반응 #71316

ord-e8e5c9b217304c25bd644baa097523f1

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타A glass reactor equipped
  2. 2
    기타at 13° C
  3. 3
    기타a solids content of 39% was obtained

실험 절차

A glass reactor equipped with several feeding devices, stirrer and pH electrode was charged with 285 g of water, 210 g of vinyloxybutylpolyethylene glycol-3000 (prepared by ethoxylation of hydroxybutyl vinyl ether with 66 mol EO) and 23.3 g of isoprenylpolyethylene glycol-500 (prepared by ethoxylation of 3-methyl-3-buten-1-ol with 10 mol EO) (solution A) and was thermostated at 13° C. 35% of a second prepared, partly neutralized solution (solution B) consisting of 50 g of water and 25.4 g of acrylic acid (99%) was added to solution A over a period of 15 min in the glass reactor. Furthermore, 1.9 g of 3-mercaptopropionic acid was added to the reactor. A third solution (solution C) consisting of 5 g of a mixture of sodium sulphite, the disodium salt of 2-hydroxy-2-sulphinatoacetic acid and the disodium salt of 2-hydroxy-2-sulphonatoacetic acid (Brüggolit FF6 from Brüggemann GmbH) and 40 g of water was prepared. Thereafter, 50 mg of iron(II) sulphate haptahydrate, dissolved in a few drops of water, and 2.5 g of 50% strength hydrogen peroxide solution were added to solution A at a temperature of 13° C. At the same time, the still remaining solution B was dosed over 45 minutes and solution C over 60 minutes into the solution A. Finally, neutralization was effected with 20% strength sodium hydroxide solution. The aqueous solution of a copolymer having an average molecular weight of Mw=24 300 g/mol (determined by GPC) and a solids content of 39% was obtained.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08536251B2uspto-grants-2013_09