二叔丁基过氧化物

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反应条件: temp:60.01; pressure:0.00; stir:

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Hydrogen peroxide is reacted with tertiary butyl alcohol in accordance with the invention to form DTBP. About 4.5 grams of 30% aqueous hydrogen peroxide are combined with 0.5 grams of 12-tungstophosphoric acid catalyst (H3PW12O40) and 5.92 grams of tertiary butyl alcohol, and the mixture is heated to 80° C. under a nitrogen blanket. After 4 hours reaction time, 3.50 grams of an organic layer was separated. Analysis of the organic layer showed 20 wt% tertiary butyl alcohol, 34 wt% tertiary butyl hydroperoxide, 35 wt% ditertiary butyl peroxide, 4 wt% acetone and 2.4 wt% methanol.

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Into a four-necked flask equipped with a stirrer, reflux condenser, thermometer and gas-inlet tube were introduced 600 parts of ethyl acetate which was heated and kept at 75° to 78° C. under a stream of nitrogen gas. A monomer mixture composed of 249 parts of monobutyl maleate, 151 parts of styrene and 4 parts of di-tert-butyl peroxide as a polymerization initiator was added dropwise into the flask taking about 2 hours to form a polymerization mixture which was agitated for further 2 hours at the same temperature to effect copolymerization of the monomers. After completion of the polymerization reaction, the polymerization mixture was freed from the solvent by stripping under reduced pressure to give a solid copolymeric resin of maleic acid and styrene. Into a four-necked flask equipped with a stirrer reflux condenser was heated kept at 75° to 78° C. under a stream of nitrogen gas was added dropwise into the flask to form a polymerization mixture which copolymerization of the monomers After completion of the polymerization reaction

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: The anhydride-functional polymers which are useful in the practice of this invention will have an average of at least two anhydride groups per molecule and are prepared by polymerizing a monomer mixture comprising the alkenyl succinic anhydride and at least one (meth)acrylic monomer under free radical addition polymerization conditions. Polymerizing under free radical addition polymerization conditions means that the monomers are reacted in the presence of a free radical source at a temperature sufficient for polymerization. Optionally, other copolymerizable monomers, such as vinyl compounds, can be included in the polymerization reaction. The monomers which are copolymerized with the alkenyl succinic anhydride should, of course, be free of any functionality which could react with the anhydride group during the polymerization. The anhydride-functional polymers can be conveniently prepared by free radical addition polymerization techniques, however, the effective incorporation of the alkenyl succinic anhydride monomers requires special considerations which are not typically involved in (meth)acrylic free radical polymerization. For example, it is preferred to conduct the polymerization at relatively high temperatures, normally in excess of 110° C., and preferably at temperatures ranging from 135° C. to about 170° C. Additionally, relatively higher amounts of initiator are generally preferred than the levels normally used for conventional free radical polymerization of (meth)acrylic monomers and initiator concentrations will typically be within a range of 0.2 to 15, and preferably 2 to 8 weight percent of the total monomer charge. Peroxide initiators, and especially those having a relatively long half-life, e.g. greater than about 15 minutes, at these reaction temperatures are generally preferred over the azo type initiators. Di-tertiary butyl peroxide, di-(tertiary-butyl peroxyisopropyl)benzene and, especially, di-tertiary-amyl peroxide are particularly useful initiators. Additionally, aromatic hydrocarbons are generally preferred as the inert solvent rather than oxygenated inert solvents when minimal color development during the polymerization if preferred. Exxate 600 (trade name for oxohexylacetate from Exxon Chemical Company) and xylene are representative useful solvents for the polymerization. Furthermore, monomers having acrylic, rather than methacrylic, unsaturation, or monomers having allylic hydrogen atoms, such as isobornyl methacrylate, generally provide higher degrees of incorporation of the alkenyl succinic anhydride into the polymer and it is especially preferred that the monomer mixture comprise at least one such monomer. Preferrably, at least 5% by weight of the monomer mixture will be monomers having such functionality. Although it is not our intent to be bound by theory, experimental evidence indicates that under these reaction conditions, the alkenyl succinic anhydride copolymerizes as alternating and/or block copolymers and also, to at least some extent, by grafting, free radical rearrangement or other mechanism to produce quaternary carbon atoms. The acrylic monomers, or monomers having allylic hydrogen, provide a preferred site for grafting or free radical rearrangement not present in the other monomers. In order to provide the lowest possible viscosity, the anhydride-functional polymers preferably are ungelled. By "ungelled" is meant that the polymer itself is substantially free of any gel structures, insoluble fractions or internal crosslinking, and that the monomer mixture used to prepare the polymer was substantially free of any monomers having multiple polymerizable unsaturated sites. are prepared by polymerizing a monomer mixture at least one (meth)acrylic monomer under free radical addition polymerization conditions Polymerizing under free radical addition polymerization conditions are reacted in the presence of a free radical source at a temperature sufficient for polymerization could react with the anhydride group during the polymerization are not typically involved in (meth)acrylic free radical polymerization the polymerization at relatively high temperatures excess of 110° C. ranging from 135° C. to about 170° C normally used for conventional free radical polymerization of (meth)acrylic monomers and initiator concentrations charge than oxygenated inert solvents when minimal color development during the polymerization for the polymerization

反应条件: temp:60.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Fifty grams of PPO ([η]=0.49, chloroform, 25° C.), 50 g of ethylbenzene, 70 g of styrene, 30 g of acrylonitrile and 1.5 g of di-tertiary-butyl peroxide were charged into a 500 cc autoclave, and stirred at 60° C. to achieve uniform dissolution, after which the inside of the autoclave was displaced with nitrogen gas. The temperature of the reaction vessel was controlled to 140° C., and graft polymerization was effected for 2.5 hours. After completion of the reaction, the contents were withdrawn, and dissolved in 3500 ml of toluene by heating. Thereafter, methanol in an amount 10 times that of toluene was added thereto to obtain a resin powder. This powder was washed with methanol and then with methyl ethyl ketone as described in Example 1 to obtain a purified acrylonitrile-styrene grafted PPO. As the result of the organic elemental microanalysis, the degree of grafting was found 71% and the acrylonitrile content in this acrylonitrile-styrene copolymer graft side-chains was found to be 27%. Two grams of this acrylonitrile-styrene grafted PPO was dissolved in 40 ml of methylene chloride, placed in a stoppered Erlenmeyer flask, and allowed to stand in a constant temperature chamber at 23° C. Observation after 48 hours revealed that this solution was opaque. This solution was filtered to obtain a precipitate, which was dried and weighed to yield 1.26 g. In other words, 63% of the resin was recovered as the precipitate. dissolution was controlled to 140° C. graft polymerization After completion of the reaction the contents were withdrawn dissolved in 3500 ml of toluene by heating Thereafter, methanol in an amount 10 times that of toluene was added to obtain a resin powder This powder was washed with methanol