Acrylic Acid → Butyl prop-2-enoate;styrene

HRID 531388Notes

Reaction equation

HRID 531388 reaction equation
[CH2:1]=[CH:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1.[C:9]([O:13][CH2:14][CH2:15][CH2:16][CH3:17])(=[O:12])[CH:10]=[CH2:11].C(O)(=O)C=C.C(=O)([O-])O.[Na+].S(OOS([O-])(=O)=O)([O-])(=O)=O.[NH4+].[NH4+].O.N>O>[CH2:1]=[CH:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1.[C:9]([O:13][CH2:14][CH2:15][CH2:16][CH3:17])(=[O:12])[CH:10]=[CH2:11]

Participants

8

Reactant 6

HCID 6581Acrylic AcidHCID 7501StyreneHCID 8846Butyl AcrylateHCID 62648Ammonium PersulfateHCID 516892Sodium BicarbonateHCID 12896473Azane;hydrate

Product 1

HCID 168422Butyl prop-2-enoate;styrene

Reagents, catalysts & solvents 1

HCID 962WaterSolvent3×

Conditions

Temperature
80 °C

Procedure

Monomers, namely 123.75 g of styrene, 123.75 g of butyl acrylate and 2.5 g of acrylic acid were mixed with 5.0 g of the emulsifier that is the invention product or comparative product and 105 g of ion-exchanged water by using a homomixer, thereby preparing a mixed monomer emulsion liquid. Separately from this, 122 g of ion-exchanged water and 0.25 g of sodium hydrogencarbonate were charged in a reactor provided with a stirrer, a reflux condenser, a thermometer, a nitrogen introducing pipe, and a dropping funnel. In the dropping funnel, 36 g of the above-described previously prepared mixed monomer emulsion liquid was charged and added batchwise in the reactor, and the temperature was then increased to 80° C. Stirring was then continued for 15 minutes, and a solution of 0.5 g of ammonium persulfate as a polymerization initiator in 20 g of ion-exchanged water was added, thereby initiating polymerization. Subsequently, 15 minutes after addition of the polymerization initiator, 324 g of the residue of the mixed monomer emulsion liquid was dropped over 3 hours, thereby conducting polymerization. Furthermore, the resultant was continuously ripened for 2 hours and then cooled, followed by adjusting the pH to 8 with ammonia water. There were thus obtained polymer dispersions to be provided for evaluation experiments of the present invention.

Workup

  1. custompreparing a mixed monomer emulsion liquid
  2. customprovided with a stirrer, a reflux condenser
  3. customIn the dropping funnel, 36 g of the above-described previously prepared
  4. additionmixed monomer emulsion liquid
  5. additionwas charged
  6. additionadded batchwise in the reactor
  7. custompolymerization
  8. additionwas dropped over 3 hours
  9. custompolymerization
  10. waitFurthermore, the resultant was continuously ripened for 2 hours
  11. temperaturecooled
  12. customto be provided for evaluation experiments of the present invention

Sources & evidence

ORD record
ord-33c190b6443443378c9fb52f4b84944d
Source dataset
uspto-grants-2016_05
Patent number
US09353195B2

Reaction notes

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