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CAS No. : | 557-05-1 | MDL No. : | MFCD00013031 |
Formula : | C36H70O4Zn | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | XOOUIPVCVHRTMJ-UHFFFAOYSA-L |
M.W : | 632.35 | Pubchem ID : | 11178 |
Synonyms : |
Zinc octadecanoate
|
Signal Word: | Warning | Class: | N/A |
Precautionary Statements: | P261-P305+P351+P338 | UN#: | N/A |
Hazard Statements: | H302-H315-H319-H335-H413 | Packing Group: | N/A |
GHS Pictogram: |
* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
100% | With zinc(II) oxide;citric acid; In water; at 60 - 70℃; for 0.5h; | A molten stearic acid (22.2 grams, Industrene 7018) was added gradually to a stirred slurry mixture of zinc oxide (4 grams), citric acid (0.1 gram), and water (70 grams) at 60 C. The mixture was stirred at 60-70 C. for 30 minutes to afford a product mixture with zinc stearate floating, which was filtered and dried to give a quantitative yield of zinc stearate as shown by its infrared spectrum. |
100% | With zinc(II) oxide; hydroxypropyl methylcellulose;citric acid; In water; at 65 - 75℃; for 1h; | A molten stearic acid (202 grams of Hystrene 4516) was added gradually to a stirred slurry of zinc oxide (32 grams), citric acid (0.5 gram), Methocel F50 (3 grams), and water (560 grams) at 65 C. The mixture was stirred at 65-75 C. for 1 hour to afford after filtering and drying a 100% yield of zinc stearate as indicated by its infrared spectrum. The resulting product was a white powder having free fatty acid content of 0.22% by weight. |
99.1 - 100% | With Tergitol 15-S-7; zinc(II) oxide; hydroxypropyl methylcellulose;citric acid; In water; at 55 - 70℃; for 0.25 - 1h; | A molten stearic acid (22.2 grams, Industrene 7018) was gradually added to a stirred slurry mixture of zinc oxide (4 grams), citric acid (0.1 gram), Methocel F50 (0.2 gram), Tergitol 15-S-7 (0.2 gram), and water (70 grams) at 55 C. The mixture was stirred at 60-70 C. for 30 minutes to afford a product mixture that showed the yield of zinc stearate to be about 100% by its infrared spectrum.Example 5 A molten stearic acid (23 grams, Industrene 7018) was added gradually to a stirred slurry of zinc oxide (3.9 grams), citric acid (0.08 gram), Methocel F50 (0.1 gram), Tergitol 15-S-7 (0.3 gram), and water (70 grams) at 60 C. The mixture was stirred at 65-70 C. for 15 minutes to give a reaction mixture showing the yield of zinc stearate to be about 100% by its infrared spectrum. Example 9. A molten stearic acid (29.5 grams, Hystrene 7018) was added gradually to a stirred mixture of zinc oxide (4.9 grams), citric acid (0.06 gram), Tergitol 15-S-7 (0.35 gram) and water (66 grams) at 65 C. The reaction mixture was stirred at 60-70 C. for one hour, cooled to 25 C., filtered and dried to give 32.6 grams (99.1% yield) of zinc stearate white powder that showed 0.08% water, 13.6% ash, 0.49% by weight of free fatty acid, and a melting point of 126 C. |
98.8 - 100% | With Tergitol 15-S-7; zinc(II) oxide;phosphoric acid; In water; at 55 - 73℃; for 1h; | A molten stearic acid (29.7 grams, Industrene 7018) was added gradually to a stirred slurry of zinc oxide (4.86 grams), phosphoric acid (0.13 gram, 85% solution in water), Tergitol 15-S-7 (0.8 gram), and water (65 grams) at 65 C. The mixture was stirred at 55-73 C. for one hour to give a quantitative yield of zinc stearate as shown by the infrared spectrum of the final product. Example 10. A molten stearic acid (29.5 grams, Hystrene 7018) was added gradually to a stirred mixture of zinc oxide (4.9 grams), phosphoric acid (0.1 gram), Tergitol 15-S-7 (0.2 gram), and water (66 grams) at 65 C. The reaction mixture was stirred at 60-70 C. for one hour, cooled to 25 C., filtered, and dried to afford 32.4 grams (98.8% yield) of zinc stearate white powder having 0.1% water, 14.3% ash, 0.44% by weight of free fatty acid, and a melting point of 126 C. |
50% | With Tergitol 15-S-7; zinc(II) oxide; hydroxypropyl methylcellulose; In water; at 55 - 70℃; for 1h; | A molten stearic acid (22 grams, Industrene 7018) was added gradually to a stirred slurry comprising zinc oxide (3.6 grams), Methocel F50 (0.2 gram), Tergitol 15-S-7 (0.2 gram), and water (70 grams) at 55 C. The mixture was stirred at 65-70 C. for 1 hour to produce a yield of zinc stearate of about 50% by its infrared spectrum. |
10% | With Tergitol 15-S-7; zinc(II) oxide; In water; at 55 - 75℃; for 3h; | Zinc oxide (6.6 grams), Tergitol 15-S-7 (2 grams), and water (70 grams) were placed in a beaker and heated to 55 C. with stirring to form a slurry mixture. Stearic acid (43 grams of Industrene 7018, titer=58-62 C.) was heated to about 75 C. and the resulting molten stearic acid was added gradually to the slurry mixture. The reaction mixture was stirred at 60-65 C. for three hours. A sample was drawn from the reaction mixture, dried, and analyzed by infrared spectrum to show about a 10% yield of zinc stearate. |
With zinc(II) oxide; at 124℃; under 5414.51 Torr;Neat (no solvent);Product distribution / selectivity; | Example 1 Molten stearic acid at ~170F (77C) was pumped from storage through an in-line continuous mixer. Solid zinc oxide at ambient temperature was metered continuously from a super sack into the same continuous mixer at a rate so as to achieve approximate stoichiometric ratios of the two reactants. The slurry of zinc oxide in stearic acid exiting the mixer was then continuously preheated to ~255F (124C) in a shell-and-tube heat exchanger prior to entering the high shear, continuous reactor. A temperature rise of ~30F (17C) was noted in the high shear reactor. The continuous discharge from the reactor was routed through a standard pipe to a receiver. A backpressure of 90 psig was maintained on the pipe and reactor during the reaction. The reaction mass discharged continuously from the pipe into a receiver where byproduct steam was flashed to the vent system. Total residence time required for the reaction, i.e. from the high shear reactor through the pipe to the receiver, was ?40 seconds. The combined feed rate of zinc oxide solids and stearic acid was maintained at 3,000 pounds per hour (1,361 Kg/hr) until 950 pounds (431 Kg) of ZnO and 6,515 pounds (2,892 Kg) of stearic acid were fed and the resulting zinc stearate product was collected in the receiver. The molten zinc stearate product had the following analysis: clear appearance, ash content 13.5%, free fatty acid 0.12%, water content 0.22%, and melt point of 250F (121C). The molten product was maintained under a nitrogen blanket to preserve color prior to being prilled (sprayed) to obtain the desired particle size, which in one embodiment, is about less than 100 microns. The characteristics of the zinc stearate were as shown in Table I. [Table I] ParameterPrior ArtNew processYellowness Index13.2-0.1% Transmittance34.673.3Color (Gardner Index)4.1 G< 1 G. The Prior Art product was made in a batch mode by introducing stearic acid into a 1000 gallon stainless steel reactor having four longitudinally-directed spaced-apart baffles positioned abot a periphery of the reactor which was further equipped with two vertically spaced-apart rotating impellers, each having three angled paddles, on a shaft rotating at about 88 revolutions per minute, tip speed 481 ft/min (147 m/min), the reactor having an internal working pressure of 50 psig maximum at 350 F (177 C). After adding the requisite amount of stearic acid, an equimolar amount of solid zinc oxide is added into the reactor with agitation followed by heating the reactor to about 250 F (121 C). Allow the reaction to proceed for about 30 min followed by reducing the pressure followed by a nitrogen purge and collection of zinc stearate from the reactor. | |
With carbon dioxide; ammonia; zinc(II) oxide; In water; at 65 - 100℃;pH 9.27 - 11.56; | Bubble 63 grams of ammonia gas and 29 grams of carbon dioxide gas into 386 grams of water, then add 65 grams of zinc oxide into the solution. Stir well and the zinc oxide completely dissolves into the solution. Analysis shows that the solution contains 9.56 wt. % zinc with a pH of 11.56. This solution is called solution A. 450 grams of stearic acid is added to solution A and stirred well. The stearic acid completely dissolves in the solution. Heat the solution in a laboratory reactor with agitation and a water cooled condenser to recover the evaporated ammonia and carbon dioxide. The solution boils at around 65 C. and as it is boiling, white gelatinous precipitates form. As water level drops, 1,500 ml more of water is added to the mixture. When most of the ammonia is boiled out the temperature rises to 100 C. and the pH drops to 9.27. Cool the mixture to 25 C. to precipitate other slightly soluble organic zinc salts which may be in the solution, then filter and predry the white precipitate at 90 C. for 2 hours to remove most of the water. Then further dry the precipitate at 105 C. for one hour, and mill it to obtain zinc stearate A.Using the conventional fusion method, zinc stearate B was prepared. Following are properties of both samples: Zinc Stearate A Zinc Stearate B Zinc (wt. %) 10.17 10.22 Acid Value (mg KOH/g) 18.43 96 Melting point ( C.) 112 116 pH 8.09 6.35 Bulk density (g/cm3) 0.36 0.45 Other water insoluble or sparingly soluble organic zinc salts or mixtures of organic zinc salts like zinc resinate, zinc laurate, zinc oleate, and zinc salts of coconut fatty acids can also be made according to the method described for the preparation of zinc stearate A. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
at 75℃; | [0112] Reaction of pure stearic acid with zinc oxide was conducted to investigate the reaction conditions and to verify the characterization method for the reaction. 17.9 g pure stearic acid (Sigma-Aldrich, St Louis, Mo.) was added to a 100 ml beaker and the beaker was heated in a water bath at 75 C. After the stearic acid melted, 4 g Nanox ZnO (Rheox, Hightstown, N.J.) was added to the melt and stirred with a spatula until all ZnO powder was incorporated into the liquid. Then the beaker was placed in a sonicator (NEY Ultrasonik 57X, CA), held at 75 C. and the mixture was sonicated at high power for 5 min. The beaker was taken out of the water bath and cooled down at room temperature. A fraction of the sample was taken from the solidified mixture for DSC analysis. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
In 4-methyl-2-pentanone; for 18h;Heating / reflux; | Preparation of Zinc Tetrastearyl Colorant To a 2-liter 3-necked roundbottom flask with TEFLON coated magnetic stir bar in a silicone oil bath is added 229 grams of the ring-closed purified tetrastearyl chromogen prepared as described in Example ID and 600 grams of MIBK. The mixture is heated to reflux. Thereafter, about 372 grams of <strong>[557-05-1]zinc stearate</strong> (available from Aldrich Chemical Co., Milwaukee, Wis.) is added in a stoichiometric amount of 2 moles of <strong>[557-05-1]zinc stearate</strong> per every one mole of tetrastearyl chromogen. The solution is stirred for about 18 hours. Thereafter, the MIBK is distilled off. The product is transferred to a jar and allowed to harden. It is believed that the product will be a deep magenta/red colored somewhat hard wax, believed to be a coordination compound of the formula |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
Comparative Example 1 In the same manner as in Example 1, 1552 g of zinc acrylate particles containing 0.2% by mass of an anionic surfactant and 10% by mass of zinc stearate were obtained. | ||
EXAMPLE 2 3,845 g of Zinc acrylate, including zinc stearate was obtained by following the procedure of Example 1 while using 11.0 g of sodium dioctyl sulfosuccinate, 347 g of stearic acid dissolved in 1,216 g of toluene, and 2,411 g of acrylic acid instead. | ||
EXAMPLE 3 3,712 g of Zinc acrylate, including zinc stearate was obtained by following the procedure of Example 1 while using 10.6 g of sodium dioctyl sulfosuccinate, 168 g of stearic acid dissolved in 588 g of toluene, and 2,456 g of acrylic acid instead. |
EXAMPLE 4 3,961 g of Zinc acrylate, including zinc stearate was obtained by following the procedure of Example 1 while using 546 g of palmitic acid dissolved in toluene in the place of stearic acid and using 2,345 g of acrylic acid. | ||
EXAMPLE 5 3,961 g of Zinc acrylate, including zinc stearate was obtained by following the procedure of Example 1 while using 0.6 g of sodium dioctyl sulfosuccinate. | ||
EXAMPLE 3 By following the procedure of Example 1, 1,553 g of zinc acrylate particles containing 0.2% by mass of an anionic surfactant and 10% by mass of zinc stearate was obtained. | ||
EXAMPLE 4 By following the procedure of Example 1, 1551 g of zinc acrylate particles containing 0.2% by mass of an anionic surfactant and 10% by mass of zinc stearate was obtained. | ||
COMPARATIVE EXAMPLE 1 In the same manner as in Example 1, 1552 g of zinc acrylate particles containing 0.2% by mass of an anionic surfactant and 10% by mass of zinc stearate were obtained. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
In octadec-1-ene; at 260 - 280℃;Product distribution / selectivity; | Synthesis of Mn doped ZnSe: For Mn doped ZnSe, a desire core size was chosen and a solution ofManganese decanoate and Zinc stearate in ODE was injected. The reaction EPO <DP n="19"/>temperature was carried out between 260-280oC. This helps a simultaneous precipitation of ZnSe and MnSe on ZnSe cores. Within an hour of the reaction, the emission of the sample was dominated by Mn-doping emission in addition to a small amount of ZnSe exciton emission.; Results and Discussion: 1. Shell-doped nanocrystals: Cu and Mn doped ZnSe nanocry stateSoft reactivity of copper makes it easier to insert inside the host lattice of either ZnS or ZnSe. Instantaneous reaction of copper acetate and TBPSe even at below 200oC to form black CuSe particles makes little difficult to use it as dopant in the system of the current invention. Moreover, presence of amine may lead to form complex with Cu2+ and it might prevent formation of CuSe at below 200oC.Interestingly, copper, at low concentration, can easily incorporate into ZnSe crystal lattice through reaction between 180 to 220oC. As shown in Figure Ia, the time dependent luminescence and insertion of Cu into perform ZnSe nanocrystals. Two methods for Cu doping were selected. One was fixed size of cores and insertion of Cu into their crystal lattice through annealing, and the second one was to put new layers of ZnSe on ZnSe cores to trap Cu atoms (or CuSe) inside. In former case, the exciton emission of ZnSe was not completely vanished but in later case it became flat and only the doping emission remained. As shown in Figure Ib, further growth of ZnSe on Cu:ZnSe cores. Increase of the size of ZnSe NCs red-shifts the doing emission from about 450 nm to 550 nm. This way, doping can be done at any size of the cores and once the Cu doping emission is evaluated, it can be further shelled with ZnSe or ZnS, or both. The absorbance positions remain similar to undoped ZnSe NCs. FWHM of this Cu-doped ZnSe NCs generally remains -60 to 80 nm. Photoluminescence quantum yield falls around 5 to 8% at room temperature. Further coating of ZnS layers onto the cu-doped ZnSe nanocrystals increased the PL brightness and stability. EPO <DP n="21"/>Hence a smaller analog of manganese carboxylate, manganese decanoate, was chosen along with <strong>[557-05-1]zinc stearate</strong>. To a fixed size of ZnSe cores, manganese decanoate and <strong>[557-05-1]zinc stearate</strong> were simultaneous precipitated on core ZnSe hosts. These Mn:ZnSe NCs also have some excitonic emission along with doing emission. Increase of Mn ions and size of ZnSe NCs were monitored through photoluminescence emission as former increases the intensity of doping related emission and later red-shifts the exciton emission as shown in Figure 2. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With tributylphosphine; 1-aminooctadecane; In octadec-1-ene; at 260 - 300℃; | 6 gm ODE and 0.054gm Zn(st)2 were loaded in a three necked flask, degassed and heated to 300oC. A separate solution of TBPSe (Zn:Se = 1:5 to 1:30 moles), TBP (typically 0.5ml to ImI) and ODA (Zn:ODA = ~ 8 to 10) were prepared and EPO <DP n="18"/>injected to the above reaction mixture. The growth was carried out at different temperatures (260oC to 300oC) to get the desired size. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
A method for the preparation of block zinc stearate,A, under normal pressure will be 1400g stearic acid into the reactor heated to 130-160 after the addition of catalyst hydrogen peroxide 70g and zinc oxide 220g reaction 90 minutes for the molten state; b, add antioxidant 5g stirring 5-20 minutes ; C, adding the molten zinc stearate prepared in step b to a mold in which a polyethylene mesh skeleton is placed; and d) cooling to obtain a block of zinc stearate of the desired shape. | ||
at 130 - 170℃; under 1575.16 Torr; for 0.75h; | a, the liquid state of stearic acid is transported to the reactor through the delivery pump stirring and heating, stirring time 20-28min, the heating temperature is 120-150 C, in this embodiment, the stirring time is 24min, the heating temperature is 130 C; b, the zinc oxide was added to the reaction vessel in three portions at a temperature of 160-180 C, a pressure of 0.18-0.24Mpa reaction, the reaction time is 40-50min, in this embodiment, at a temperature of 170 C, pressure 0.21Mpa reaction, the reaction time was 45min; c, the reaction is good zinc stearate tablets sent to the tabletting machine; d, the good zinc stearate tablet crushed by a common crush; e, the coarsely pulverized zinc stearate was finely pulverized by a jet mill system to obtain zinc stearate. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With sodium hydroxide; at 40℃; | General procedure: Catalyst preparation The synthesis of zinc carboxylates (Zn(CnH2n+1COO)2 with n = 11, 15 and 17) was carried out in an alcoholic solution [14]. The corresponding fatty acid and NaOH were mixed in stoichiometric amounts at 40 C with constant stirring. Then ZnCl2 was added drop-wise in stoichiometric ratio. The precipitate obtained was filtered, washed with deionized water and dried for 12 h at 50 C. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
Example - synthesis of chlor in e4-Zn complexchlorin e4-Zn complex; 0.5mmol (276mg) of chlorin e4 were dissolved in 60ml of N,N-dimethylformamide (DMF), and the solution was stirred slowly for 10 minutes at 400C. 15ml of tetrabutylammonium hydroxide (IM methanol solution) was added, and stirring was continued for a further 20 minutes, mmol (378mg) of <strong>[557-05-1]zinc stearate</strong> were dissolved in 50ml of N,lambda/-dimethylformamide (DMF), and the solution was stirred at 400C. The <strong>[557-05-1]zinc stearate</strong> solution was added to the chlorin e4 solution, and the reaction mixture was stirred slowly for 3 hours at 400C. Then the reaction mixture was filtered through a 45mum Millipore filter. The product was purified by flash <n="19"/>chromatography on a dry silica gel column using a methanol mobile phase. Then the solution was distilled and the product isolated as a dry powder by lyophilization.Chemical Formula: C33H34N4O4Zn |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
Synthesis of core doped MnJZnSe: The above synthesis of MnSe was repeated but the reaction mixture was cooled to 180oC after an hour and calculated amount of Zinc acetate solution in TBP was injected. As Se remains excess in the solution, ZnSe starts growing on preformed MnSe. The growth process was continued till it reached a desired size. Finally the temperature was again increased to 240oC for annealing. In this process, no ZnSe exciton emission along with Mn-doping emission was observed. But if the injection of Zinc acetate is carried out at above 240oC, the ZnSe exciton emission is observed because of formation of free ZnSe NCs at higher temperature. When the Mn:Se ratio was high, such as Mn:Se = 1:30, it was not necessary to wait for a hour before the growth of ZnSe shell. For this case, the growth of ZnSe shell was able to be carried out under high temperatures, as high as the boiling point of the solvent system. In atypical experiment, 0.015gm (2.42x10-5 moles) manganese stearate (MnSt2) and 13 gm ODE were loaded in a 50 ml three necked flask, degassed by purging argon and heated to 290oC. MnSt2 started dissolving nearly lOOoC and the solution turned little dark but became clear at above 250oC. A solution of 0.3 gm TBP, 0.015gm (2x10-4 moles) Se powder and 0.08 gm (2.5x10-4 moles) ODA were prepared in Glove-box and hot injected to the above reaction mixture at 290oC. The EPO <DP n="20"/>color of the resulting solution slightly turned yellowish but it intensified with the progress of the reaction. After 60 min at 280oC, the reaction mixture was cooled to 250oC and a solution of 0.008 gm (1.2 xlO-5 moles) ZnSt2 in lgm ODE was hot injected. The reaction was monitored at that temperature until the emission peak -580 nm came out. Then the temperature was reduced to 180oC and 0.022 gm (1.2x10-4 moles) zinc acetate in 2ml TBP was injected in thee phases each with 30 minutes duration. Finally the reaction temperature was increased to 240oC for at least 30 minutes for annealing.; Results and Discussion: 1. Shell-doped nanocrystals: Cu and Mn doped ZnSe nanocry stateSoft reactivity of copper makes it easier to insert inside the host lattice of either ZnS or ZnSe. Instantaneous reaction of copper acetate and TBPSe even at below 200oC to form black CuSe particles makes little difficult to use it as dopant in the system of the current invention. Moreover, presence of amine may lead to form complex with Cu2+ and it might prevent formation of CuSe at below 200oC.Interestingly, copper, at low concentration, can easily incorporate into ZnSe crystal lattice through reaction between 180 to 220oC. As shown in Figure Ia, the time dependent luminescence and insertion of Cu into perform ZnSe nanocrystals. Two methods for Cu doping were selected. One was fixed size of cores and insertion of Cu into their crystal lattice through annealing, and the second one was to put new layers of ZnSe on ZnSe cores to trap Cu atoms (or CuSe) inside. In former case, the exciton emission of ZnSe was not completely vanished but in later case it became flat and only the doping emission remained. As shown in Figure Ib, further growth of ZnSe on Cu:ZnSe cores. Increase of the size of ZnSe NCs red-shifts the doing emission from about 450 nm to 550 nm. This way, doping can be done at any size of the cores and once the Cu doping emission is evaluated, it can be further shelled with ZnSe or ZnS, or both. The absorbance positions remain similar to undoped ZnSe NCs. FWHM of this Cu-doped ZnSe NCs generally remains -60 to 80 nm. Photoluminescence quantum yield falls around 5 to 8% at room temperature. Further coating of ZnS layers onto the cu-doped ZnSe nanocrystals increased the PL brightness and stability. EPO <DP n="21"/>Hence a smaller analog of manganese carboxylate, manganese decanoate, was chosen along with <strong>[557-05-1]zinc stearate</strong>. To a fixed size of ZnSe cores, manganese decanoate and <strong>[557-05-1]zinc stearate</strong> were simultaneous precipitated on core ZnSe hosts. These Mn:ZnSe NCs also have some excitonic emission along with doing emission. Increase of Mn ions and size of ZnSe NCs were monitored through photoluminescence emission as former increases the intensity of doping related emission and later red-shifts the exciton emission as shown in Figure 2. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
Polysulfide from Undecenole: fn=2, OH no.=238 Zinc stearate: vulcanization activator Tetramethyl thiuram disulfide: vulcanization catalyst/-accelerator |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
In neat (no solvent); at 150 - 250℃;Inert atmosphere; | In this eighth example, 6.57 g zinc metal and 28.4 g stearic acid were put into a reactor. The mixture was heated with stirring in a nitrogen atmosphere. Zinc began to react with stearic acid when the temperature was above 150 C. The reaction become vigorous after the temperature increased to 250 C. Zinc stearate was obtained after the reaction was completed. | |
With dihydrogen peroxide; zinc(II) oxide; In water; at 40 - 80℃; under 0.375038 - 0.750075 Torr; for 0.833333h;Sealed tube; | By mass of zinc as a reference compound, was added to the reaction vessel 640 parts by weight of deionized water, warmed to 40 ; under stirring, to the reaction vessel 70 parts by weight of stearic acid was added and dissolved;Continue to heat to 80 deg.] C, at a stirring speed of 1000rpm conditions, the reaction vessel was added 10 parts by weight of zinc oxide and 2.3 parts by weight of hydrogen peroxide, the reaction vessel sealed, evacuated to a vacuum degree of 50-100Pa, the reaction 50min, The product is washed with hot water at 80 C, water is removed, and pulverized into a pulverizer to obtain zinc stearate. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
General procedure: All the chemicals were analytical-grade reagents and were used without further purification. In a typical synthesis, 122.6 mg <strong>[598-54-9]copper(I) acetate</strong> (Cu(Ac)), 347.7 mg Zinc stearate (ZNO) and 186.3 mg Tin(II) iodide (SnI2) were added into a 50 mL three-neck flask containing30 mL of Hexane, and then 2mL oleylamine (OLA) and 2mL oleic acid (OA) was added. The mixture was degassed under vacuum for 10 min and then purged with nitrogen for 10 min. After that, the mixture was heated to 65 C forming a transparent solution. A mixture of elemental sulfur powder (S) (4 mmol) and OLA(4 mL) separately were loaded into a 25 mL three-neck flask and heated to 130 C maintaining for 30 min to obtain a brown OLA-S solution under nitrogen atmosphere. When the solution was cooled down to 65 C naturally, it was rapidly injected into the mixture. After the injection, the mixture turned to black and formed a colloidal solution. The colloidal solution was transferred into a 50 mL Teflon-lined stainless-steel autoclave. After being sealed, the autoclave was maintained at 200 C for 24 h in a heating furnace, and then the furnace was cooled down to 60 C naturally.Then the solution was added into a mixture of toluene and isopropanol(1:1) to precipitate the product. The black precipitate CZTS nanoparticles were centrifuged several times at 7000 rpm for 5 min to ensure removal all of the excess capping agent. After then,the CZTS nanocrystals were dispersed in toluene for the further study. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
General procedure: All the chemicals were analytical-grade reagents and were used without further purification. In a typical synthesis, 122.6 mg <strong>[598-54-9]copper(I) acetate</strong> (Cu(Ac)), 347.7 mg Zinc stearate (ZNO) and 186.3 mg Tin(II) iodide (SnI2) were added into a 50 mL three-neck flask containing30 mL of Hexane, and then 2mL oleylamine (OLA) and 2mL oleic acid (OA) was added. The mixture was degassed under vacuum for 10 min and then purged with nitrogen for 10 min. After that, the mixture was heated to 65 C forming a transparent solution. A mixture of elemental sulfur powder (S) (4 mmol) and OLA(4 mL) separately were loaded into a 25 mL three-neck flask and heated to 130 C maintaining for 30 min to obtain a brown OLA-S solution under nitrogen atmosphere. When the solution was cooled down to 65 C naturally, it was rapidly injected into the mixture. After the injection, the mixture turned to black and formed a colloidal solution. The colloidal solution was transferred into a 50 mL Teflon-lined stainless-steel autoclave. After being sealed, the autoclave was maintained at 200 C for 24 h in a heating furnace, and then the furnace was cooled down to 60 C naturally.Then the solution was added into a mixture of toluene and isopropanol(1:1) to precipitate the product. The black precipitate CZTS nanoparticles were centrifuged several times at 7000 rpm for 5 min to ensure removal all of the excess capping agent. After then,the CZTS nanocrystals were dispersed in toluene for the further study. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
General procedure: All the chemicals were analytical-grade reagents and were used without further purification. In a typical synthesis, 122.6 mg <strong>[598-54-9]copper(I) acetate</strong> (Cu(Ac)), 347.7 mg Zinc stearate (ZNO) and 186.3 mg Tin(II) iodide (SnI2) were added into a 50 mL three-neck flask containing30 mL of Hexane, and then 2mL oleylamine (OLA) and 2mL oleic acid (OA) was added. The mixture was degassed under vacuum for 10 min and then purged with nitrogen for 10 min. After that, the mixture was heated to 65 C forming a transparent solution. A mixture of elemental sulfur powder (S) (4 mmol) and OLA(4 mL) separately were loaded into a 25 mL three-neck flask and heated to 130 C maintaining for 30 min to obtain a brown OLA-S solution under nitrogen atmosphere. When the solution was cooled down to 65 C naturally, it was rapidly injected into the mixture. After the injection, the mixture turned to black and formed a colloidal solution. The colloidal solution was transferred into a 50 mL Teflon-lined stainless-steel autoclave. After being sealed, the autoclave was maintained at 200 C for 24 h in a heating furnace, and then the furnace was cooled down to 60 C naturally.Then the solution was added into a mixture of toluene and isopropanol(1:1) to precipitate the product. The black precipitate CZTS nanoparticles were centrifuged several times at 7000 rpm for 5 min to ensure removal all of the excess capping agent. After then,the CZTS nanocrystals were dispersed in toluene for the further study. |
Yield | Reaction Conditions | Operation in experiment |
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General procedure: All the chemicals were analytical-grade reagents and were used without further purification. In a typical synthesis, 122.6 mg <strong>[598-54-9]copper(I) acetate</strong> (Cu(Ac)), 347.7 mg Zinc stearate (ZNO) and 186.3 mg Tin(II) iodide (SnI2) were added into a 50 mL three-neck flask containing30 mL of Hexane, and then 2mL oleylamine (OLA) and 2mL oleic acid (OA) was added. The mixture was degassed under vacuum for 10 min and then purged with nitrogen for 10 min. After that, the mixture was heated to 65 C forming a transparent solution. A mixture of elemental sulfur powder (S) (4 mmol) and OLA(4 mL) separately were loaded into a 25 mL three-neck flask and heated to 130 C maintaining for 30 min to obtain a brown OLA-S solution under nitrogen atmosphere. When the solution was cooled down to 65 C naturally, it was rapidly injected into the mixture. After the injection, the mixture turned to black and formed a colloidal solution. The colloidal solution was transferred into a 50 mL Teflon-lined stainless-steel autoclave. After being sealed, the autoclave was maintained at 200 C for 24 h in a heating furnace, and then the furnace was cooled down to 60 C naturally.Then the solution was added into a mixture of toluene and isopropanol(1:1) to precipitate the product. The black precipitate CZTS nanoparticles were centrifuged several times at 7000 rpm for 5 min to ensure removal all of the excess capping agent. After then,the CZTS nanocrystals were dispersed in toluene for the further study. |
Yield | Reaction Conditions | Operation in experiment |
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With water; In water; at 120℃; under 0.375038 Torr; for 0.5h;Sealed tube; | According to mass percentage, the 80% of stearic acid is added to the pressure in the reactor, the stirring and heating to melting temperature, the stirring speed is set as 1250rpm, for 120 C to under 15% in purity of 99.7 wt %, the average particle size is 20-100 nano zinc oxide, reaction 10 minutes later, by adding 5% pure water, the reactor sealed, evacuated to the vacuum degree is 50 Pa, to continue reaction 20 min, cooling and enters into the crushing, the resulting product is zinc stearate. |
Yield | Reaction Conditions | Operation in experiment |
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With hydrogen; at 280℃; under 18751.9 Torr; for 6h;Autoclave; | General procedure: 1.2.4. Activity tests and product analysesThe catalytic deoxygenation of oleic acid was carried out in a100 mL batch stainless autoclave furnished with a mechanical stir-rer. In a typical reaction, 0.2 g of fresh catalyst, 2.0 g of oleic acid, and 30.0 g of decalin were loaded in the autoclave. Prior to the reaction,the reactor was purged three times with H2to remove the inside air and then pressurized to 2.5 MPa at ambient temperature. The reaction system was subsequently heated to 280C and maintained at this temperature for 360 min at a stirring rate of 600 rpm. Finally,the reaction system was cooled to ambient temperature, and theliquid products were collected for subsequent analysis.The products in the gas phase were analyzed by gas chromatography mass spectrometry (GC-MS) with a TCD and a HP-PLOT/Qcolumn (30 m, 0.32 mm inner diameter, 20 m film thickness). Theliquid products were analyzed by GC-MS with a flame ionizationdetector (FID) and a HP-INNOWAX column (30 m, 0.25 mm innerdiameter, 0.25 m film thickness). N-octadecane was used as anexternal standard for the quantification of the liquid products.Besides, Fourier transform infrared spectroscopy (FT-IR) spec-tra were recorded using a Nicolet 6700 spectrometer to identifythe C(O)O group in the liquid products. Considering that zincstearate as a by-product cannot be dissolved into decalin and ana-lyzed by GC-MS, the amount of zinc stearate was obtained by agravimetric method. The generated zinc stearate can be obtainedby heating, centrifugation, washing, and drying processes. |
Yield | Reaction Conditions | Operation in experiment |
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In ethanol; at 60℃; for 4.33333h; | (1) 9.7 g of <strong>[557-05-1]zinc stearate</strong>,80.9 mL of absolute ethanol was placed in a three-necked flask.Heat and stir for 20 minutes to completely dissolve.Then 3.9g3-amino-1,2,4-triazole is dissolved in 20.0 mL of absolute ethanol.Slowly drip into a three-necked flask,Stir evenly,The reaction temperature is 60 C,The reaction time was 4 hours.After the reaction,Cool to room temperature,filter,The filter cake was washed with ethanol (200.0 mL x 3),Put in a blast oven,Produced by drying at 100 CObjectZinc distearate-bis(3-amino-1,2,4-triazole); |
Yield | Reaction Conditions | Operation in experiment |
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99% | In chloroform; at 64℃; for 3h;Inert atmosphere; | In an argon atmosphere, zinc oxide (1.0 g, 12.3 mmol), zinc acrylate (7.01 g, 33.8 mmol), <strong>[557-05-1]zinc stearate</strong> (1.94 g, 3.1 mmol) and 150 ml of chloroform were charged into a reaction vessel. The mixture was stirred at 64 C. for 3 hours. It is noted that the solvent was refluxed. The obtained reaction liquid was filtered to remove the insoluble precipitate in the solvent. 75 ml of hexane was added into the filtrate, and concentration under reduced pressure was performed until the liquid amount was reduced to about one-fourth, to obtain a precipitate. The precipitate was removed by filtration, and the filtrate was concentrated and dried to obtain a product 11 (9.9 g, yield 99%). Zinc oxide used above was available from Kishida Chemical Co. Ltd., zinc acrylate used above was available from Sigma-Aldrichi Corporation, and <strong>[557-05-1]zinc stearate</strong> used above was available from Wako Pure Chemical Industries, Ltd. |
Yield | Reaction Conditions | Operation in experiment |
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91% | In chloroform; at 64℃; for 3h;Inert atmosphere; | In an argon atmosphere, zinc oxide (1.0 g, 12.3 mmol), zinc acrylate (6.37 g, 30.7 mmol), <strong>[557-05-1]zinc stearate</strong> (3.88 g, 6.1 mmol) and 150 ml of chloroform were charged into a reaction vessel. The mixture was stirred at 64 C. for 3 hours. It is noted that the solvent was refluxed. The reaction liquid was cooled to 35 C. or below, 75 ml of hexane was added therein, and the resultant liquid was stirred for 10 minutes. The obtained reaction liquid was filtered to remove the insoluble precipitate in the solvent. The filtrate was concentrated and dried to obtain a product 13 (10.3 g, yield 91%). Zinc acrylate used above was available from Sigma-Aldrichi Corporation, and zinc oxide and <strong>[557-05-1]zinc stearate</strong> used above was available from Wako Pure Chemical Industries, Ltd. |