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Terephthaloyl chloride → Terephthalohydrazide

HRID 1660530
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HRID 1660530 반응식
[C:1]([NH:12][NH2:13])(=[O:11])[C:2]1[CH:10]=[CH:9][C:5]([C:6]([OH:8])=O)=[CH:4][CH:3]=1.NC1C=CC(C([NH:21][NH2:22])=O)=CC=1.C1C(N)=CC=C(N)C=1.NC1C=CC(C(Cl)=O)=CC=1.C(Cl)(=O)C1C=CC(C(Cl)=O)=CC=1>>[C:6]([NH:21][NH2:22])(=[O:8])[C:5]1[CH:9]=[CH:10][C:2]([C:1]([NH:12][NH2:13])=[O:11])=[CH:3][CH:4]=1
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6

반응물 5

HCID 7488Terephthaloyl chlorideHCID 7814P-PhenylenediamineHCID 214504-Aminobenzoic acid hydrazideHCID 177720Benzoyl chloride, 4-amino-HCID 2794374-(Hydrazinocarbonyl)benzoic acid

생성물 1

HCID 67294Terephthalohydrazide

실험 절차

Terephthalic acid hydrazide, p-aminobenzoic acid hydrazide, p-phenylenediamine, p-aminobenzoyl chloride and terephthaloyl chloride are properly combined, and a 5 wt% solution of polyamide resin comprising 33 mol% of terephthalhydrazide, 33 mol% of p-benzamide, and 33 mol% of p-phenyleneterephthalamide is obtained by low temperature (about 10° to 35° C.) solution polymerization process. The solvent used for the solution polymerization is preferably dimethylacetamide and calcium chloride is contained in the polymerization solution as a neutralization product. This solution is cast on a metallic belt and dried until the polymer concentration becomes about 30 wt% by heating at about 100° C. for 5 minutes. The film is then dipped for about 2 minutes in water at normal temperatures (about 10° to 35° C.) to remove the solvent and calcium chloride. After further washing with water and drying at 230° C., the resulting film is rolled up. Orientation is conducted by stretching the dried film in the longitudinal direction in a 50° C. dimethylacetamide aqueous solution through the difference in rotating speeds of associated nip rolls, and subsequently stretching it in a lateral direction by guiding it to a tenter and expanding the rail distance. The draw ratio is generally kept from about 1.1 to 2.0 times in both longitudinal and lateral directions. Thus, a 3 μm thick aromatic polyamide film is obtained.

출처 및 근거

ORD 기록
ord-58a6422fa5a4409583e0e1c213ba6bfc
출처 데이터셋
uspto-grants-1981_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04308311

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