autoclave, by Parr - Product details

1

Crystallization of EMM-17 in Parr Autoclave

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Example 2

The free-flowing powder of the freeze dried synthesis mixture was crystallized in a standard Parr Autoclave, the fill level being slightly above the bottom blade using a stacked agitation system. The stacked agitator is shown in the inset of FIG. 2A. The gel was agitated slowly at 320° F. (160° C.) for 10 days. This method produced EMM-17 crystals with a mixed morphology and amorphous material, as shown in the SEMs in FIGS. 2A and 2B.

Example 3

The free-flowing powder of the freeze dried synthesis mixture was crystallized in a standard Parr Autoclave, the fill level being slightly above the bottom blade using a spiral agitation system. The spiral agitator is shown in the inset of FIG. 3A. The gel was agitated slowly at 320° F. (160° C.) for 10 days. This method produced EMM-17 crystals with a more uniform morphology than Example 2 in addition to amorphous material, as shown in the SEMs in FIGS. 3A and 3B. The EMM-17 crystals were large, plate-like crystals ˜3 μm×0.5 μm (particle size ˜3 μm).

US10696560B2. Small crystal EMM-17, its method of making and use (2020-06-30). ExxonMobil Research and Engineering Company [US]. Inventors: Ivy D. Johnson [US], Nadya A. Hrycenko [US], Theodore E. Datz [US], William W. Lonergan [US], Karl G. Strohmaier [US], Hilda B. Vroman [US], Keith C. Gallow [US], Simon C. Weston [US].

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2

Formation of Hydroxymethanesulfonic Acid

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Example 4

At room temperature into a 600 ml Parr Autoclave fitted with in situ IR optics was loaded a solution of 7.29 grams trioxane and 250 ml of water. The reactor was sealed and 15.5 grams of SO₂was added via blow case injector. The solution was heated to 50° C. and no change was observed in the infrared spectra with IR bands of all major components remaining unchanged. The solution was then heated to 80° C., again no change was observed. The solution was then heated to 100° C. without any observed change. The solution was then heated to 130° C. and the formation of hydroxyl methane sulfonic acid was observed. A plot of the IR optic data showing the concentration of the SO₂, trioxane, and generated hydroxymethanesulfonic acid are shown in FIG. 4.

US11156074B2. Thermally activated strong acids (2021-10-26). SHELL OIL COMPANY [US]. Inventors: Paul Richard Weider [US], Robert Lawrence Blackbourn [US], Ying Zhang [US], Lee Nicky Morgenthaler [US], Ryan Matthew Van Zanten [US].

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3

Trioxane Sulfonation Reaction Kinetics

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Example 4

At room temperature into a 600 ml Parr Autoclave fitted with in situ IR optics was loaded a solution of 7.29 grams trioxane and 250 ml of water. The reactor was sealed and 15.5 grams of SO₂was added via blow case injector. The solution was heated to 50° C. and no change was observed in the infrared spectra with IR bands of all major components remaining unchanged. The solution was then heated to 80° C., again no change was observed. The solution was then heated to 100° C. without any observed change. The solution was then heated to 130° C. and the formation of hydroxyl methane sulfonic acid was observed. A plot of the IR optic data showing the concentration of the SO₂, trioxane, and generated hydroxymethanesulfonic acid are shown in FIG. 4.

US11603491B2. Thermally activated strong acids (2023-03-14). SHELL OIL COMPANY [US]. Inventors: Paul Richard Weider [US], Robert Lawrence Blackbourn [US], Ying Zhang [US], Lee Nicky Morgenthaler [US], Ryan Matthew Van Zanten [US].

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4

Formation of Hydroxymethanesulfonic Acid

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Example 4

At room temperature into a 600 ml Parr Autoclave fitted with in situ IR optics was loaded a solution of 7.29 grams trioxane and 250 ml of water. The reactor was sealed and 15.5 grams of SO₂was added via blow case injector. The solution was heated to 50° C. and no change was observed in the infrared spectra with IR bands of all major components remaining unchanged. The solution was then heated to 80° C., again no change was observed. The solution was then heated to 100° C. without any observed change. The solution was then heated to 130° C. and the formation of hydroxyl methane sulfonic acid was observed. A plot of the IR optic data showing the concentration of the SO₂, trioxane, and generated hydroxymethanesulfonic acid are shown in FIG. 4.

US10443368B2. Thermally activated strong acids (2019-10-15). SHELL OIL COMPANY [US]. Inventors: Paul Richard Weider [US], Robert Lawrence Blackbourn [US], Ying Zhang [US], Lee Nicky Morgenthaler [US], Ryan Matthew Van Zanten [US].

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5

Synthesis and Reduction of Graphene Oxide Foams

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In a first step, GO was synthesized according to a modified Hummers method starting from graphite powder^{59 (link)}. In a typical synthesis, the graphite was oxidized by concentrated sulfuric acid and potassium permanganate. Deionized water was slowly added, followed by hydrogen peroxide. GO was then washed with deionized water and subsequently centrifuged several times until a concentrated solution with a neutral pH was obtained. GO foams were synthesized by hydrothermal synthesis; where aqueous solutions of GO (1.5 mg mL⁻¹) were introduced in an autoclave (Parr instrument company) and heated at 180 °C for 12 h. The as-formed wet gels were then fully frozen and consequently freeze-dried (Labonco Freezone 4.5; 0.05 mBar) yielding 3D GO foams. The reduction of the GO into reduced graphene oxide (rGO) foams was carried out by thermal treatment at 900 °C for 2 h under reducing atmosphere (Varigon, 5%H₂/Ar) in a Vecstar tubular furnace.

Hanniet Q., Boussmen M., Barés J., Huon V., Iatsunskyi I., Coy E., Bechelany M., Gervais C., Voiry D., Miele P, & Salameh C. (2020). Investigation of polymer-derived Si–(B)–C–N ceramic/reduced graphene oxide composite systems as active catalysts towards the hydrogen evolution reaction. Scientific Reports, 10, 22003.

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6

Hydrocarbon Conversion Catalysis Protocol

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n-Hexadecane (1.59 g, 7.0 mmol; 112 mmol based on carbon) and the catalyst (0.10 g) were added to a glass vial (20 mL) with a glass magnetic stir bar, and the vial was then placed into an autoclave (75 mL, Parr Instrument). The autoclave was purged three times with H₂ and then pressurized to 45 bar and sealed. The pressurized autoclave was placed in a heating block at the desired temperature (275–375 °C) and stirred (350 rpm) for the given reaction time (2–6 h). After the reaction, the autoclave was cooled to room temperature in a water bath. The gaseous products were transferred into a gas-sampling bag (1 L) and injected into a specialized gas-sampling gas chromatography-flame ionization detector (GC-FID) for analysis. For GC-mass spectrometry (GC-MS) analysis of the liquid products, n-dodecane (0.085 g, 0.5 mmol) was added to the vial as an internal standard and diethyl ether was used as the solvent if the resulting liquid was insufficient for GC sample preparation. In certain cases, dichloromethane was used to wash (8 mL × 3) the catalyst, and the catalyst was then vacuum dried overnight before conducting the thermogravimetric analysis (TGA).

Lee W.T., van Muyden A., Bobbink F.D., Mensi M.D., Carullo J.R, & Dyson P.J. (2022). Mechanistic classification and benchmarking of polyolefin depolymerization over silica-alumina-based catalysts. Nature Communications, 13, 4850.

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7

Hydrogenation of Polyethylene using Autoclaved Reactor

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PE (1.59 g, Mw ~4000, Sigma-Aldrich; ~112 mmol of carbon) and the catalyst (0.20 g) were added to a glass vial (20 mL) with a glass-coated magnetic stir bar, and the vial was then placed into an autoclave (75 mL, Parr Instrument). The autoclave was purged three times with H₂ and then pressurized to 45 bar and sealed. The pressurized autoclave was placed in a heating block at the desired temperature (275–375 °C) and stirred (500 rpm) for the given reaction time (2–16 h). After the reaction, the autoclave was cooled to room temperature in a water bath. The gaseous products were transferred into a gas-sampling bag (1 L) and injected into a specialized gas-sampling gas chromatography-flame ionization detector (GC-FID) for analysis. For GC-mass spectrometry (GC-MS) analysis of the liquid products, n-dodecane (0.085 g, 0.5 mmol) was added to the vial as an internal standard and diethyl ether was used as the solvent if the resulting liquid was insufficient (<0.5 mL) for GC sample preparation.

Lee W.T., van Muyden A., Bobbink F.D., Mensi M.D., Carullo J.R, & Dyson P.J. (2022). Mechanistic classification and benchmarking of polyolefin depolymerization over silica-alumina-based catalysts. Nature Communications, 13, 4850.

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8

Accelerated Thermal Aging Protocol

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Physic-mechanical investigation was repeated after thermal aging. Accelerated ageing tests were conducted in autoclave (Parr Instrument Company, Moline, IL, USA) according to the EN ISO 2440 standard. At first, samples were conditioned at a temperature of 23 ± 2 °C and a humidity equal to 50 ± 5% for 24 h. After the conditioning process, samples were placed in an autoclave where the temperature was set up to 120 °C, the humidity was 100%, and the pressure was 0.3 MPa. The ageing process lasted for 144 h.

Bazan P., Mierzwiński D., Bogucki R, & Kuciel S. (2020). Bio-Based Polyethylene Composites with Natural Fiber: Mechanical, Thermal, and Ageing Properties. Materials, 13(11), 2595.

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9

Lignin Hydrogenolysis over Ru@NC

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Typically, CEL (50 mg) or lignin model compounds (15 mg), Ru@NC (5 mg), and MeOH (10 mL) were charged into an autoclave (50 mL, Parr Instrument Company, Moline, IL, USA), which was then flushed with N₂ for three times and pressurized with 3 MPa H₂ at room temperature. Afterwards, the mixture was stirred at 800 rpm and heated to the desired temperature. After the reaction, the autoclave was cooled and depressurized carefully. The reaction mixture was filtered through a nylon 66 membrane filter (0.22 μm), and the insoluble fraction was washed with DCM. Lignin oily product was obtained after removing DCM under a vacuum condition. An external standard (1,3,5-trimethoxybenzene) was added to the lignin oily solution in DCM.

Xiao L.P., Lv Y.H., Yang Y.Q., Zou S.L., Shi Z.J, & Sun R.C. (2023). Unraveling the Lignin Structural Variation in Different Bamboo Species. International Journal of Molecular Sciences, 24(12), 10304.

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10

Polystyrene-Reinforced Resorcinol-Formaldehyde Aerogels

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We used monodisperse polystyrene (PS) spheres with a diameter of 210 ± 6 nm, as determined by image analysis of scanning electron micrographs (the corresponding average particle diameter was 244 nm determined by dynamic light scattering). The PS spheres were prepared by emulsion polymerization of styrene using potassium persulfate (KPS) as the initiator and polyvinylpyrrolidone (PVP) as the stabilizer, as previously reported.^{23 (link)} A mass of 0.1 g of PS spheres was added to a resorcinol formaldehyde (RF) sol which was prepared according to ref. 15 (link). For comparison, pristine RF samples were also prepared without PS addition. The sol–gel reaction of resorcinol with formaldehyde was catalyzed by sodium carbonate (Na₂CO₃; R/C = 50), and we adjusted the pH value to 5.45 by adding diluted nitric acid (HNO₃) for condensation. We obtained cylindrical monolithic RF aerogels samples after gelation and aging at 80 °C for seven days. The RF aerogels were immersed in an acetone bath (50 mL) and the liquid was exchanged and replenished three times in three days. Wet RF aerogels were dried with supercritical CO₂ in an autoclave by Parr Instruments with a volume of 300 mL at 9 MPa and 55 °C. Subsequently, the RF samples were carbonized in a tube furnace at 800 °C under argon gas.

Salihovic M., Hüsing N., Bernardi J., Presser V, & Elsaesser M.S. (2018). Carbon aerogels with improved flexibility by sphere templating. RSC Advances, 8(48), 27326-27331.

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Autoclave

Lab products found in correlation

13 protocols using autoclave

Crystallization of EMM-17 in Parr Autoclave

Formation of Hydroxymethanesulfonic Acid

Trioxane Sulfonation Reaction Kinetics

Formation of Hydroxymethanesulfonic Acid

Synthesis and Reduction of Graphene Oxide Foams

Hydrocarbon Conversion Catalysis Protocol

Hydrogenation of Polyethylene using Autoclaved Reactor

Accelerated Thermal Aging Protocol

Lignin Hydrogenolysis over Ru@NC

Polystyrene-Reinforced Resorcinol-Formaldehyde Aerogels

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