Styrene → 2-Propenoic acid, butyl ester, polymer with diethenylbenzene and ethenylbenzene

HRID 2301256Notes

Reaction equation

HRID 2301256 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].[CH:18]([C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][C:21]=1[CH:26]=[CH2:27])=[CH2:19].S(OOS([O-])(=O)=O)([O-])(=O)=O.[NH4+].[NH4+]>O>[CH:18]([C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][C:21]=1[CH:26]=[CH2:27])=[CH2:19].[C:9]([O:13][CH2:14][CH2:15][CH2:16][CH3:17])(=[O:12])[CH:10]=[CH2:11].[CH2:1]=[CH:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1

Participants

6

Reactant 4

HCID 7501Styrene2×HCID 8846Butyl Acrylate2×HCID 62648Ammonium PersulfateHCID 666661,2-Diethenylbenzene2×

Product 1

HCID 64540352-Propenoic acid, butyl ester, polymer with diethenylbenzene and ethenylbenzene

Reagents, catalysts & solvents 1

HCID 962WaterSolvent7×

Conditions

Temperature
75 °C

Procedure

A crosslinked latex resin emulsion comprised of crosslinked resin or polymer particles derived from the emulsion polymerization of styrene, butyl acrylate, beta carboxyl ethyl acrylate (Beta CEA) and divinylbenzene was prepared as follows. An organic phase was prepared by blending 380 grams of styrene, 162 grams of butyl acrylate, 16.2 grams of beta carboxyl ethyl acrylate (Beta CEA) and 5.4 grams of divinylbenzene. An aqueous phase was then prepared by mixing 9.4 grams of the surfactant DOWFAX® in 230 grams of water. The organic phase was then added to the aqueous phase and the resulting mixture was stirred to form an oil in water dispersion. To a 2 liter Buchi stainless steel reactor equipped with a stirrer, a thermocouple and a nitrogen inlet was added an aqueous solution of a surfactant, and 2 grams of DOWFAX® in 500 grams of water. The reactor was heated to 75° C. under a nitrogen atmosphere with stirring (300 rpm). To the reactor was then added 14 grams of the above prepared oil in water dispersion followed by the addition of an aqueous solution of 8.5 grams of ammonium persulfate in 90 grams of water. The resulting mixture was stirred for 10 minutes at 75° C., and then the remainder of the above oil in water dispersion was added slowly over a two hour period. After the complete addition of the oil in water dispersion to the reactor, the resulting mixture was heated for a further two hours to complete the polymerization, cooled to room temperature, about 25° C. and discharged to yield a crosslinked polymer latex with a polymer of a styrene butyl acrylate divinylbenzene polymer, which polymer was fully crosslinked, about 100 percent crosslinked, 40 percent polymer solids in water with a polymer particle diameter size of 114 nanometers as measured by a disc centrifuge.

Workup

  1. customwas prepared
  2. customAn organic phase was prepared
  3. customAn aqueous phase was then prepared
  4. additionThe organic phase was then added to the aqueous phase
  5. stirringwith stirring (300 rpm)
  6. additionTo the reactor was then added 14 grams of the
  7. stirringThe resulting mixture was stirred for 10 minutes at 75° C.
  8. temperaturethe resulting mixture was heated for a further two hours
  9. customthe polymerization
  10. temperaturecooled to room temperature, about 25° C.

Sources & evidence

ORD record
ord-4dcefe360bac44038ac2cc13985e6f2f
Source dataset
uspto-grants-2002_12
Patent number
US06500597B1

Reaction notes

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