Potassium persulfate, preparation

Methylene iodide [75-11-6], CH2I2, also known as diio dome thane, mol wt 267.87, 94.76% I, mp 6.0°C, and bp 181°C, is a very heavy colorless Hquid. It has a density of 3.325 g/mL at 20°C and a refractive index of 1.7538 at 4°C. It darkens in contact with air, moisture, and light. Its solubiHty in water is 1.42 g/100 g H2O at 20°C it is soluble in alcohol, chloroform, ben2ene, and ether. Methylene iodide is prepared by reaction of sodium arsenite and iodoform with sodium hydroxide reaction of iodine, sodium ethoxide, and hydroiodic acid on iodoform the oxidation of iodoacetic acid with potassium persulfate and by reaction of potassium iodide and methylene chloride (124,125). Diiodoform is used for determining the density and refractive index of minerals. It is also used as a starting material in the manufacture of x-ray contrast media and other synthetic pharmaceuticals (qv). 

Diaminoazobenzene was reported by Nietzki to have been prepared by diazotizing -nitroaniline and coupling the product with aniline. The resulting 4-nitrodiazoaminobenzene is rearranged and the nitro group reduced. The submitters tried several times to carry out this procedure but were unsuccessful. 4,4 -Diaminoazobenzene has been prepared by the oxidation of -nitroaniline with potassium persulfate followed by the reduction of the nitro groups. ... 

The oxidizing agent is prepared in a 500-ml flask equipped with a magnetic stirrer and cooled in an ice bath as follows In the flask are placed 60 ml of concentrated sulfuric acid and 20 ml of water, and the solution is cooled to 10°. Potassium persulfate (42 g, 0.15 mole) is added slowly to the stirred solution while maintaining the temperature below 10°. The solution is diluted with an additional 65 ml of water maintaining the temperature below 15°. The solution is now cooled to about 7° and 0.08 mole of the ketone is added over 40 minutes. After the addition has been completed, the solution is allowed to come to room temperature and stirring is continued for 20 hours. The solution is diluted carefully with 150 ml of water and extracted twice with 75-ml portions of ether. The ether is washed with sodium bicarbonate solution, followed by water, and the ethereal solution is dried. Removal of the solvent, followed by fractional distillation, affords the product ester. 

Radical polymerization of styrene was carried out in the presence of bare silica particles, and of the HPC-coated silica particles in water by using potassium persulfate as an initiator. Table 2 gives the typical ingredients used for these polymerizations. The HPC-coated silica particles were prepared under the same conditions as in the adsorption experiments. The polymerization temperature was kept at 1+5 °C to protect the adsorption layer of HPC, and polymerized for 2l+ hrs in the same manner as that... 

Potassium persulfate can be prepared by electrolysis of a mixture of potassium sulfate and potassium hydrogen sulfate at a high current density ... 

Silver(ll) oxide is prepared by reacting silver nitrate with potassium persulfate in the presence of a base. 

Polymer-supported persulfonic acid was prepared from potassium persulfate and the cation exchange resin P—SO3H in water. The authors reported various applications of this new oxidizing reagent such as epoxidation of olefins, Baeyer-Villiger reaction and cleavage of disulfide and Af-formylamino acids. 

The procedure for using aqueous Caro s acid as an oxidizing agent usually involves the preparation of the dilute acid from either potassium persulfate or ammonium persulfate. The following preparation illustrates the method [80],... 

Polymerization. Poly (methyl methacrylate) was obtained commercially. The polymers of other methacrylates and their copolymers were prepared in toluene with 2,2 -azobisisobutyronitrile (AIBN) at 60 °C. All the polymers prepared free radically were syndiotactic or atactic. Isotactic poly(a,a-dimethylbenzyl methacrylate) was obtained using C6H5MgBr as the initiator in toluene at 0°C. Poly(methacrylic acid) was prepared in water using potassium persulfate at as the initiator 60 °C. The molecular weights, glass transition temperatures and tacticities of the polymethacrylates are summarized in Table I. 

Finally, the ASA graft copolymer is prepared. To the alkyl acrylate rubber polymer obtained as described just above, styrene and acrylonitrile are added in the desired quantities. Dodecylmercaptan and potassium persulfate are added as chain transfer agent and radical initiator, respectively. An ASA copolymer with a mean diameter of 550 nm is obtained. 

A solution of sodium iodate, prepared from lOg of iodine according to (I), is diluted to 120ml with water and 4g of sodium hydroxide are added. Twenty-two grams of potassium persulfate are used as m (II) and then a second portion of 17g sodium hydroxide is added. The mixture is boiled for 15 minutes longer, then cooled to 40° C, and the liquid is decanted. The solid is broix it on to the filter with about 25ml of ice water, pressed dry, and then heated at 110°C for one or two hours. 

Complexes of di- and tri-methylenecyclopropanes are unknown. However, the alkali metal salts of substituted trimethylenecyclopropane dianions and their corresponding radical anions are stable. The dianions are prepared by base-induced condensation of tetra-chlorocyclopropene with three equivalents of malonic derivatives, or alternatively in two steps, via a zwitterionic aminotriafulvene (equation 368). Further oxidation with potassium persulfate gave the corresponding radical anions431. 

A 62 35 3 ethyl acrylate-methyl methacrylate-acrylic acid copolymer latex was prepared by continuous addition of the monomer mixture over a 4-hour period at 80° (22). The emulsifier was a sodium lauryl ether sulfate-nonylphenol polyoxyethylene adduct (20 moles ethylene oxide) mixture, the initiator a potassium persulfate-sodium hydroxulfite mixture, and the buffer a sodium bicarbonate-potassium hydroxide mixture. The final latex of pH 6.5 contained 40% solids, and the Tg of the copolymer was 13°. 

Vinyl acetate-butyl acrylate copolymers (0-100% butyl acrylate) were prepared by both batch and starved semi-continuous polymerization using sodium lauryl sulfate emulsifier, potassium persulfate initiator, and sodium bicarbonate buffer. This copolymer system was selected, not only because of its industrial importance, but also because of its copolymerization reactivity ratios, which predict a critical dependence of copolymer compositional distribution on the technique of polymerization. The butyl acrylate is so much more reactive than the vinyl acetate that batch polymerization of any monomer ratio would be expected to give a butyl acrylate-rich copolymer until the butyl acrylate is exhausted and polyvinyl acetate thereafter. 

Comonomer l-vinyl-2-pyrrolidone (VP) comonomer can be purified by distillation at reduced pressure prior to use. Potassium persulfate (KPS) can be purified in a mixture of water and methanol. NIPAM-co-VP copolymers with different amounts of VP can be prepared at temperatures lower or higher than the LCST of PNIPAM by free radical polymerization in water with an initiator of KPS/N,N,N/,N/-tetramethylethylenediamine (TEMED) redox. The resultant copolymer can be harvested by precipitation, i.e., pouring the reaction mixture into an equal volume of methanol. Each resultant copolymer can be further purified by several cycles of re-dissolution in water and precipitation in methanol to ensure a complete removal of residual monomers. The final product can be dried under reduced pressure at 40 °C. 

A) 2-Nitroso-5-nitrotoluene.—In a 5-1. round-bottomed flask fitted with a mechanical stirrer is placed 50 g. (0.33 mole) of pulverized 5-nitro-2-aminotoluene (Note 1). To this is added an ice-cold solution of 200 cc. of concentrated sulfuric acid in 50 cc. of water. While the suspension is stirred at room temperature, a solution of Caro s acid is prepared, as follows to 175 cc. of ice-cold sulfuric acid (sp. gr. 1.84) in a 2-1. beaker is added 300 g. (1.11 moles) of pulverized potassium persulfate. The mixture is thoroughly stirred with a glass rod, and to it is added 900 g. of crushed ice and 300 cc. of water. 

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