Sulfuric Acid → Butyl prop-2-enoate--methyl 2-methylprop-2-enoate (1/1)

HRID 611725

반응식

HRID 611725 반응식
S(=O)(=O)(O)O.[C:6]([O:11][CH3:12])(=[O:10])[C:7]([CH3:9])=[CH2:8].[C:13]([O:17][CH2:18][CH2:19][CH2:20][CH3:21])(=[O:16])[CH:14]=[CH2:15].C(S)CCCCCCCCCCC.S(OOS([O-])(=O)=O)([O-])(=O)=O.[K+].[K+]>O>[C:6]([O:11][CH3:12])(=[O:10])[C:7]([CH3:9])=[CH2:8].[C:13]([O:17][CH2:18][CH2:19][CH2:20][CH3:21])(=[O:16])[CH:14]=[CH2:15]

참가 물질

7

반응물 5

HCID 1118Sulfuric AcidHCID 6658Methyl Methacrylate2회HCID 81951-Dodecanethiol2회HCID 8846Butyl Acrylate2회HCID 24412Potassium Persulfate

생성물 1

HCID 62802Butyl prop-2-enoate--methyl 2-methylprop-2-enoate (1/1)

시약·촉매·용매 1

HCID 962Water용매2회

반응 조건

온도
70 °C

실험 절차

A glass-made vessel equipped with a reflux condenser, a dropping funnel, a thermometer, a nitrogen blowing-in nozzle and a stirrer was charged with 5 parts of PVA having a mercapto group at only one end thereof (PVA-3: degree of polymerization of 550, degree of hydrolysis of 88.3 mol %, mercapto group content of 3.3×10-5 equivalent/g) and 90 parts of ion-exchanged water, and the PVA was completely dissolved in the water at 95° C. The resultant aqueous solution of the PVA was adjusted to pH=4 with dilute sulfuric acid, and incorporated, under stirring at 150 r.p.m., with 10 parts of methyl methacrylate, 10 parts of n-butyl acrylate and 0.1 part of n-dodecyl mercaptan. Then, the reaction system was replaced with nitrogen, and the temperature in the system was raised to 70° C. Subsequently, emulsion polymerization was initiated by adding to the system, 5 parts of aqueous solution of potassium persulfate having a concentration of 1%. To the system were continuously added the mixture of 40 parts of methyl methacrylate, 40 parts of n-butyl acrylate and 0.4 part of n-dodecyl mercaptan over a period of 2 hours. The polymerization was finished at the time when a conversion of 99.5% was achieved after 3 hours from the start of the polymerization. As a result, there was obtained a stable emulsion of methyl methacrylate/n-butyl acrylate copolymer having a solid concentration of 52.0%. Thereafter, the procedure in Example 1 was repeated to produce the synthetic resin powder except that the emulsion thus obtained was used. The results of evaluation of the powder are given in Tables 3 and 4.

후처리

  1. customA glass-made vessel equipped with a reflux condenser, a dropping funnel
  2. additiona thermometer, a nitrogen blowing-in nozzle and a stirrer was charged with 5 parts of PVA
  3. customSubsequently, emulsion polymerization
  4. additionTo the system were continuously added
  5. customwas achieved after 3 hours from the start of the polymerization

출처 및 근거

ORD 기록
ord-b956cc9a74984f7cbc4d6df830b542e6
출처 데이터셋
uspto-grants-1999_12
특허 번호
US06001903

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