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US4758665A Expired / Lapsed US ⏱️ 0.0 years remaining

Process for preparing high-hiding gamma-modification of unsubstituted linear transquinacridone

Assignee: Hoechst AG
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Filing: 1986-11-13
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Granted: 1988-07-19
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Expires: 2006-11-13
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Abstract

Abstract A process for preparing the high-hiding form of the γ-crystal modification of unsubstituted linear transquinacridone having improved tinctorial strength and producing a coating of higher gloss, which comprises carrying out (a) the known cyclization of 2,5-diphenylaminoterephthalic acid in highly concentrated polyphosphoric acid or in acid polyphosphoric acid ester to the quinacridone and/or (b) the known hydrolysis of the quinacridone melt obtained in (a) and/or (c) the known aqueous alkali extraction of the quinacridone obtained in (b) and/or (d) the known finishing of the quinacridone obtained in (a) in the presence of 0.5 to 10 percent by weight, based on quinacridone, of surface-active agents.

Inventors

  • 👤 Ernst Spietschka
  • 👤 Adolf Kroh

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-11-02 01:30
CPC Classifications
C; C09; C09B; C09B67/00; C09B67/0025; C09B67/0027; C09B48/00

Claims Analysis

Total Claims: 17
Claim 1
Independent Claim 191 words
In a process for preparing the high-hiding form of the γ-crystal modification of unsubstituted linear transquinacridone having improved tinctorial strength and producing a coating of higher gloss, which process includes (a) cyclizing 2,5-diphenylaminoterephthalic acid, in highly concentrated polyphosphoric acid or in acid polyphosphoric acid ester, to obtain essentially the quinacridone in its α-modification; (b) hydrolyzing the resulting quinacridone melt obtained in step (a); (c) extracting the quinacridone obtained in step (b) with aqueous alkali, and (d) finishing the thus-isolated quinacridone, the improvement which comprises the further step of providing the presence of 0.5 to 10 percent by weight, based on the weight of the quinacridone, of a surface-active agent component during at least one of said steps (a), (b), (c), and (d), said surface-active agent component being a cationic quaternary ammonium compound; a cationic quaternary phosphonium compound; a nonionic colphony derivative; or combinations of said cationic compounds and nonionic compounds; provided, that if a said surface active component is present during said step (d), the same or a different one of said surface active components is present during at least one other of the remaining three steps (a), (b) or (c).
Claim 2
Dependent Claim 191 words
In a process for preparing the high-hiding form of the γ-crystal modification of unsubstituted linear transquinacridone having improved tinctorial strength and producing a coating of higher gloss, which process includes (a) cyclizing 2,5-diphenylaminoterephthalic acid, in highly concentrated polyphosphoric acid or in acid polyphosphoric acid ester, to obtain essentially the quinacridone in its α-modification; (b) hydrolyzing the resulting quinacridone melt obtained in step (a); (c) extracting the quinacridone obtained in step (b) with aqueous alkali, and (d) finishing the thus-isolated quinacridone, the improvement which comprises the further step of providing the presence of 0.5 to 10 percent by weight, based on the weight of the quinacridone, of a surface-active agent component during at least one of said steps (a), (b), (c), and (d), said surface-active agent component being a cationic quaternary ammonium compound; a cationic quaternary phosphonium compound; a nonionic colphony derivative; or combinations of said cationic compounds and nonionic compounds; provided, that if a said surface active component is present during said step (d), the same or a different one of said surface active components is present during at least one other of the remaining three steps (a), (b) or (c).
Claim 3
Dependent Claim 46 words
A process as claimed in claim 1, wherein said combinations of the surface active agents are, in addition to combinations of said cationic quaternary ammonium compounds with each other or nonionic colophony derivatives with each other: dehydroabietylamine or its salt with a nonionic surface active agent.
Claim 4
Dependent Claim 62 words
A process as claimed in claim 1, wherein said cationic quaternary ammonium compound or cationic quaternary phosphonium compound is permethylated tallow-propylenediamine, stearyltrimethylammonium, alkyl-C 20 -C 22 -trimethylammonium, dioctyldimethylammonium, distearyldimethylammonium, didecyldimethylammonium, cetyltrimethylammonium, benzylcocoalkyldimethylammonium, di-cocoalkyldimethylammonium, cocoalkyl-2,4-dichlorobenzyldimethylammonium, stearylbenzyldimethylammonium, di-β-isopropoxycarbonylhexadecyldimethylammonium, permethylated N-stearoyldiethylenetriamine, permethylated N-stearoyltriethylenetetramine, laurylpyridinium, 2-hydroxy-5-chloro-1,3-xylylenebispyridinium, 2-hydroxy-5-isooctyl-1,3-xylylenebispyridinium, 2-hydroxy-5-t-butyl-1,3-xylylenebispyridinium, 2-hydroxy-5-n-nonyl-1,3-xylylenebispyridinium, 2-methoxy-5-isooctyl-1,3-xylylenebispyridinium, 2-hydroxy-5-isooctyl-1,3-xylylenebisquinolinium, 2-hydroxy-5-isooctyl-1,3-xylylenebisisoquinolinium, hexadecyltributylphosphonium, ethyltrioctylphosphonium and/or tetrabutylphosphonium, or combinations thereof, in which the associated anion can vary.
Claim 5
Dependent Claim 14 words
The process as claimed in claim 1, wherein the nonionic colophony derivative is dehydroabietylamine.
Claim 6
Dependent Claim 16 words
A process as claimed in claim 1, wherein the cationic quaternary ammonium compound is a halide.
Claim 7
Dependent Claim 37 words
A process as claimed in claim 1, wherein the surface active agent component is: (1) at least one said cationic quaternary ammonium compound, or (2) dehydroabietylamine or its salt, or (3) dehydroabietylamine and a nonionic surface-active agent.
Claim 8
Dependent Claim 46 words
A process as claimed in claim 6, wherein the surface active agent component is cetyltrimethylammonium chloride, alkyl C 20 -C 22 -trimethylammonium chloride, dioctyldimethylammonium chloride, benzylstearyldimethylammonium chloride, didecyldimethylammonium chloride, stearyltrimethylammonium chloride, distearyldimethylammonium chloride, cocoalkyldimethylbenzylammonium chloride, dicocoalkyldimethylammonium chloride, dehydroabietylamine, an acid derivative of colophony, or combinations thereof.
Claim 9
Dependent Claim 26 words
A process as claimed in claim 1, wherein the surface active agent component is present during all four of said steps (a), (b), (c), and (d).
Claim 10
Dependent Claim 29 words
A process as claimed in claim 1, wherein a said surface-active agent component is added during said step (b) in the form of a solution in the hydrolyzing water.
Claim 11
Dependent Claim 25 words
A process as claimed in claim 1, wherein a said surface-active agent component is present in the aqueous alkaline extracting medium during said step (c).
Claim 12
Dependent Claim 26 words
A process as claimed in claim 10, wherein the same or a different one of said surface-active agent components is additionally present during said step (d).
Claim 13
Dependent Claim 21 words
A process as claimed in claim 1, wherein a said surface-active agent component is present at least during said step (a).
Claim 14
Dependent Claim 181 words
In a process for preparing the high-hiding form of the γ-crystal modification of unsubstituted linear transquinacridone having improved tinctorial strength and producing a coating of higher gloss, which process includes (a) cyclizing 2,5-diphenylaminoterephthalic acid, in highly concentrated polyphosphoric acid or in acid polyphosphoric acid ester, to obtain essentially the quinacridone in its α-modification; (b) hydrolyzing the resulting quinacridone melt obtained in step (a); (c) extracting the quinacridone obtained in step (b) with aqueous alkali, and (d) finishing the thus-isolated quinacridone, the improvement which comprises the further step of providing the presence of 0.5 to 10 percent by weight, based on the weight of the quinacridone, of a surface-active agent component during at least one of said steps (a), (b), (c), and (d), said surface-active agent component being a combination of a cationic quaternary ammonium or phosphonium compound with an anionic sulfonate salt, sulfate salt, sulfamide-acetate salt, fatty acid tauride or sarcoside salt, sulfosuccinate salt, or resin derivative, the cationic quaternary ammonium or phosphonium compound and the anionic salt being added together during the same step or in succession in different steps.
Claim 15
Dependent Claim 181 words
In a process for preparing the high-hiding form of the γ-crystal modification of unsubstituted linear transquinacridone having improved tinctorial strength and producing a coating of higher gloss, which process includes (a) cyclizing 2,5-diphenylaminoterephthalic acid, in highly concentrated polyphosphoric acid or in acid polyphosphoric acid ester, to obtain essentially the quinacridone in its α-modification; (b) hydrolyzing the resulting quinacridone melt obtained in step (a); (c) extracting the quinacridone obtained in step (b) with aqueous alkali, and (d) finishing the thus-isolated quinacridone, the improvement which comprises the further step of providing the presence of 0.5 to 10 percent by weight, based on the weight of the quinacridone, of a surface-active agent component during at least one of said steps (a), (b), (c), and (d), said surface-active agent component being a combination of a cationic quaternary ammonium or phosphonium compound with an anionic sulfonate salt, sulfate salt, sulfamide-acetate salt, fatty acid tauride or sarcoside salt, sulfosuccinate salt, or resin derivative, the cationic quaternary ammonium or phosphonium compound and the anionic salt being added together during the same step or in succession in different steps.
Claim 16
Dependent Claim 20 words
A process as claimed in claim 1, wherein a said surface-active component is present during at least said step (b).
Claim 17
Dependent Claim 21 words
A process as claimed in claim 1, wherein a said surface-active agent is present during all of steps (a) through (d).

USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 1991-07-19 1992-01-18 1992-07-19 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1995-07-19 1996-01-18 1996-07-19 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 1999-07-19 2000-01-18 2000-07-19 $7700.00 Window Closed / Lapsed

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