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Azobisisobutyronitrile → Acrylurethane

HRID 381615
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인쇄 미리보기

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HRID 381615 반응식
[C:1]([O:5][CH2:6][CH:7](CC)CCCC)(=[O:4])C=C.C(#N)C=C.CC(C(OCCO)=O)=C.CC(N=NC(C#N)(C)C)(C#N)C.C1CCN(C[CH:46]2C(C3C=CC(Cl)=CC=3)=N[NH:50][C:48](=[O:49])[CH2:47]2)CC1.Cl.C(NN)(=O)CCCC(NN)=O>O.CC(O)C.CCC(C)=O>[C:48]([NH:50][C:1]([O:5][CH2:6][CH3:7])=[O:4])([CH:47]=[CH2:46])=[O:49]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

10

반응물 6

HCID 6547AzobisisobutyronitrileHCID 76362-Ethylhexyl acrylateHCID 7855AcrylonitrileHCID 133602-Hydroxyethyl Methacrylate2회HCID 30313456-(p-Chlorophenyl)-5-(piperidinomethyl)-4,5-dihydro-3(2H)-pyridazinone monohydrochlorideHCID 3958848Pentanedihydrazide

생성물 1

HCID 11768685
Acrylurethane

시약·촉매·용매 3

HCID 962Water용매HCID 3776Isopropanol용매2회HCID 6569Methyl Ethyl Ketone용매2회

반응 조건

온도
75 °C

실험 절차

In the dropping tank of a reaction vessel (tank) equipped with a stirrer, a thermometer, a nitrogen-sealing tube, a condenser and a dropping tank were placed 8.0 parts of MMA, 15.0 parts of BA, 1.0 part of AA, 1.0 part of 2-ethylhexyl acrylate (referred to here-inafter as EHA), 10.0 parts of acrylonitrile (referred to hereinafter as AN), 5.0 parts of HEMA, 5.0 parts of DAAA, 1.0 part of AIBN, 25 parts of MEK and 25 parts of IPA and then uniformly mixed. Separately, in the reaction tank were placed 20.0 parts of PA-8, 8.0 parts of MMA, 15.0 parts of BA, 1.0 part of AA, 1.0 part of EHA, 10.0 parts of AN, 5.0 parts of HEMA, 5.0 parts of DAAA, 20 parts of MEK and 20 parts of IPA and then uniformly mixed. Subsequently, the reaction tank was heated to 75° C. and the liquid mixture in the dropping tank was dropped into the reaction tank over 5 hours. Thereafter, the resulting mixture was further subjected to reaction at the same temperature for 4 hours. Thereafter, 2.8 parts of TEA was added to the reaction mixture to sufficiently neutralize the same and then aqueous hydrazide consisting of 148 parts of distilled water and 4.7 parts of glutaric acid dihydrazide (referred to hereinafter as GDH) was added thereto to emulsify the reaction mixture. Thereafter, the MEK and the IPA present in the system were removed at 60° C. at 100 Torr to obtain an aqueous emulsion of a self-emulsifiable acryl-urethane copolymer having a solid content of 39.9% (the emulsion is referred to hereinafter as EA-11).

후처리

  1. customIn the dropping tank of a reaction vessel (tank) equipped with a stirrer
  2. additionuniformly mixed
  3. additionuniformly mixed
  4. additionthe liquid mixture in the dropping tank was dropped into the reaction tank over 5 hours
  5. customThereafter, the resulting mixture was further subjected to reaction at the same temperature for 4 hours
  6. additionThereafter, 2.8 parts of TEA was added to the reaction mixture
  7. additionwas added
  8. customThereafter, the MEK and the IPA present in the system were removed at 60° C. at 100 Torr

출처 및 근거

ORD 기록
ord-f52317c0476c4330a5e4a6f1b79aa82f
출처 데이터셋
uspto-grants-2001_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06306947B1

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