panreac, CAS: 78-93-3) was used to adjust the viscosity of the prepolymer in an intermediate state as well as to transfer the neutralized DMPA into the reaction medium. The neutralization of the carboxylic groups of DMPA has been carried out by using triethylamine (TEA, 99.5% purity, CAS: 121-44-8), provided by Fluka. Cellulose nanocrystals (CNC) provided by the University of Maine (2018-FPL-CNC-117) were used and CaCl2 solution (0.1 M, CAS: 10043-52-4) was provided by Sigma-Aldrich.
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8

Polyurethane Shaping Protocol

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All chemicals used in this study were purchased from Macklin with AR grade or higher (unless otherwise specified) and used as received. Dibutyltin dilaurate (DBTDL, 95%) was purchased from Sigma-Aldrich. Tetrahydrofuran (THF, 99.9%, superdry) and N,N-dimethylformamide (DMF, 99.9%, superdry) were purchased from J&K Scientific Ltd. Teflon molds of various shapes and depths were manufactured in-house to shape polyurethane.
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9

Synthesis of Silica-Based Polymer Composites

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Before the experimental procedures, all glassware utilized in the synthesis was thoroughly washed with ethanol, rinsed with distilled water, and dried with absorbent paper to eliminate potential impurities. The used reagents for the experimental procedures were dimethyl ketone (C3H6O) (99.5%, Meyer®, Mexico City, Mexico); hydroxy-terminated polydimethylsiloxane (PDMS-OH) (2550–3570 cSt, Sigma Aldrich®, Milwaukee, WI, USA); tetraethylorthosilicate (TEOS) (98% Sigma Aldrich®, Wuxi, China); ammonium hydroxide (NH4OH) (28% J.T.Baker®, Madrid, Spain); nitric acid (HNO3) (65–70% J.T.Baker®, Madrid, Spain); and dibutyltin dilaurate (DBTDL) (95% Sigma Aldrich®, Milwaukee, WI, USA).
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10

Polymer-Hydroxyapatite Composite Preparation

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Commercially available POM copolymer (Ultraform®, BASF, Ludwigshafen, Germany) with melt flow rate (MFR (190/2.16, ISO 1133) 2.6 g/10 min has been used for composite preparation. The average molar mass was determined using the GPC method according to ASTM D5296-05 at a temperature 40 °C with the VE2001 Viscotek GPC system equipped with the RI-VE 3580 Viscotek detector (PL HFIPgel, 605 E901506 and HFIP 603 E910606 columns). Average molar mass has been determined based on the polystyrene standard as: Mn = 8 269, Mw = 78 565 and dispersity Mw/Mn = 8.96. Stoichiometric spherical-shaped hydroxyapatite (HAp) with general chemical formula C10(PO4)6(OH)2 was supplied from nGimat Co. (Atlanta, USA). The diameter of 99% HAp particles was below 100 nm. 1,6-heksamethylenodiisocyanate (HDI), poly(ε-caprolactone) diol (PCL) with average molar mass of 2000 g/mol and dibutyltin dilaurate (DBTDL) were supplied from Sigma Aldrich and used as received. Anhydrous N,N-dimethylformamide (DMF) and ethanol were produced by Avantor (Gliwice, Poland).
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