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24 protocols using trimesoyl chloride

1

Fabrication of Thin-Film Membranes

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Polysulfone (PSF, average Mn ≈ 22,000), N-methyl-2-pyrrolidone (NMP,
99%), m-phenylenediamine (MPD, 99%), trimesoyl chloride (TMC, 98%),
hexane (anhydrous 95%), sodium chloride (NaCl, ACS reagent 99.0%),
and urea (ACS reagent 99.0–100.5%) were all purchased from
Sigma–Aldrich. 1-Cyclohexylpiperidine (CHP, 97%) was purchased
from Alfa Aesar. All chemicals and solvents were used as received
and without further purification. The polyester mesh (PE), 105 micrometer–52%
open area, was purchased from Elko Filtering Co. Nanopure water (18.2
MΩ·cm2) was used at all times.
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2

Polysulfone-Based Nanofiltration Membrane Fabrication

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The polysulfone used here was obtained from Sigma-Aldrich. polysulfone is included in the family of thermoplastic polymers and has the formula of (C6H4C(CH3)2C6H4OC6H4SO2C6H4O)n. The polyvinyl pyrrolidone (PVP, K-90) and N-methyl pyrrolidone, used for support preparation, were also from Sigma-Aldrich. The interfacial polymerization reactants, trimesoylchloride (TMC, ≥98.5%) and m-phenylenediamine (MPD, ≥99%), were obtained from Sigma-Aldrich (Sigma-Aldrich, St. Louis, MO, USA) and Fisher Scientific (Thermo Fisher Scientific Houston, Houston, TX, USA), respectively. MNT used in this work was nanoclay monomer® I.34 TCN from Sigma-Aldrich (Qatar, Sigma-Aldrich, St. Louis, MO, USA). The properties of nanoclay MNT are presented in Table 1. Further, the cloisite used in this study was cloisite®15A obtained from Neunano. The properties of nanoclay CS-15A are presented in Table 2. The percentage weight loss on ignition of CS-15A was 43%. A millipore deionized (DI) water system (Synergy185, Synergy185, Billerica, MA, USA, 18.2 MΩ cm) was utilized in the current work to make aqueous solutions and to soak as well as flush the membrane specimens in the course of experiments.
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3

Fabrication of PES Membranes with Additives

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Polyethersulfone (PES) membranes (Express Plus, 0.22 µm) were purchased from Millipore (Merck Millipore, Billerica, MA, USA). Piperazine (PIP), trimesoyl chloride (TMC), n-hexane, ethanol, sodium hypochlorite, hydrochloric acid, and sodium hydroxide were purchased from Sigma-Aldrich (St. Louis, MO, USA). Hydroxylated SP was bought from Tokyo Chemical Industries Company Ltd. (Tokyo, Japan). Deionized water (pH 6.8) was used in all of the experiments.
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4

Polysulfone Membrane Fabrication and Characterization

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Polysulfone base membrane B1 and B2 were supplied by SEAPS Science and Technology Co., Tangshan, China, and the specific parameters are shown in Table 1. The main difference of the above two membranes is that the BSA (bovine serum albumin) rejection of the B1 membrane is 98.67%, and that of the B2 membrane is 81%, corresponding to a low water flux (112.36 Lm−2h−1bar−1) and a high-water flux (677.52 Lm−2h−1bar−1), respectively. Polysulfone (Ultrason S 6010, Mw = 60,000 g/mol and glass transition temperature Tg = 187 °C) was supplied by BASF China (Mainland) (Shanghai, China). N-N-dimethylacetamide (DMAc ≥99.5%), and polyethylene glycol (average Mn 600) were obtained from Sinopharm (Shanghai, China). 4-formylbenzoic acid (98%), trimesoyl chloride (98%) and pyrrole (99%) were purchased from SIGMA-ALDRICH (Shanghai, China). Propionic acid, sodium hydroxide, hydrogen chloride, tetrahydrofuran, sodium bicarbonate and hexane were obtained from Sinopharm. Bovine serum albumin (BSA, pI = 4.8, Mw = 67,000 g mol−1) was obtained from Shanghai LanJi (Shanghai, China). All chemicals were used as received. Deionized (DI) water (18.2 MΩ cm) was used throughout the experiment.
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5

Polyethersulfone Membrane Fabrication

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Polyethersulfone (PES) (Veradel 3000P) was purchased from BASF Co. (Oudenaarde, Belgium). Dimethyl sulfoxide (DMSO, 99.5%) from Sigma-Aldrich (Diegem, Belgium) was used as solvent for the dope solution, and deionized water was used as the solvent and coagulant for ultrafiltration (UF) membrane fabrication. Tris(3-aminoethyl)amine (TAEA, ≥97%), piperazine (PIP, 99%), trimesoyl chloride (TMC, 98%), and n-hexane (95%) purchased from Sigma-Aldrich (Diegem, Belgium) were used to prepare PA TFC membranes. Various salts including magnesium chloride (MgCl2), magnesium sulfate (MgSO4, 99%), sodium chloride (NaCl, 99%), and sodium sulfate (Na2SO4, 99%) from Sigma-Aldrich (Diegem, Belgium) were used to test salt rejection at an inlet concentration of 1.0 g L−1. Unless specified, the aqueous solutions were prepared by deionized water purified through a Milli-Q ultrapure unit (Darmstadt, Germany).
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6

Fabrication of Polysulfone-based Membranes

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Polysulfone (PSU, MW = 35,000) and N,N-dimethylformamide (DMF, 99.8%) were obtained from Sigma-Aldrich, St. Louis, MO, USA and used in PSU support fabrication. m-Phenylenediamine (MPD, ≥99%, Sigma-Aldrich, St. Louis, MO, USA) and trimesoyl chloride (TMC, ≥98.5%, Sigma-Aldrich, St. Louis, MO, USA) were used as raw materials to synthesis the PA film. TiO2 nanoparticles (<100 nm, Sigma-Aldrich, St. Louis, MO, USA) were added as fillers into membrane surface. Humic acid (HA, Sigma-Aldrich, St. Louis, MO, USA) was used in fouling test.
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7

Polymeric Membranes for Solute Separation

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The polyimide polymer Matrimid® 5218 (Vantico Inc.), solvent N-methyl-2-pyrrolidinone (NMP, >99.5%, Merck) and non-solvent polyethylene glycol 400 (PEG 400, Mw = 400 g mol−1, Merck) were utilized to fabricate the membrane substrate. 1, 6-Hexanediamine (HDA, >98%) was purchased from Alfa-Aesar to crosslink the substrate. M-phenylenediamine (MPD, >99%), trimesoylchloride (TMC, >98%) and sodium dodecyl sulfate (SDS, >99%) were ordered from Sigma-Aldrich and employed for the interfacial polymerization reaction. LiCl (>99%, Sigma-Aldrich), CA (>99%, Sigma-Aldrich), DEA (>99%, Sigma-Aldrich), PEG 1000 (Mw = 1000 g mol−1, Merck) and methyl palmitate (>97.0%, Tokyo Chemical Industry) were utilized as the draw solutes. Ethanol (HPLC grade), isopropanol (IPA, HPLC grade), and n-hexane (HPLC grade) were ordered from Fisher Scientific and employed as the solvents to evaluate the membrane performance. Tetracycline (≥98.0 %, Sigma-Aldrich) and industrial sample, triglycerides from soybean oil (liquid, GIIAVA Singapore), were used as the model feed solutes. The commercial OSN membrane DuraMem 300 obtained from Evonik was utilized for transport mechanism studies. The deionized (DI) water was produced by a Milli-Q ultrapure water system (Millipore, USA). All chemicals were used as received.
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8

Synthesis of Silver Nanoparticles

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Example 1

Some of the main materials used in this work include: (1) Silver nitrate, (2) polysulfone (PS), (3) m-phenylenediamine (MPD), (4) trimesoyl chloride (TMC), (5) n-hexane, and (5) N,N-dimethylformamide (DMF), which were obtained from Sigma-Aldrich.

Silver nanoparticles (Ag NPs) were prepared as follows: First, 50 mL of an aqueous 0.01 M AgNO3 solution was prepared as a precursor of the Ag NPs. Second, 150 mL of an aqueous 0.02 M NaBH4 solution was prepared as a stabilizing agent by dissolving 0.1134 g in distilled water. The sodium borohydride solution was placed in an ice bath for 20 min to be cooled. Then, the AgNO3 solution was added to NaBH4 solution at rate of 1 drop/sec with continual stirring the mixture in the ice bath. After the addition of the Silver nitrate solution, the color of the mixture was turned to dark yellow indicating the formation of the nanoparticles. Finally, the solution and side products were removed by centrifuging the mixture. The resulting silver nanoparticles may further be sonicated in deionized water.

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9

Fabrication of Microporous PES Membranes

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Microporous PES (0.45 µm, Millipore Express) and n-hexane were purchased from MERCK (Darmstadt, Germany). Trimesoyl chloride (TMC), hexamethylenediamine (HMD), adipoyl chloride (ADC), piperazine (PIP), and 17β-Estradiol (E2) were obtained from Sigma Aldrich (St. Louis, MO, USA). Ethanol and toluene were purchased from VWR (Radnor, PA, USA). Deionized water in Millipore® quality was used for all steps. All materials were used as they were received from suppliers.
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10

Polyamide Thin-Film Composite Membranes

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Aluminium nitrate and ammonium hydroxide solution (NH4OH) were purchased from Merck Chemicals Co., Darmstadt, Germany. Polysulfone was purchased from Solvay advanced polymers, USA. M-phenylenediamine (99.4%), n-hexane (high purity, 97%), Polysorbates-80 (polyoxyethylene sorbitan monooleate, Tween-80), Trimesoyl chloride (98.5%), Sodium laurylsulfate (SLS, CH3(CH2)11SO4Na), Na2SO4, MgSO4, MgCl2, and NaCl were all brought from Sigma-Aldrich. All solvents used in this work were of high purity acquired from Sigma-Aldrich. Other chemicals in the present study were of analytical grade utilized as it is without any further purification.
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