Method of making adjuvant for elastomeric composition

Claim 1

A method of making a molding composition comprising (A) performing an adjuvant by slurrying zinc oxide in a volatile liquid medium selected from the group consisting of water and an alkanol, the concentration of zinc oxide in the slurry being from 31 to 65 percent by weight, thereafter rapidly adding to the slurry, while agitating the slurry, methacrylic acid in an amount such as to provide a zinc oxide-methacrylic acid molar ratio of at least 0.8 to 1, the methacrylic acid being added within a 30-second addition time, whereby an exothermic reaction between the zinc oxide and the methacrylic acid takes place, the said liquid medium serving to dissipate the heat liberated by the exothermic reaction, subsequently removing the volatile liquid medium from the resulting reaction product by evaporation to provide a dried product having a moisture content below 0.5% by weight, and grinding the resulting dried product at least to a fineness sufficient to pass a 200 mesh sieve, the resulting product being of white color and having an assay of at least 90% by weight of material in which zinc oxide and methacrylic acid are combined in the proportions required by basic zinc methacrylate, the product having a pH of from 6.0 to 6.25 in a water slurry, and displaying in thermogravimetric analysis a 5% weight loss between 120° and 140° C, an additional 10% loss between 180° and 240° C, and an additional 35% loss between 320° and 430° C, and displaying in differential thermal analysis a pronounced endothermic change peaking at 180° C followed by a smaller endothermic change at 235° C, and (B) thereafter uniformly mixing from 10 to 60 parts by weight of the resulting preformed adjuvant with 100 parts by weight of a free-radical crosslinkable resilient elastomer and a free-radical curing agent for the elastomer in amount sufficient to cure the elastomer.

Claim 2

A method of making a molding composition comprising (A) performing an adjuvant by slurrying zinc oxide in a volatile liquid medium selected from the group consisting of water and an alkanol, the concentration of zinc oxide in the slurry being from 31 to 65 percent by weight, thereafter rapidly adding to the slurry, while agitating the slurry, methacrylic acid in an amount such as to provide a zinc oxide-methacrylic acid molar ratio of at least 0.8 to 1, the methacrylic acid being added within a 30-second addition time, whereby an exothermic reaction between the zinc oxide and the methacrylic acid takes place, the said liquid medium serving to dissipate the heat liberated by the exothermic reaction, subsequently removing the volatile liquid medium from the resulting reaction product by evaporation to provide a dried product having a moisture content below 0.5% by weight, and grinding the resulting dried product at least to a fineness sufficient to pass a 200 mesh sieve, the resulting product being of white color and having an assay of at least 90% by weight of material in which zinc oxide and methacrylic acid are combined in the proportions required by basic zinc methacrylate, the product having a pH of from 6.0 to 6.25 in a water slurry, and displaying in thermogravimetric analysis a 5% weight loss between 120° and 140° C, an additional 10% loss between 180° and 240° C, and an additional 35% loss between 320° and 430° C, and displaying in differential thermal analysis a pronounced endothermic change peaking at 180° C followed by a smaller endothermic change at 235° C, and (B) thereafter uniformly mixing from 10 to 60 parts by weight of the resulting preformed adjuvant with 100 parts by weight of a free-radical crosslinkable resilient elastomer and a free-radical curing agent for the elastomer in amount sufficient to cure the elastomer.