Preparation of lakes having improved performance characteristics

Claim 2

A process for the preparation of a lake which has improved performance characteristics and is obtained from a basic dye and a heteropolyacid based on phosphoric acid, molybdic acid, tungstic acid or silicic acid by after-treating the crude pigment obtained during the laking procedure, in aqueous suspension and at elevated temperatures, wherein from 5 to 50% by weight based on the dye used for the laking procedure, of at least one compound selected from the group consisting of (1) primary, secondary or tertiary aliphatic amines which carry one or more C 10 -C 20 -alkyl or C 8 -C 20 -alkoxy-C 2 -C 4 -alkyl groups, (2) N-C 8 -C 20 -alkylamino-C 2 -C 8 -alkanoic acids, (3) diaryl- or triarylamines, (4) acidic or neutral phosphates based on a fatty alcohol, a fatty alcohol oxyalkylate, polypropylene glycol, polyethylene glycol or block copolymers of propylene oxide and ethylene oxide, (5) sulfuric acid half esters based on C 10 -C 20 -fatty alcohols, fatty alcohol/ethylene oxide adducts or C 5 -C 20 -alkylphenol/ethylene oxide adducts, (6) C 8 -C 20 -alkane- or alkenesulfonic acids, C 6 -C 20 -alkylbenzenesulfonic acids, C 1 -C 20 -alkylnaphthalene sulfonic acids or di-C 6 -C 20 -alkylsulfimides, (7) ethylene oxide adducts of C 1 -C 20 -alkylphenols, C 8 -C 20 -alkanols or C 10 -C 20 -alkylamines, the adducts containing not less than 5 ethylene oxide radicals, (8) propylene glycols or block copolymers based on alkanediols or -polyols of 2 to 8 carbon atoms with propylene oxide ad ethylene oxide, and (9) naphthols or C 1 -C 20 -alkylphenols, or mixtures of these are added to the aqueous mixtures before, during or after the laking procedure, the crude pigment in the aqueous suspension is heated to 50°-100° C. at pH 2-5, and the pigment is then isolated.

Claim 3

A process as claimed in claim 1, wherein from 10 to 45% by weight, based on the dye used for the laking procedure, of the agents stated under (1) to (9) is used.

Claim 4

A process as claimed in claim 1, wherein the heat treatment of the crude pigment is carried out in the presence of (1.1) a C 10 -C 20 -alkylamine or a 3-(C 8 -C 20 -alkoxy)-propylamine, where the N atom in the amine may be substituted by 1 or 2 C 1 -C 4 -alkyl radicals, (2.1) an N-C 10 -C 20 -alkylamino-C 2 -C 8 -alkanoic acid, (4.1)(a) a neutral phosphate based on a C 3 -C 18 -alkanol, as a mixture with nonionic ethylene oxide adducts of group (7), (b) an acidic phosphate based on an adduct of ethylene oxide or of propylene oxide/ethylene oxide with a C 10 -C 20 -alkanol, (5.1) a sulfuric acid half ester of an adduct of ethylene oxide with a C 10 -C 20 -alkylphenol, the adduct containing on average from 2 to 6 moles of ethylene oxide per mole, (6.1) a C 8 -C 20 -alkylbenzenesulfonic acid, (7.1) an adduct of ethylene oxide with a C 6 -C 20 -alkylphenol or a C 8 -C 20 -alkanol, containing from 5 to 55 moles of ethylene oxide per mole of phenol or alkanol, or a mixture or these agents.

Claim 5

A process as claimed in claim 1, wherein the heat treatment of the crude pigment is carried out in the presence of (1.2) a C 14 -C 20 -alkylamine or a 3-(C 10 -C 20 -alkoxy)-propylamine, where the N atom may be substituted by one or two C 1 -C 4 -alkyl radicals, (2.2) a β-(N-C 10 -C 20 -alkylamino)-butyric acid, (4.2)(a) a neutral phosphate based on a C 3 -C 18 -alkanol, as a mixture with an adduct of ethylene oxide with a C 6 -C 20 -alkylphenol or a C 8 -C 20 -alkanol, containing from 5 to 55 moles of ethylene oxide per mole of phenol or alkanol, (4.2)(b) an acidic phosphate based on an adduct of ethylene oxide or of propylene oxide/ethylene oxide with a C 10 -C 20 -alkanol, (5.2) a sulfuric acid half ester of an adduct of ethylene oxide with a C 10 -C 20 -alkanol or a C 6 -C 20 -alkylphenol, the adduct containing on average from 2 to 6 moles of ethylene oxide per mole of alkanol or phenol, (6.2) a C 8 -C 20 -alkylbenzenesulfonic acid, (7.2) an adduct of ethylene oxide with a C 6 -C 20 -alkylphenol or a C 8 -C 20 -alkanol, the adduct containing from 5 to 55 moles of ethylene oxide per mole of phenol or alkanol, (10) a mixture of the acidic phosphates stated under (4.2.b) with a C 10 -C 20 -alkylamine or a 3-(C 8 -C 20 -alkoxy)-propylamine, where the amino group may be substituted by one or two C 1 -C 4 -alkyl radicals, or (11) a mixture of a C 8 -C 20 -alkylbenzenesulfonic acid with a C 10 -C 20 -alkylamine or a 3-(C 8 -C 20 -alkoxy)-propylamine, where the amino group may be substituted by one or two C 1 -C 4 -alkyl radicals.

Claim 6

A process as claimed in claim 4, wherein the agents (1) to (11) are used in the form of a solution or suspension.

Claim 7

A process as claimed in claim 5, wherein the agents (1) to (11) are added to an aqueous suspension of the crude pigment, the mixture is heated to 50°-100° C. at pH 2-5 with thorough mixing, and the pigment is then isolated.

Claim 8

A pigment which consists of a basic dye converted to a lake with a heteropolyacid and is obtained by a process as claimed in claim 1.

Claim 9

A process for the preparation of a lake which has improved performance characteristics and is obtained from a basic dye and a heteropolyacid based on phosphoric acid, molybdic acid, tungstic acid and/or silicic acid by after-treating the crude pigment obtained during the laking procedure, in aqueous suspension and at elevated temperatures, wherein the crude pigment is heated to 50°-100° C. at pH 2-5 in the presence of from 10 to 45% by weight, based on the dye used for the laking procedure, of one or more compounds from the groups consisting of (1.1) C 10 -C 20 -alkylamines or 3-(C 8 -C 20 -alkoxy)-propylamines, where the N atoms of the amines may be monosubstituted or disubstituted by C 1 -C 4 -alkyl, (2.1) N-C 10 -C 20 -alkylamino-C 2 -C 8 -alkanoic acids, (4.1)(a) neutral phosphates based on C 3 -C 18 -alkanols, as a mixture with nonionic ethylene oxide adducts of group (7), (b) acidic phosphates based on adducts of ethylene oxide or of propylene oxide/ethylene oxide with C 10 -C 20 -alkanols, (5.1) sulfuric acid half esters of adducts of ethylene oxide with C 10 -C 20 -alkylphenols, the adducts containing on average from 2 to 6 moles of ethylene oxide per mole, (6.1) C 8 -C 20 -alkylbenzenesulfonic acids and (7.1) adducts of ethylene oxide with C 6 -C 20 -alkylphenols or C 8 -C 20 -alkanols, containing from 5 to 55 moles of ethylene oxide per mole of phenol or alkanol, and the pigment is then isolated.

Claim 10

A process for the preparation of a lake which has improved performance characteristics and is obtained from a basic dye and a heteropolyacid based on phosphoric acid, molybdic acid, tungstic acid and/or silicic acid by after-treating the crude pigment obtained during the laking procedure, in aqueous suspension and at elevated temperatures, wherein the crude pigment is heated to 50°-100° C. at pH 2-5 in the presence of from 10 to 45% by weight, based on the dye used for the laking procedure, of one or more compounds from the groups consisting of (1.1) C 10 -C 20 -alkylamines or 3-(C 8 -C 20 -alkoxy)-propylamines, where the N atoms of the amines may be monosubstituted or disubstituted by C 1 -C 4 -alkyl, (2.1) N-C 10 -C 20 -alkylamino-C 2 -C 8 -alkanoic acids, (4.1)(a) neutral phosphates based on C 3 -C 18 -alkanols, as a mixture with nonionic ethylene oxide adducts of group (7), (b) acidic phosphates based on adducts of ethylene oxide or of propylene oxide/ethylene oxide with C 10 -C 20 -alkanols, (5.1) sulfuric acid half esters of adducts of ethylene oxide with C 10 -C 20 -alkylphenols, the adducts containing on average from 2 to 6 moles of ethylene oxide per mole, (6.1) C 8 -C 20 -alkylbenzenesulfonic acids and (7.1) adducts of ethylene oxide with C 6 -C 20 -alkylphenols or C 8 -C 20 -alkanols, containing from 5 to 55 moles of ethylene oxide per mole of phenol or alkanol, and the pigment is then isolated.

Claim 11

A process as claimed in claim 8, wherein the heat-treatment of the crude pigment is carried out in the presence of (1.2) a C 14 -C 20 -alkylamine or a 3-(C 10 -C 20 -alkoxy)-propylamine, where the N atom may be substituted by one or two C 1 -C 4 -alkyl radicals, (2.2) a β-(N-C 10 -C 20 -alkylamino)-butyric acid, (4.2)(a) a neutral phosphate based on a C 3 -C 18 -alkanol, as a mixture with an adduct of ethylene oxide with a C 6 -C 20 -alkylphenol or a C 8 -C 20 -alkanol, containing from 5 to 55 moles of ethylene oxide per mole of phenol or alkanol, (4.2)(b) an acidic phosphate based on an adduct of ethylene oxide or of propylene oxide/ethylene oxide with a C 10 -C 20 -alkanol, (5.2) a sulfuric acid half ester of an adduct of ethylene oxide with a C 10 -C 20 -alkanol or a C 6 -C 20 -alkylphenol, the adduct containing on average from 2 to 6 moles of ethylene oxide per mole of alkanol or phenol, (6.2) a C 8 -C 20 -alkylbenzenesulfonic acid, (7.2) an adduct of ethylene oxide with a C 6 -C 20 -alkylphenol or a C 8 -C 20 -alkanol, the adduct containing from 5 to 55 moles of ethylene oxide per mole of phenol or alkanol, (10) a mixture of the acidic phosphates stated under (4.2.b.) with a C 10 -C 20 -alkylamine or a 3-(C 8 -C 20 -alkoxy)-propylamine, where the amino group may be substituted by one or two C 1 -C 4 -alkyl radicals, or (11) a mixture of a C 8 -C 20 -alkylbenzenesulfonic acid with a C 10 -C 20 -alkylamine or a 3-(C 8 -C 20 -alkoxy)-propylamine, where the amino group may be substituted by one or two C 1 -C 4 -alkyl radicals.

Claim 12

A process as claimed in claim 8, wherein the heat treatment is carried out in the presence of from 15 to 45% by weight, based on the basic dye used for the laking procedure, of the compounds stated under (1.1) to (7.1).

Claim 13

A process as claimed in claim 9, wherein the heat treatment is carried out in the presence of from 15 to 45% by weight, based on the basic dye used for the laking procedure, of the compounds stated under (1.1) to (7.1).

Claim 14

A process for the preparation of a lake which has improved performance characteristics and is obtained from a basic dye and a heteropolyacid based on phosphoric acid, molybdic acid, tungstic acid and/or silicic acid by after-treating the crude pigment obtained during the laking procedure, in aqueous suspension and at elevated temperatures, wherein the crude pigment is heated to 50°-100° C. at pH 2-5 in the presence of from 10 to 45% by weight, based on the basic dye used for the laking procedure, of one or more compounds from the groups consisting of (1.2) C 14 -C 20 -alkylamines or 3-(C 10 -C 20 -alkoxy)-propylamines, where the N atoms of the amines may carry one or two C 1 -C 4 -alkyl radicals, (2.2) N-C 10 -C 20 -alkylaminobutyric acids, (4.2)(a) neutral phosphates of C 3 -C 18 -alkanols, as a mixture with C 6 -C 20 -alkylphenol/ethylene oxide adducts or C 8 -C 20 -alkanol/ethylene oxide adducts, containing in each case from 5 to 55 moles of ethylene oxide per mole of phenol or alkanol, (4.2)(b) acidic phosphates of adducts of ethylene oxide or of propylene oxide/ethylene oxide with C 10 -C 20 -alkanols, (5.2) sulfuric acid half esters of adducts of ethylene oxide with C 10 -C 20 -alkanols or C 6 -C 20 -alkylphenols, the adducts containing on average from 2 to 6 moles of ethylene oxide per mole of alkanol or phenol, (6.2) C 8 -C 20 -alkylbenzenesulfonic acids, (7.2) adducts of ethylene oxide with C 6 -C 20 -alkylphenols or C 8 -C 20 -alkanols, the adducts containing from 5 to 55 moles of ethylene oxide per mole of alkylphenol or alkanol, (9.1) α-naphthol, β-naphthol, 3,4-dimethylphenol, hexylphenol, octylphenol, nonylphenol and dodecylphenol, and (10) mixtures of acidic phosphates of ethylene oxide/C 10 -C 20 -alkanol adducts or of propylene oxide/ethylene oxide/C 10 -C 20 -alkanol adducts with C 10 -C 20 -alkylamines, N-C 1 -C 4 -alkyl-N-C 10 -C 20 -alkylamines, di-N-C 1 -C 4 -alkyl-N-C 10 -C 20 -alkylamines, C 8 -C 18 -alkoxypropylamines or di-N,N-C 1 -C 4 -alkyl-N-C 8 -C 18 -alkoxypropylamines, and the pigment is then isolated.

Claim 15

A process for the preparation of a lake which has improved performance characteristics and is obtained from a basic dye and a heteropolyacid based on phosphoric acid, molybdic acid, tungstic acid and/or silicic acid by after-treating the crude pigment obtained during the laking procedure, in aqueous suspension and at elevated temperatures, wherein the crude pigment is heated to 50°-100° C. at pH 2-5 in the presence of from 10 to 45% by weight, based on the basic dye used for the laking procedure, of one or more compounds from the groups consisting of (1.2) C 14 -C 20 -alkylamines or 3-(C 10 -C 20 -alkoxy)-propylamines, where the N atoms of the amines may carry one or two C 1 -C 4 -alkyl radicals, (2.2) N-C 10 -C 20 -alkylaminobutyric acids, (4.2)(a) neutral phosphates of C 3 -C 18 -alkanols, as a mixture with C 6 -C 20 -alkylphenol/ethylene oxide adducts or C 8 -C 20 -alkanol/ethylene oxide adducts, containing in each case from 5 to 55 moles of ethylene oxide per mole of phenol or alkanol, (4.2)(b) acidic phosphates of adducts of ethylene oxide or of propylene oxide/ethylene oxide with C 10 -C 20 -alkanols, (5.2) sulfuric acid half esters of adducts of ethylene oxide with C 10 -C 20 -alkanols or C 6 -C 20 -alkylphenols, the adducts containing on average from 2 to 6 moles of ethylene oxide per mole of alkanol or phenol, (6.2) C 8 -C 20 -alkylbenzenesulfonic acids, (7.2) adducts of ethylene oxide with C 6 -C 20 -alkylphenols or C 8 -C 20 -alkanols, the adducts containing from 5 to 55 moles of ethylene oxide per mole of alkylphenol or alkanol, (9.1) α-naphthol, β-naphthol, 3,4-dimethylphenol, hexylphenol, octylphenol, nonylphenol and dodecylphenol, and (10) mixtures of acidic phosphates of ethylene oxide/C 10 -C 20 -alkanol adducts or of propylene oxide/ethylene oxide/C 10 -C 20 -alkanol adducts with C 10 -C 20 -alkylamines, N-C 1 -C 4 -alkyl-N-C 10 -C 20 -alkylamines, di-N-C 1 -C 4 -alkyl-N-C 10 -C 20 -alkylamines, C 8 -C 18 -alkoxypropylamines or di-N,N-C 1 -C 4 -alkyl-N-C 8 -C 18 -alkoxypropylamines, and the pigment is then isolated.

Claim 16

A process as claimed in claim 12, wherein the heat treatment is carried out at a pH of from 2.2 to 4.

Claim 17

A process as claimed in claim 12, wherein the heat treatment is carried out at from 75 to 95° C.

Claim 18

A process as claimed in claim 13, wherein the heat treatment is carried out at a pH of from 2.2 to 4.

Claim 19

A pigment which consists of a basic dye converted to a lake with a heteropolyacid and is obtained by a process as claimed in claim 12.