Sulfuric Acid → ethylphosphonous acid aluminum(III) salt

HRID 338048

반응식

HRID 338048 반응식
O.[PH2]([O-])=O.[Na+].S(=O)(=O)(O)O.C=C.C([O-])([O-])=O.C([O-])([O-])=O.OO.OO.OO.[Na+].[Na+].[Na+].[Na+].[Al:31].[Al+3].[CH2:33]([P:35](CC)(=[O:37])[O-:36])[CH3:34].[CH2:40]([P:42](CC)(=[O:44])[O-:43])[CH3:41].[CH2:47]([P:49](CC)(=[O:51])[O-:50])[CH3:48]>O>[Al+3:31].[CH2:33]([P:35]([O-:37])[O-:36])[CH3:34].[CH2:40]([P:42]([O-:44])[O-:43])[CH3:41].[CH2:47]([P:49]([O-:51])[O-:50])[CH3:48].[Al+3:31]

참가 물질

8

반응물 6

HCID 1118Sulfuric AcidHCID 6325Ethylene3회HCID 159762Sodium percarbonate2회HCID 5359268AluminumHCID 21863131Phosphinic acid, P,P-diethyl-, aluminum salt (3:1)HCID 178418950HCID 178418950, 화합물

생성물 1

HCID 131732054ethylphosphonous acid aluminum(III) salt수율 95%

시약·촉매·용매 1

HCID 962Water용매2회

반응 조건

온도
100 °C

실험 절차

1500 g (14 mol) of sodium hypophosphite monohydrate and 14 g of concentrated sulfuric acid are dissolved in 7.5 kg of water and initially charged in a 16 l steel-enamel jacketed pressure reactor. After heating the reaction mixture to 100° C., a reducing valve set to 6 bar is used to introduce ethylene into the reactor up to saturation. While stirring constantly at an ethylene pressure of 6 bar and a temperature of 100-110° C., a solution of 22 g (1 mol %) of sodium percarbonate in 300 g of water is metered in homogeneously. At a conversion of ethylene of 83.5%, the metered addition of sodium percarbonate is stopped and the reactor is decompressed. After cooling to about 90° C., 3000 g (4.67 mol of aluminum) of a 46% aqueous solution of Al2(SO4)3.14H2O were added within 60 minutes. Subsequently, the resulting solid is filtered off, washed with 2 l of hot water and dried at 130° C. under reduced pressure. The resulting mixture comprises diethylphosphinic acid aluminum(III) salt and ethylphosphonous acid aluminum(III) salt in a ratio of 76.4% by weight of diethylphosphinic acid aluminum(III) salt and 23.6% by weight of ethylphosphonous acid aluminum(III) salt (95.0% yield).

후처리

  1. customa reducing valve set to 6 bar
  2. customa temperature of 100-110° C.
  3. temperatureAfter cooling to about 90° C.
  4. filtrationSubsequently, the resulting solid is filtered off
  5. washwashed with 2 l of hot water
  6. customdried at 130° C. under reduced pressure

출처 및 근거

ORD 기록
ord-7f2fd969a5af482caf1e2b43b6f80bbd
출처 데이터셋
uspto-grants-2014_11
특허 번호
US08889772B2

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