Composite form of tetraacetylenediamine
The present invention relates to a composite form of tetraacetylethylenediamine (TAED) and a method for its preparation. The composite form may comprise a new crystalline form. The invention also relates to the crystalline form itself. The present invention also relates to compositions comprising tetraacetylethylenediamine in these forms.
1 . A composite form of tetraacetylethylenediamine (TAED), said composite form comprising TAED and an ionic component, wherein said ionic component is a Deep Eutectic Solvent (DES).
2 . The composite form of claim 1 , wherein the TAED is in a crystalline form (form III), said crystalline form being characterised in that said form has an XRPD pattern having only two peaks at 2θ 9.1746±0.2 and 18.1788±0.2 when the crystalline form is dispersed in the ionic component and wherein the XRPD is measured using Cu radiation with a K α2 /K α1 ratio of 0.5.
3 . The composite form of claim 1 , wherein the composite form is a gel in which the TAED is the solid component and the ionic component is the liquid component.
4 . The composite form of claim 1 , wherein the composite form is a solid.
5 . The composite form of claim 4 wherein the solid composite form further comprises a solid surfactant.
6 . The composite form of claim 5 , wherein the surfactant is selected from: Cresylic acid, Denatonium benzoate, Potassium peroxomonosulphate (KMPS), Glycollic acid, Sodium peroxodisulphate (NPS), Surface modifying polymers, Sodium sulphate, Zinc ricinoleate, Ethylene glycol distearate, Alkyl Polypentosides (APPs), Alkylpolyglucosides (APGs), Amine oxides, Amphoacetates, Cocamide DEA and MEA, Cocoaminopropionate, Cocoamphodipropionate, Cocoiminodipropionate, Didecyl dimethyl ammonium carbonate/bicarbonate, Dodecyl Benzene Sulfonic Acid (DDBSA), MEA & TEA neutralised DDBSA, Ethoxylated fatty amines, Fluorinated surfactants, Octyliminodipropionate, OXO alcohol ethoxylates, PEG-7 glyceryl cocoate, Propoxylate/Ethoxylates, Silicone surfactants, Sodium C 14-16 Olefin Sulphonate (AOS), Sodium C 14-17 Alkyl Sec-Sulphonate (SAS), Sodium Laureth Sulphate (SLES), Sodium Lauryl Sulphate (SLS), Urea and mixtures thereof.
7 . The composite form of claim 4 wherein the composite form is a powder.
8 . The composite form of claim 1 , wherein the molar ratio of TAED to the ionic component is in the range 3:1 to 1:3.
9 . The composite form of claim 1 , wherein the DES is selected from choline chloride:lactic acid DES; proline:lactic acid DES; choline chloride:citric acid DES and propylene glycol:citric acid DES.
10 . The composite form of claim 1 , wherein the DES is propylene glycol:citric acid DES.
11 . A method of forming a composite form of TAED, the method comprising:
a) heating TAED with deep eutectic solvent (DES) forming components, a DES solvent (DES), an Ionic liquid (IL) or a mixture thereof to a temperature≥150° C.; and
b) allowing the mixture to cool to form the composite form of TAED.
12 . The method of claim 11 , wherein the eutectic solvent (DES) forming components, DES solvents (DES) or Ionic liquid (IL) are selected such that the product of step b) has a viscosity in the range from 5000 cP to 120000 cP.
13 . The method of claim 11 , wherein the heating step a) is optionally conducted in the presence of propylene glycol (1,2-Propylene Glycol), sodium tripolyphosphate, caustic soda, sulphonic acid, or mixtures thereof.
14 . The method of claim 11 , wherein the composite form formed in step b) is a gel and the method comprises step c): adding a solid surfactant to the product of b) to provide a composite form that is a solid.
15 . The method of claim 14 , wherein the solid surfactant is selected from: Cresylic acid, Denatonium benzoate, Potassium peroxomonosulphate (KMPS), Glycollic acid, Sodium peroxodisulphate (NPS), Surface modifying polymers, Sodium sulphate, Zinc ricinoleate, Ethylene glycol distearate, Alkyl Polypentosides (APPs), Alkylpolyglucosides (APGs), Amine oxides, Amphoacetates, Cocamide DEA and MEA, Cocoaminopropionate, Cocoamphodipropionate, Cocoiminodipropionate, Didecyl dimethyl ammonium carbonate/bicarbonate, Dodecyl Benzene Sulfonic Acid (DDBSA), MEA & TEA neutralised DDBSA, Ethoxylated fatty amines, Fluorinated surfactants, Octyliminodipropionate, OXO alcohol ethoxylates, PEG-7 glyceryl cocoate, Propoxylate/Ethoxylates, Silicone surfactants, Sodium C 14-16 Olefin Sulphonate (AOS), Sodium C 14-17 Alkyl Sec-Sulphonate (SAS), Sodium Laureth Sulphate (SLES), Sodium Lauryl Sulphate (SLS), Urea and mixtures thereof.
16 . A composite form of TAED characterised in that it is obtainable by the method of claim 11 .
17 . A composition comprising the composite form of TAED of claim 1 .
18 . The composition of claim 17 , wherein the composition is a solid composition.
19 . The composition of claim 18 , wherein the composition is a powder composition.
20 . The composition of claim 17 , wherein the composition comprises from 0.1% to 20% or 0.1 to 50% or more 75% by weight of the crystalline form of composite form of TAED.
21 . The composition of claim 17 , wherein the composition further comprises a bleaching agent.
22 . The composition of claim 17 , wherein the composition further comprises at least one of a surfactant or wetting agent.
23 . The composition of claim 17 , wherein the composition further comprises at least one of an additive selected from the group consisting of a pH modifier, a chelating agent, a stabilising agent, a diluent, a glidant, a binding agent, an effervescing agent, a disintegrating agent and a coating agent.
24 . A crystalline form of TAED (form III), said crystalline form being characterised in that said form has an XRPD pattern having only two peaks at 2θ 9.1746±0.2 and 18.1788±0.2 when the crystalline form is dispersed in a DES solvent (DES), an Ionic liquid (IL) and wherein the XRPD is measured using Cu radiation with a K α2 /K α1 ratio of 0.5.