Nitric Acid → Styrene acrylic acid copolymer

HRID 2045751Notes

Reaction equation

HRID 2045751 reaction equation
[CH2:1]=[CH:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1.[C:9]([O:13]CCCC)(=[O:12])[CH:10]=[CH2:11].C(O)(=O)C=C.C(S)CCCCCCCCCCC.C(Br)(Br)(Br)Br.[OH-].[Na+].[N+]([O-])(O)=O>O.S(OOS([O-])(=O)=O)([O-])(=O)=O.[NH4+].[NH4+]>[CH2:1]=[CH:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1.[CH2:11]=[CH:10][C:9]([OH:13])=[O:12]

Participants

10

Reactant 7

HCID 944Nitric AcidHCID 6581Acrylic AcidHCID 7501StyreneHCID 81951-DodecanethiolHCID 8846Butyl AcrylateHCID 11205Carbon tetrabromideHCID 14798Sodium Hydroxide

Product 1

HCID 22481611Styrene acrylic acid copolymer

Reagents, catalysts & solvents 2

HCID 962WaterSolvent2×HCID 62648Ammonium PersulfateSolvent

Conditions

Temperature
70 °C

Procedure

370 parts of styrene, 30 parts of n-butyl acrylate, 8 parts of acrylic acid, 24 parts of dodecanethiol and 4 parts of carbon tetrabromide are mixed and dissolved, and put in a flask together with 6 parts of a nonionic surfactant (trade name: NONIPOL 400, manufactured by Sanyo Chemical Industries, Ltd.) and 10 parts of anionic surfactant (trade name: NEOGEN SC, Dai-ichi Kogyo Seiyaku Co., Ltd.), which are dissolved in 550 parts of ion exchange water, and the mixture is dispersed and emulsified. While slowly mixing for 10 minutes, 50 parts of ion exchange water in which 4 parts of ammonium persulfate is dissolved is put in the mixture and, after performing nitrogen-substitution, the mixture is heated to 70° C. in an oil bath while agitating, and in the same condition emulsion aggregation is continued for five hours. Thereafter, the pH in the system is adjusted to 12.5 with a 0.5 mol/l aqueous solution of sodium hydroxide and treatment is carried out at 96° C. for six hours. The pH is then adjusted to 3.0 with a nitric acid aqueous solution and the solid content of the mixture is adjusted, thereby obtaining a styrene/acrylic acid resin dispersion (E1) having a volume average particle diameter of 155 nm, glass transition temperature of 59° C., weight average molecular weight of 12,000 and a solid content of 40%.

Workup

  1. dissolutiondissolved
  2. customput in a flask together with 6 parts of a nonionic surfactant (trade name: NONIPOL 400, manufactured by Sanyo Chemical Industries, Ltd.) and 10 parts of anionic surfactant (trade name: NEOGEN SC, Dai-ichi Kogyo Seiyaku Co., Ltd.), which
  3. additionthe mixture is dispersed
  4. additionWhile slowly mixing for 10 minutes
  5. waitis carried out at 96° C. for six hours

Sources & evidence

ORD record
ord-680d2ce36f2b484e8e7c5616b502809b
Source dataset
uspto-grants-2013_11
Patent number
US08592124B2

Reaction notes

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