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8 protocols using li2co3

1

Electrochemical Analysis of Graphene

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KMnO4, 2-propanol, ethanol, acetone, nitric acid, ethylene carbonate (EC), and dimethyl carbonate (DMC) were purchased from Kanto Chemical. Tetrabutylammonium bromide (TBABr) was purchased from TCI. LiCl, MnCO3•nH2O, Li2CO3, and naphthalene were acquired from Wako. Graphene was obtained from Graphene Laboratories, Inc. The 1 M LiPF6 solution in 1:1 EC/DMC (v/v) was acquired from Kishida. Solvents and substrates for thiol homocoupling, sulfide oxidation, alkylarene oxidation, and oxidative amidation were purchased from Kanto, TCI, Wako, and Aldrich. All reagents were used as received without purification.
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2

Synthesis of Li-based Oxides with Transition Metals

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Li3NbO4 was prepared by solid-state reaction from stoichiometric amounts of Li2CO3 (> 98.5%; Kanto Kagaku) and Nb2O5 (99.9%; Wako Pure Chemical Industries) at 950 °C for 24 h in air. Li1.3Nb0.3Me0.4O2 (Me=Fe3+, Mn3+ and V3+) samples were prepared from Li2CO3, Nb2O5 and precursors containing each transition metal: Mn2O3, Fe2O3 (99.9%; Wako Pure Chemical Industries), V2O3 (98%; Sigma-Aldrich Japan). Mn2O3 was obtained by heating of MnCO3 (Kishida Chemical) at 700 °C for 12 h. The precursors were thoroughly mixed by wet mechanical ball milling and then dried in air. Thus obtained mixtures of the samples were pressed into pellets. The pellets were heated at 900 °C for 12 h in air (Fe3+) or inert atmosphere (Mn3+ and V3+). The samples were stored in an Ar-filled glove box until use.
Li1.2Ti0.4Mn0.4O2 was prepared from Li2CO3, TiO2 (Anatase, 98.5%; Wako Pure Chemical Industries), and Mn2O3. The precursors were thoroughly mixed by wet mechanical ball milling and the mixture was heated at 900 °C for 12 h in inert atmosphere. Particle morphology of the samples was observed using a scanning electron microscope (JCM-6000, JEOL) with acceleration voltage of 15 keV.
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3

Synthesis and Photocatalytic Treatment

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K4Nb6O17,15 KLaNb2O7,16 RbCa2Ta3O10,17 LiTaO3,18 NaTaO318 and KTaO318 were prepared by a solid-state reaction, as previously reported. The starting materials used were as follows: Li2CO3 (Wako Pure Chemical; 99.0%), Na2CO3 (Kanto Chemical; 99.0%), K2CO3 (Kanto Chemical; 99.5%), Rb2CO3 (Kojundo Chemical; 99%), CaCO3 (Kanto Chemical; 99.5%), La2O3 (Kanto Chemical; 99.99%), Nb2O5 (Kojundo Chemical; 99.95%) and Ta2O5 (Rare Metallic; 99.99%). K2La2Ti3O1019 was prepared using a polymerized complex method. The precursor was obtained from K2CO3 (Kanto Chemical; 99.5%), Ti(OC4H9)4 (Kanto Chemical; 97%), La(NO3)3 (Kanto Chemical; 99.99%), ethylene glycol (Kanto Chemical; 99.5%) and citric acid (Sigma Aldrich; 99.5%) by pyrolysis and was calcined at 1173 K for 2 h in air using an alumina crucible. CuCl was freshly prepared by reduction of CuCl2 (Wako Pure Chemical; 99.0%) with metallic Cu in boiling dilute hydrochloric acid. The molten CuCl treatment was carried out by immersing the prepared photocatalysts in molten CuCl at 773 K for 10 h in a quartz ampoule tube under vacuum. After the molten salt treatment, the excess CuCl was removed using an aqueous NH3 solution.
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4

Synthesis and Characterization of Li-Doped Ca(OH)2

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LiOH·H2O (Wako Pure
Chemical Industries, Ltd.), LiCl·H2O (99.9%, Wako
Pure Chemical Industries, Ltd.), Li2CO3 (Wako
Pure Chemical Industries, Ltd.), and Ca(OH)2 (99.9%, FUJIFILM
Wako Pure Chemical Corporation) were used to prepare
Ca(OH)2 with Li compounds being added. LiOH/Ca(OH)2, LiCl/Ca(OH)2, Li2CO3/Ca(OH)2, LiOH/LiCl/Ca(OH)2, LiCl/Li2CO3/Ca(OH)2, and LiCl/Li2CO3/Ca(OH)2 were prepared by the impregnation method.14 (link)−18 (link),32 (link),33 (link) First, an aqueous solution of Li compounds was prepared from LiOH
and/or LiCl and/or Li2CO3 and ultrapure water.
The solution was impregnated with pure Ca(OH)2 powder and
stirred for 30 min. After this, water was evaporated at 40 °C
using a rotary evaporator. Finally, the samples were dried overnight
at 120 °C. All the samples were obtained as a white powder. For
comparison, Ca(OH)2 and Mg(OH)2 without Li compound
addition were also prepared in the same way. Ca(OH)2 and
Mg(OH)2 without added Li compounds are expressed as Ca(OH)2-w and Mg(OH)2-w, respectively. Table 6 shows the prepared samples
and the ratio of the additive.
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5

Synthesis of Li2RuO3 and Li2Ru1-xSxO3+x

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The Li2RuO3 crystal was synthesized from Li2CO3 (>99%; Wako Pure Chemical) and RuO2 (99.9%; Sigma-Aldrich) by a typical solid-state reaction (10 ). A mixture of Li2CO3 (10% excess) and RuO2 was put into Al2O3 crucible and then preheated at 900°C for 12 hours. The preheated sample was well ground by using an agate mortar and a pestle. The obtained powder was heated at 1150°C for 24 hours to obtain a well-crystallized Li2RuO3 sample. The Li2SO4 crystal was obtained by heat treatment of Li2SO4·H2O (99.9%; Wako Pure Chemical) at 300°C for 3 hours in dry Ar atmosphere. The Li2Ru1−xSxO3+x (x = 0, 0.1, 0.2, 0.3, 0.4, and 0.5) positive electrode active materials were synthesized by mechanical milling using a planetary ball-milling apparatus (Pulverisette 7; Fritsch). A mixture of Li2RuO3 and Li2SO4 crystals was used as a precursor for milling. The mixture was put into a 45-ml zirconia pot with 160 balls (5 mm in diameter) and milled at a rotating speed of 370 rpm with a milling time of 50 hours. All processes were conducted in dry Ar atmosphere.
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6

Preparation of LAGP Solid Electrolyte

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LAGP powder for the air electrode and LAGP pellet for the electrolyte layer were prepared using methods reported elsewhere18 . LAGP was synthesized by the conventional solid-state reaction. Reagent-grade chemicals of Li2CO3 (Wako Pure Chemical Industries, Ltd., 99%), Al2O3 (Kojundo Chemical lab. Co., Ltd, 99.999%), GeO2 (Kojundo Chemical lab. Co., Ltd, 99.995%) and (NH4)H2PO4 (Wako Pure Chemical Industries, Ltd., 99%) were used as starting materials. The mixture of starting materials was milled at 250 rpm for 4 hours by using a planetary ball mill (Pulverisette 5, Fritsch). The milling process was repeated after heat treatment of 600 °C and 900 °C. The milled precursors were heated at 600 °C for 1 h and 900 °C for 6 h in the oxygen atmosphere. The obtained LAGP powder was used for the air electrode. LAGP pellet for the solid electrolyte layer was prepared from LAGP powder. LAGP powder was pressed into pellets and sintered at 900 °C for 6 h in the oxygen atmosphere. The thickness of the obtained LAGP pellets was about 1 mm. The lithium ion conductivity is about 2 × 10−4 S cm−1.
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7

Spent Autocatalyst Characterization and Recycling

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A spent autocatalyst (NIST, Standard Reference Materials 2557 Used Auto Catalyst (Monolith)), Li2CO3 (FUJIFILM Wako Pure Chemical Corporation, Osaka, Japan, Wako Special Grade 122–01132), LiF (FUJIFILM Wako Pure Chemical Corporation, Osaka, Japan, Wako Special Grade 127–01785), and synthetic cordierite (2MgO·2Al2O3·5SiO2, Marusu Glaze Co., Ltd., Aichi, Japan, SS-200, mean particle size of 7.5 µm) were used. The spent autocatalyst comprised monolith catalysts collected from vehicles in the 1990s, which were then crushed and sieved through a 200 mesh (<75 µm). Table 1 lists the concentrations of the various elements detected in the spent autocatalyst sample [29 ].
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8

Synthesis and Characterization of LBO Powder

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The LBO powder was synthesized by
heating mixtures of Li2CO3 (99.0%, FUJIFILM
Wako Pure Chemical Corporation, Japan) and B2O3 (95%, Kanto Chemical Co., Inc., Japan) in a molar ratio of 3:1 at
600 °C for 10 h in air. The LBO powder was further pulverized
(to reduce the average particle size to less than 1 μm) by ball
milling (400 rpm, 10 min milling followed by a 20 min pause to avoid
overheating, repeated for 99 times). Figure S2 shows the XRD pattern of the synthesized LBO powder.
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