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Methane → Resorcinol

HRID 487511
ノート
印刷プレビュー

反応式

HRID 487511 の反応式
[CH4:1].[CH2:2]=[CH:3][C:4]1[CH:9]=CC=[CH:6][CH:5]=1.[CH3:10][N:11]1[CH:15]=[C:14]([N+]([O-])=[O:17])[N:13]=[CH:12]1.C(OOC(=O)CCCCCCCCCCC)(=O)CCCCCCCCCCC.CC1C(N=C=O)=CC(N=C=O)=CC=1.C1(N=C=O)C=CC=CC=1.C(OCC(CC)CCCC)(=O)C=C.C(C1C=CC=CC=1C=C)=C.P([O-])([O-])([O-])=O.[Ca+2].P([O-])([O-])([O-])=O.[Ca+2].[Ca+2].Cl.[OH2:106]>C(O)(C)(C)C>[C:1]1([CH:6]=[CH:5][CH:4]=[C:3]([OH:17])[CH:2]=1)[OH:106].[NH2:11][C:1]1[CH:2]=[C:3]([OH:106])[CH:4]=[CH:5][CH:6]=1.[N:13]12[CH2:4][CH2:9][N:11]([CH2:10][CH2:12]1)[CH2:15][CH2:14]2
参加物実験手順後処理出典と根拠反応ノート

参加物

15

反応物 11

HCID 297Methane2 回HCID 313Hydrochloric AcidHCID 962WaterHCID 7501Styrene3 回HCID 76362-Ethylhexyl acrylateHCID 7672Phenyl isocyanateHCID 7773Lauroyl peroxide
HCID 11443
Toluene 2,4-Diisocyanate
HCID 182091-Methyl-4-nitroimidazole
HCID 24456Tricalcium Phosphate
HCID 666661,2-Diethenylbenzene

生成物 3

HCID 5054ResorcinolHCID 9237DabcoHCID 115683-Aminophenol

試薬・触媒・溶媒 1

HCID 6386tert-Butanol溶媒

実験手順

40 parts by weight of carbon black grafted with styrene "GP-E-3" (manufactured by Ryoyu Kogyo K. K.), which contains 40% by weight of styrene monomer, 30% by weight of polystyrene and 30% by weight of grafted carbon black, 1.5 parts by weight of charge control agent of negative charging type 3-methyl-5-nitroimidazole, 4.5 parts by weight of lauroyl peroxide, 9.0 parts by weight of tolylene diisocyanate "Coronate T-100" (mfd. by Nippon Polyurethane Industry Co., Ltd.) and 0.5 part by weight of phenyl isocyanate were added to a mixture of 50 parts by weight of styrene with 35 parts by weight of 2-ethylhexyl acrylate and 0.9 part by weight of divinylbenzene to prepare a polymerizable composition. The polymerizable composition was added to 800 g of a 4 wt. % solution of calcium phosphate in an aqueous colloid previously prepared in a 2-l separable glass flask in such an amount that the concentration of the polymerizable composition became 30 % by weight based on the total of the aqueous colloid solution and the polymerizable composition. The mixture was dispersed and emulsified on a TK Homomixer mfd. by Tokushu Kika Kogyo Co., Ltd. at 10,000 rpm at 5° C. for 2 min. A four neck glass lid was placed on the flask and fitted with a reflux condenser, a thermometer, a dropping funnel having a nitrogen-inlet tube and a stainless steel stirring rod. The flask was placed in an electric mantle. A mixed solution of 24.0 g of resorcinol, 3.0 g of m-aminophenol, 2.2 g of t-butyl alcohol, 0.5 g of 1,4-diazabicyclo[2.2.2]-octane and 40 g of deionized water was prepared and added dropwise into the flask through the dropping funnel while stirring over a period of 30 min. Then the temperature was elevated to 85° C. while continuing the stirring under nitrogen and the reaction was conducted for 10 h. After cooling the reaction mixture, the dispersant was dissolved by adding 10% aqueous hydrochloric acid solution, and the mixture was filtered. The residue was washed with water, dried at 45° C. for 12 hr under a reduced pressure of 20 mmHg, and classified by means of an air classifier to give an encapsulated toner having an average particle diameter of 9 μm wherein the shell comprises a resin having thermally dissociable urethane bonds. The glass transition point of the resin in the core material of the encapsulated toner and the softening point of the encapsulated toner were 32.0° C. and 129.5° C., respectively.

後処理

  1. customto prepare a polymerizable composition
  2. custompreviously prepared in a 2-l separable glass flask in such an amount that the concentration of the polymerizable composition
  3. additionThe mixture was dispersed
  4. customfitted with a reflux condenser
  5. additionadded dropwise into the flask through the dropping funnel
  6. customwas elevated to 85° C.
  7. waitthe reaction was conducted for 10 h
  8. temperatureAfter cooling the reaction mixture
  9. dissolutionthe dispersant was dissolved
  10. filtrationthe mixture was filtered
  11. washThe residue was washed with water
  12. customdried at 45° C. for 12 hr under a reduced pressure of 20 mmHg
  13. customto give an encapsulated toner
  14. customwere 32.0° C. and 129.5° C.

出典と根拠

ORDレコード
ord-745390f1ad1346cabf82b62a14670b2a
出典データセット
uspto-grants-1994_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05294490

反応ノート

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