تفاعل #171136

ord-6b1b3ec280464829a4233e45fed7bdff

معادلة التفاعل

C=CC=C
butadiene
O
water
N
ammonia
O=S(=O)([O-])OOS(=O)(=O)[O-].[Na+].[Na+]
sodium persulfate
O=S([O-])CO.[Na+]
sodium hydroxymethylsulfinate
O
water
O
water
O=S([O-])CO.[Na+]
sodium hydroxymethylsulfinate
CC(=O)ON(CCN(OC(C)=O)OC(C)=O)OC(C)=O.[Na].[Na].[Na].[Na]
tetrasodium ethylene diamine tetraacetate
CC(C)C(C)(C)C(C)(C)C(C)(C)S
tert-dodecylmercaptan
C=C1CCOC1=O
α-methylene-γ-butyrolactone
C=CC(=O)O
acrylic acid
CCCCCCCCCCCCOS(=O)(=O)c1ccccc1.[Na]
sodium dodecyl benzenesulfonate
O
water
→
C=C1CCOC1=O.C=CC(=O)O.C=CC=C
α-methylene-γ-butyrolactone butadiene acrylic acid

المتفاعلات

C=CC=C
butadiene
—
aqueous mixture
O
water
N
ammonia
O=S(=O)([O-])OOS(=O)(=O)[O-].[Na+].[Na+]
sodium persulfate
—
monomer
O=S([O-])CO.[Na+]
sodium hydroxymethylsulfinate
O
water
O
water
O=S([O-])CO.[Na+]
sodium hydroxymethylsulfinate
CC(=O)ON(CCN(OC(C)=O)OC(C)=O)OC(C)=O.[Na].[Na].[Na].[Na]
tetrasodium ethylene diamine tetraacetate
CC(C)C(C)(C)C(C)(C)C(C)(C)S
tert-dodecylmercaptan
C=C1CCOC1=O
α-methylene-γ-butyrolactone
C=CC(=O)O
acrylic acid
CCCCCCCCCCCCOS(=O)(=O)c1ccccc1.[Na]
sodium dodecyl benzenesulfonate
O
water

الكواشف

لا شيء

ظروف التفاعل

درجة الحرارة
80°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.ADDITIONis added by cannula over 3 minutes
  2. 2
    workup.ADDITIONis added over 2 minutes
  3. 3
    workup.ADDITIONthe remainder of the monomer pre-emulsion and aqueous mixture is added uniformly over 300 minutes
  4. 4
    workup.STIRRINGto stir for an additional 7 hours at 80° C
  5. 5
    workup.STIRRINGwith stirring
  6. 6
    أخرىis dried under vacuum at elevated temperature for isolation

الإجراء التجريبي

A 150 mL round bottom flask with a magnetic stir bar is charged with 17 g (0.943 mol) of water, 0.01 g (6.49×10−5 mol) of sodium hydroxymethylsulfinate and 0.001 g (2.63×10−6 mol) of tetrasodium ethylene diamine tetraacetate. The reactor is heated to 80° C. under nitrogen. After 5 minutes at 80° C., 8 g of a monomer pre-emulsion consisting of 26.5 g (0.490 mol) of butadiene, 18.5 g (0.189 mol) of α-methylene-γ-butyrolactone, 1.5 g (2.50×10−2 mol) of acrylic acid, 1.332 g (3.82×10−3 mol) of sodium dodecyl benzenesulfonate (15% aqueous solution), 0.25 g (1.24×10−3 mol) of tert-dodecylmercaptan and 22 g (1.22 mol) of water is added by cannula over 3 minutes. Additionally, 1 g of an aqueous mixture consisting of 0.25 g (4.20×10−3 mol) of sodium persulfate and 7 g (0.389 mol) of water is added over 2 minutes. After stirring for 20 minutes at 80° C., the remainder of the monomer pre-emulsion and aqueous mixture is added uniformly over 300 minutes. When all additions were completed, the polymerization is allowed to stir for an additional 7 hours at 80° C. Upon completion, steam is passed through the mixture under reduced pressure and a solution of 0.25 g (1.62×10−3 mol) of sodium hydroxymethylsulfinate in 1 g (5.55×10−2 mol) of water is added slowly, with stirring. The pH of the dispersion is brought to 7 with 10% strength aqueous ammonia before the dispersion is dried under vacuum at elevated temperature for isolation.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08846817B2uspto-grants-2014_09