EP3894532A1 - An encapsulated dye composition and a method for preparation thereof - Google Patents
An encapsulated dye composition and a method for preparation thereofInfo
- Publication number
- EP3894532A1 EP3894532A1 EP19812786.2A EP19812786A EP3894532A1 EP 3894532 A1 EP3894532 A1 EP 3894532A1 EP 19812786 A EP19812786 A EP 19812786A EP 3894532 A1 EP3894532 A1 EP 3894532A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- dye
- composition
- clay
- silica
- mixture
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000000203 mixture Substances 0.000 title claims abstract description 320
- 238000000034 method Methods 0.000 title claims abstract description 71
- 238000002360 preparation method Methods 0.000 title abstract description 24
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 300
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 125
- 239000004927 clay Substances 0.000 claims abstract description 97
- 239000011230 binding agent Substances 0.000 claims abstract description 26
- 239000000975 dye Substances 0.000 claims description 243
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 58
- 239000000843 powder Substances 0.000 claims description 45
- 239000002245 particle Substances 0.000 claims description 35
- IHZXTIBMKNSJCJ-UHFFFAOYSA-N 3-{[(4-{[4-(dimethylamino)phenyl](4-{ethyl[(3-sulfophenyl)methyl]amino}phenyl)methylidene}cyclohexa-2,5-dien-1-ylidene)(ethyl)azaniumyl]methyl}benzene-1-sulfonate Chemical compound C=1C=C(C(=C2C=CC(C=C2)=[N+](C)C)C=2C=CC(=CC=2)N(CC)CC=2C=C(C=CC=2)S([O-])(=O)=O)C=CC=1N(CC)CC1=CC=CC(S(O)(=O)=O)=C1 IHZXTIBMKNSJCJ-UHFFFAOYSA-N 0.000 claims description 32
- -1 kerolite Inorganic materials 0.000 claims description 32
- 239000000463 material Substances 0.000 claims description 31
- 238000002156 mixing Methods 0.000 claims description 27
- 229910000278 bentonite Inorganic materials 0.000 claims description 23
- 239000000440 bentonite Substances 0.000 claims description 23
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 claims description 23
- 239000003599 detergent Substances 0.000 claims description 23
- 239000008187 granular material Substances 0.000 claims description 19
- 229920003088 hydroxypropyl methyl cellulose Polymers 0.000 claims description 19
- 239000011148 porous material Substances 0.000 claims description 17
- 230000002209 hydrophobic effect Effects 0.000 claims description 16
- 230000008569 process Effects 0.000 claims description 15
- 229910052906 cristobalite Inorganic materials 0.000 claims description 13
- 229910052500 inorganic mineral Inorganic materials 0.000 claims description 13
- 239000011707 mineral Substances 0.000 claims description 13
- 229910052681 coesite Inorganic materials 0.000 claims description 12
- 229910052682 stishovite Inorganic materials 0.000 claims description 12
- 229910052905 tridymite Inorganic materials 0.000 claims description 12
- 238000002441 X-ray diffraction Methods 0.000 claims description 11
- 229920000642 polymer Polymers 0.000 claims description 10
- 239000004094 surface-active agent Substances 0.000 claims description 7
- 238000005341 cation exchange Methods 0.000 claims description 6
- GUJOJGAPFQRJSV-UHFFFAOYSA-N dialuminum;dioxosilane;oxygen(2-);hydrate Chemical compound O.[O-2].[O-2].[O-2].[Al+3].[Al+3].O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O GUJOJGAPFQRJSV-UHFFFAOYSA-N 0.000 claims description 6
- 229910052901 montmorillonite Inorganic materials 0.000 claims description 6
- 229910000275 saponite Inorganic materials 0.000 claims description 6
- 238000010521 absorption reaction Methods 0.000 claims description 5
- 239000006185 dispersion Substances 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 5
- 239000011734 sodium Substances 0.000 claims description 5
- 229910052708 sodium Inorganic materials 0.000 claims description 5
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 4
- 238000000576 coating method Methods 0.000 claims description 4
- 229910052710 silicon Inorganic materials 0.000 claims description 4
- 239000010703 silicon Substances 0.000 claims description 4
- UWOFGIXNNCPENM-UHFFFAOYSA-N 3,3-difluoropentan-2-one Chemical compound CCC(F)(F)C(C)=O UWOFGIXNNCPENM-UHFFFAOYSA-N 0.000 claims description 3
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 claims description 3
- 239000004113 Sepiolite Substances 0.000 claims description 3
- 125000000129 anionic group Chemical group 0.000 claims description 3
- VNSBYDPZHCQWNB-UHFFFAOYSA-N calcium;aluminum;dioxido(oxo)silane;sodium;hydrate Chemical compound O.[Na].[Al].[Ca+2].[O-][Si]([O-])=O VNSBYDPZHCQWNB-UHFFFAOYSA-N 0.000 claims description 3
- 125000002091 cationic group Chemical group 0.000 claims description 3
- 239000011248 coating agent Substances 0.000 claims description 3
- VVIVVAIHOWVTHB-UHFFFAOYSA-L disodium;3-[[4-amino-9,10-dioxo-3-[2-sulfonato-4-(2,4,4-trimethylpentan-2-yl)phenoxy]anthracen-1-yl]amino]-2,4,6-trimethylbenzenesulfonate Chemical compound [Na+].[Na+].CC1=CC(C)=C(S([O-])(=O)=O)C(C)=C1NC1=CC(OC=2C(=CC(=CC=2)C(C)(C)CC(C)(C)C)S([O-])(=O)=O)=C(N)C2=C1C(=O)C1=CC=CC=C1C2=O VVIVVAIHOWVTHB-UHFFFAOYSA-L 0.000 claims description 3
- 229910000271 hectorite Inorganic materials 0.000 claims description 3
- KWLMIXQRALPRBC-UHFFFAOYSA-L hectorite Chemical compound [Li+].[OH-].[OH-].[Na+].[Mg+2].O1[Si]2([O-])O[Si]1([O-])O[Si]([O-])(O1)O[Si]1([O-])O2 KWLMIXQRALPRBC-UHFFFAOYSA-L 0.000 claims description 3
- 229910052624 sepiolite Inorganic materials 0.000 claims description 3
- 235000019355 sepiolite Nutrition 0.000 claims description 3
- 229910002027 silica gel Inorganic materials 0.000 claims description 3
- 239000000741 silica gel Substances 0.000 claims description 3
- FJBHGWADYLMEJG-UHFFFAOYSA-M sodium;3-[[4-[[4-(diethylamino)phenyl]-[4-[ethyl-[(3-sulfonatophenyl)methyl]azaniumylidene]cyclohexa-2,5-dien-1-ylidene]methyl]-n-ethylanilino]methyl]benzenesulfonate Chemical compound [Na+].C1=CC(N(CC)CC)=CC=C1C(C=1C=CC(=CC=1)N(CC)CC=1C=C(C=CC=1)S([O-])(=O)=O)=C(C=C1)C=CC1=[N+](CC)CC1=CC=CC(S([O-])(=O)=O)=C1 FJBHGWADYLMEJG-UHFFFAOYSA-M 0.000 claims description 3
- 239000001003 triarylmethane dye Substances 0.000 claims description 3
- VEPOHXYIFQMVHW-XOZOLZJESA-N 2,3-dihydroxybutanedioic acid (2S,3S)-3,4-dimethyl-2-phenylmorpholine Chemical compound OC(C(O)C(O)=O)C(O)=O.C[C@H]1[C@@H](OCCN1C)c1ccccc1 VEPOHXYIFQMVHW-XOZOLZJESA-N 0.000 claims description 2
- PCNDJXKNXGMECE-UHFFFAOYSA-N Phenazine Natural products C1=CC=CC2=NC3=CC=CC=C3N=C21 PCNDJXKNXGMECE-UHFFFAOYSA-N 0.000 claims description 2
- 239000001000 anthraquinone dye Substances 0.000 claims description 2
- 229960000892 attapulgite Drugs 0.000 claims description 2
- 239000000987 azo dye Substances 0.000 claims description 2
- 125000000664 diazo group Chemical group [N-]=[N+]=[*] 0.000 claims description 2
- 229910021485 fumed silica Inorganic materials 0.000 claims description 2
- 125000001434 methanylylidene group Chemical group [H]C#[*] 0.000 claims description 2
- 229910052625 palygorskite Inorganic materials 0.000 claims description 2
- 239000001007 phthalocyanine dye Substances 0.000 claims description 2
- 229910052903 pyrophyllite Inorganic materials 0.000 claims description 2
- IZMJMCDDWKSTTK-UHFFFAOYSA-N quinoline yellow Chemical compound C1=CC=CC2=NC(C3C(C4=CC=CC=C4C3=O)=O)=CC=C21 IZMJMCDDWKSTTK-UHFFFAOYSA-N 0.000 claims description 2
- 239000000454 talc Substances 0.000 claims description 2
- 229910052623 talc Inorganic materials 0.000 claims description 2
- AAAQKTZKLRYKHR-UHFFFAOYSA-N triphenylmethane Chemical compound C1=CC=CC=C1C(C=1C=CC=CC=1)C1=CC=CC=C1 AAAQKTZKLRYKHR-UHFFFAOYSA-N 0.000 claims description 2
- 230000000740 bleeding effect Effects 0.000 abstract description 6
- 238000009472 formulation Methods 0.000 description 41
- 239000002734 clay mineral Substances 0.000 description 34
- 235000012239 silicon dioxide Nutrition 0.000 description 32
- 239000012071 phase Substances 0.000 description 27
- 235000012216 bentonite Nutrition 0.000 description 22
- 229940092782 bentonite Drugs 0.000 description 21
- 239000004744 fabric Substances 0.000 description 20
- 229910021647 smectite Inorganic materials 0.000 description 20
- 238000003756 stirring Methods 0.000 description 16
- 238000005538 encapsulation Methods 0.000 description 15
- 238000003860 storage Methods 0.000 description 15
- 238000012360 testing method Methods 0.000 description 15
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 14
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 11
- 239000011159 matrix material Substances 0.000 description 11
- 239000000243 solution Substances 0.000 description 11
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 10
- 230000000052 comparative effect Effects 0.000 description 10
- 239000012153 distilled water Substances 0.000 description 10
- CXKWCBBOMKCUKX-UHFFFAOYSA-M methylene blue Chemical compound [Cl-].C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 CXKWCBBOMKCUKX-UHFFFAOYSA-M 0.000 description 8
- 229960000907 methylthioninium chloride Drugs 0.000 description 8
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 7
- 238000004458 analytical method Methods 0.000 description 7
- 229910052697 platinum Inorganic materials 0.000 description 7
- 238000005406 washing Methods 0.000 description 7
- 229910000281 calcium bentonite Inorganic materials 0.000 description 6
- 150000001875 compounds Chemical class 0.000 description 6
- 125000000217 alkyl group Chemical group 0.000 description 5
- 229910052742 iron Inorganic materials 0.000 description 5
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 4
- 239000004372 Polyvinyl alcohol Substances 0.000 description 4
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 4
- 239000002253 acid Substances 0.000 description 4
- 239000004411 aluminium Substances 0.000 description 4
- 229910052782 aluminium Inorganic materials 0.000 description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 4
- SAOKZLXYCUGLFA-UHFFFAOYSA-N bis(2-ethylhexyl) adipate Chemical compound CCCCC(CC)COC(=O)CCCCC(=O)OCC(CC)CCCC SAOKZLXYCUGLFA-UHFFFAOYSA-N 0.000 description 4
- 238000009835 boiling Methods 0.000 description 4
- 235000014113 dietary fatty acids Nutrition 0.000 description 4
- 239000000194 fatty acid Substances 0.000 description 4
- 229930195729 fatty acid Natural products 0.000 description 4
- KWIUHFFTVRNATP-UHFFFAOYSA-N glycine betaine Chemical compound C[N+](C)(C)CC([O-])=O KWIUHFFTVRNATP-UHFFFAOYSA-N 0.000 description 4
- 239000011777 magnesium Substances 0.000 description 4
- 229910052749 magnesium Inorganic materials 0.000 description 4
- 229920002689 polyvinyl acetate Polymers 0.000 description 4
- 239000011118 polyvinyl acetate Substances 0.000 description 4
- 229920002451 polyvinyl alcohol Polymers 0.000 description 4
- 230000011514 reflex Effects 0.000 description 4
- 238000010186 staining Methods 0.000 description 4
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 3
- 239000011575 calcium Substances 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 239000001177 diphosphate Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 150000004665 fatty acids Chemical class 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 229920003229 poly(methyl methacrylate) Polymers 0.000 description 3
- 239000004926 polymethyl methacrylate Substances 0.000 description 3
- 238000012216 screening Methods 0.000 description 3
- 239000013049 sediment Substances 0.000 description 3
- FQENQNTWSFEDLI-UHFFFAOYSA-J sodium diphosphate Chemical compound [Na+].[Na+].[Na+].[Na+].[O-]P([O-])(=O)OP([O-])([O-])=O FQENQNTWSFEDLI-UHFFFAOYSA-J 0.000 description 3
- 238000001179 sorption measurement Methods 0.000 description 3
- 235000019818 tetrasodium diphosphate Nutrition 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 238000004438 BET method Methods 0.000 description 2
- 229910021532 Calcite Inorganic materials 0.000 description 2
- 229920002134 Carboxymethyl cellulose Polymers 0.000 description 2
- ROSDSFDQCJNGOL-UHFFFAOYSA-N Dimethylamine Chemical compound CNC ROSDSFDQCJNGOL-UHFFFAOYSA-N 0.000 description 2
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 2
- 206010027146 Melanoderma Diseases 0.000 description 2
- 229910019142 PO4 Inorganic materials 0.000 description 2
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 2
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 2
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 239000003463 adsorbent Substances 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 239000002280 amphoteric surfactant Substances 0.000 description 2
- 239000003945 anionic surfactant Substances 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 239000011324 bead Substances 0.000 description 2
- 229960003237 betaine Drugs 0.000 description 2
- 238000004061 bleaching Methods 0.000 description 2
- 229910052791 calcium Inorganic materials 0.000 description 2
- 239000003093 cationic surfactant Substances 0.000 description 2
- 238000012512 characterization method Methods 0.000 description 2
- 239000003086 colorant Substances 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- ONCZQWJXONKSMM-UHFFFAOYSA-N dialuminum;disodium;oxygen(2-);silicon(4+);hydrate Chemical compound O.[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[Na+].[Na+].[Al+3].[Al+3].[Si+4].[Si+4].[Si+4].[Si+4] ONCZQWJXONKSMM-UHFFFAOYSA-N 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 239000010433 feldspar Substances 0.000 description 2
- 239000012065 filter cake Substances 0.000 description 2
- 239000000706 filtrate Substances 0.000 description 2
- 239000004615 ingredient Substances 0.000 description 2
- 238000004900 laundering Methods 0.000 description 2
- 229910052744 lithium Inorganic materials 0.000 description 2
- 229910044991 metal oxide Inorganic materials 0.000 description 2
- 150000004706 metal oxides Chemical class 0.000 description 2
- 238000013508 migration Methods 0.000 description 2
- 230000005012 migration Effects 0.000 description 2
- 239000002736 nonionic surfactant Substances 0.000 description 2
- 210000002741 palatine tonsil Anatomy 0.000 description 2
- 235000021317 phosphate Nutrition 0.000 description 2
- 239000011591 potassium Substances 0.000 description 2
- 229910052700 potassium Inorganic materials 0.000 description 2
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 description 2
- 239000010453 quartz Substances 0.000 description 2
- 229910000280 sodium bentonite Inorganic materials 0.000 description 2
- 229940080314 sodium bentonite Drugs 0.000 description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 description 2
- 239000011780 sodium chloride Substances 0.000 description 2
- 229910052938 sodium sulfate Inorganic materials 0.000 description 2
- 235000011152 sodium sulphate Nutrition 0.000 description 2
- 238000013112 stability test Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 235000011149 sulphuric acid Nutrition 0.000 description 2
- UIJMHOVIUFGSNF-UHFFFAOYSA-N 2-[dimethyl-[3-(undec-10-enoylamino)propyl]azaniumyl]acetate Chemical compound [O-]C(=O)C[N+](C)(C)CCCNC(=O)CCCCCCCCC=C UIJMHOVIUFGSNF-UHFFFAOYSA-N 0.000 description 1
- YJHSJERLYWNLQL-UHFFFAOYSA-N 2-hydroxyethyl(dimethyl)azanium;chloride Chemical compound Cl.CN(C)CCO YJHSJERLYWNLQL-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- 102000008186 Collagen Human genes 0.000 description 1
- 108010035532 Collagen Proteins 0.000 description 1
- 229920000742 Cotton Polymers 0.000 description 1
- 239000004677 Nylon Substances 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- 229920000388 Polyphosphate Polymers 0.000 description 1
- 238000003991 Rietveld refinement Methods 0.000 description 1
- 239000004115 Sodium Silicate Substances 0.000 description 1
- 229920002334 Spandex Polymers 0.000 description 1
- VBIIFPGSPJYLRR-UHFFFAOYSA-M Stearyltrimethylammonium chloride Chemical compound [Cl-].CCCCCCCCCCCCCCCCCC[N+](C)(C)C VBIIFPGSPJYLRR-UHFFFAOYSA-M 0.000 description 1
- ULUAUXLGCMPNKK-UHFFFAOYSA-N Sulfobutanedioic acid Chemical class OC(=O)CC(C(O)=O)S(O)(=O)=O ULUAUXLGCMPNKK-UHFFFAOYSA-N 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 125000002252 acyl group Chemical group 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 150000001343 alkyl silanes Chemical class 0.000 description 1
- 150000008051 alkyl sulfates Chemical class 0.000 description 1
- DLHONNLASJQAHX-UHFFFAOYSA-N aluminum;potassium;oxygen(2-);silicon(4+) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[Al+3].[Si+4].[Si+4].[Si+4].[K+] DLHONNLASJQAHX-UHFFFAOYSA-N 0.000 description 1
- 150000001413 amino acids Chemical group 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 238000010009 beating Methods 0.000 description 1
- YSJGOMATDFSEED-UHFFFAOYSA-M behentrimonium chloride Chemical compound [Cl-].CCCCCCCCCCCCCCCCCCCCCC[N+](C)(C)C YSJGOMATDFSEED-UHFFFAOYSA-M 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000001768 carboxy methyl cellulose Substances 0.000 description 1
- 235000010948 carboxy methyl cellulose Nutrition 0.000 description 1
- 125000002057 carboxymethyl group Chemical group [H]OC(=O)C([H])([H])[*] 0.000 description 1
- 239000008112 carboxymethyl-cellulose Substances 0.000 description 1
- 229940105329 carboxymethylcellulose Drugs 0.000 description 1
- 239000012876 carrier material Substances 0.000 description 1
- WOWHHFRSBJGXCM-UHFFFAOYSA-M cetyltrimethylammonium chloride Chemical compound [Cl-].CCCCCCCCCCCCCCCC[N+](C)(C)C WOWHHFRSBJGXCM-UHFFFAOYSA-M 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 229920001688 coating polymer Polymers 0.000 description 1
- 229920001436 collagen Polymers 0.000 description 1
- 238000005056 compaction Methods 0.000 description 1
- 238000004590 computer program Methods 0.000 description 1
- 230000003750 conditioning effect Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- IQDGSYLLQPDQDV-UHFFFAOYSA-N dimethylazanium;chloride Chemical compound Cl.CNC IQDGSYLLQPDQDV-UHFFFAOYSA-N 0.000 description 1
- REZZEXDLIUJMMS-UHFFFAOYSA-M dimethyldioctadecylammonium chloride Chemical compound [Cl-].CCCCCCCCCCCCCCCCCC[N+](C)(C)CCCCCCCCCCCCCCCCCC REZZEXDLIUJMMS-UHFFFAOYSA-M 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 239000004664 distearyldimethylammonium chloride (DHTDMAC) Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 238000000705 flame atomic absorption spectrometry Methods 0.000 description 1
- 230000009969 flowable effect Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 125000005456 glyceride group Chemical group 0.000 description 1
- 150000002334 glycols Chemical class 0.000 description 1
- 238000005469 granulation Methods 0.000 description 1
- 230000003179 granulation Effects 0.000 description 1
- 230000005661 hydrophobic surface Effects 0.000 description 1
- 239000001866 hydroxypropyl methyl cellulose Substances 0.000 description 1
- 235000010979 hydroxypropyl methyl cellulose Nutrition 0.000 description 1
- UFVKGYZPFZQRLF-UHFFFAOYSA-N hydroxypropyl methyl cellulose Chemical compound OC1C(O)C(OC)OC(CO)C1OC1C(O)C(O)C(OC2C(C(O)C(OC3C(C(O)C(O)C(CO)O3)O)C(CO)O2)O)C(CO)O1 UFVKGYZPFZQRLF-UHFFFAOYSA-N 0.000 description 1
- 230000003116 impacting effect Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000010348 incorporation Methods 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 239000011872 intimate mixture Substances 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- SUMDYPCJJOFFON-UHFFFAOYSA-N isethionic acid Chemical class OCCS(O)(=O)=O SUMDYPCJJOFFON-UHFFFAOYSA-N 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- HOVAGTYPODGVJG-UHFFFAOYSA-N methyl beta-galactoside Natural products COC1OC(CO)C(O)C(O)C1O HOVAGTYPODGVJG-UHFFFAOYSA-N 0.000 description 1
- 239000004570 mortar (masonry) Substances 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 229920001778 nylon Polymers 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 229910052652 orthoclase Inorganic materials 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 229910052655 plagioclase feldspar Inorganic materials 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 239000001205 polyphosphate Substances 0.000 description 1
- 235000011176 polyphosphates Nutrition 0.000 description 1
- 229920000136 polysorbate Polymers 0.000 description 1
- 229910000027 potassium carbonate Inorganic materials 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
- 238000011158 quantitative evaluation Methods 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 238000010058 rubber compounding Methods 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 150000004760 silicates Chemical class 0.000 description 1
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 1
- 229910052911 sodium silicate Inorganic materials 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000004611 spectroscopical analysis Methods 0.000 description 1
- 239000012798 spherical particle Substances 0.000 description 1
- 150000003871 sulfonates Chemical class 0.000 description 1
- 239000001117 sulphuric acid Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 239000003760 tallow Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 230000008719 thickening Effects 0.000 description 1
- SOBHUZYZLFQYFK-UHFFFAOYSA-K trisodium;hydroxy-[[phosphonatomethyl(phosphonomethyl)amino]methyl]phosphinate Chemical compound [Na+].[Na+].[Na+].OP(O)(=O)CN(CP(O)([O-])=O)CP([O-])([O-])=O SOBHUZYZLFQYFK-UHFFFAOYSA-K 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/40—Dyes ; Pigments
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D17/00—Detergent materials or soaps characterised by their shape or physical properties
- C11D17/0039—Coated compositions or coated components in the compositions, (micro)capsules
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D17/00—Detergent materials or soaps characterised by their shape or physical properties
- C11D17/06—Powder; Flakes; Free-flowing mixtures; Sheets
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/02—Inorganic compounds ; Elemental compounds
- C11D3/12—Water-insoluble compounds
- C11D3/124—Silicon containing, e.g. silica, silex, quartz or glass beads
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/02—Inorganic compounds ; Elemental compounds
- C11D3/12—Water-insoluble compounds
- C11D3/124—Silicon containing, e.g. silica, silex, quartz or glass beads
- C11D3/1246—Silicates, e.g. diatomaceous earth
- C11D3/1253—Layer silicates, e.g. talcum, kaolin, clay, bentonite, smectite, montmorillonite, hectorite or attapulgite
- C11D3/126—Layer silicates, e.g. talcum, kaolin, clay, bentonite, smectite, montmorillonite, hectorite or attapulgite in solid compositions
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
- C11D7/02—Inorganic compounds
- C11D7/20—Water-insoluble oxides
Definitions
- the present invention relates to an encapsulated dye composition for detergent powder.
- the present invention relates to non-bleeding dye composition encapsulated in a carrier, method for the preparation of said encapsulated dye composition and detergent compositions comprising the same.
- the colored particles used in the detergent powder mostly comprise of the colorant such as dye.
- the use of dye stuff as colored material is associated with flaws. Conventionally used colored particles tend to bleed the dye in the detergent powder and therefore tend to convert the colour of the white powder. This may affect the customer base for that particular detergent powder.
- the dye gets stuck in the fabric and does not shed off the fabric thereby affecting the fabrics.
- US-20110053823 discloses colored speckles comprising a porous material, a releasing agent, and a dye. This patent describes the colored speckles which quickly release color from the porous carrier using releasing agent and provide desirable color to the wash water.
- the releasing agent is selected from the group consisting of salt compounds, sugar compounds, alkoxylated aromatic
- WO-0210327 discloses colored speckles comprising sodium chloride and colorant. It discloses presence of significant amount of hygroscopic material i.e. sodium chloride (at least 90%) in the matrix. This could cause the bleeding of dye in powder detergent under humidity in storage.
- the present disclosure provides the encapsulated dye composition that does not bleed in the detergent powder and shed off the fabric easily during washing.
- an encapsulated dye composition comprising a dye, a carrier consisting of a mixture of silica and clay and optionally a binder.
- the present invention provides methods for the preparation of the encapsulated dye composition.
- the present invention provides a detergent
- composition comprising encapsulated dye composition of the present invention.
- the present invention provides a method of laundering fabrics which includes a step of treating the fabrics with encapsulated dye composition of present invention.
- Weight percentages are calculated based upon total weight of the composition, unless otherwise indicated.
- an encapsulated dye composition comprising:
- a carrier material consisting of a mixture of silica and clay
- the encapsulated composition of the present invention further comprises a binder such as a surfactant or a polymer.
- Suitable surfactant includes nonionic, anionic, cationic or amphoteric surfactants.
- suitable nonionic surfactants are polyoxyethylene sorbitan esters, polyoxyethylene sorbitol esters, polyoxyalkylene fatty alcohol ethers, polyoxyalkylene fatty acid esters, alkoxylated glycerides, polyoxyethylene methyl glucoside ester, alkyl polyglucosides, EO-PO
- anionic surfactants are sulfonates of alkylbenzene-sulfonates, alkanesulfonates, olefinsulfonates, alkyl ether sulfate, alkyl sulfate, sulfo- succinates, alkyl phosphates, alkyl ether phosphates, protein fatty acid
- condensates perferably collagen hydrolysates modified with fatty acid, amino acid-based surfactants, isethionates, taurides, acyl lactylates, neutralized fatty acids or combinations of two or more thereof.
- cationic surfactants are esterquats, ditallow dimethyl ammonium chloride, C12/14 alkyl dimethyl benzyl ammonium chloride, alkyl dimethyl benzil ammonium chloride, cetyl trimethyl ammonium chloride, stearyl trimethyl ammonium chloride, behenyl trimethyl ammonium chloride alkyl hydroxyethyl dimethyl ammonium chloride, distearyl dimethyl ammonium chloride,
- amphoteric surfactants are alkyl amphoacetate, alkyl amidopropyl betaine, alkyl amidopropyl dimethylamine betaine, undecylenamidopropyl betaine, alkyl dimethyl amine oxide.
- polymers examples include cellulosic polymers such as hydroxyl propyl methyl cellulose (HPMC), carboxy methyl cellulose (CMC); polyvinyl alcohol (PVA) polymers:polyvinyl acetate (PVAc) polymer and any combinations thereof.
- HPMC hydroxyl propyl methyl cellulose
- CMC carboxy methyl cellulose
- PVA polyvinyl alcohol
- PVAc polyvinyl acetate
- T1O2 dispersion may be added to enhance whiteness.
- the binder is hydroxyl propyl methyl cellulose (HPMC).
- the dye is selected from the group consisting of azine dye for example anionic azine dye, cationic phenazine dye; triarylmethane dyes for example triphenyl-methane dye; anthraquinone dye; azo dye, disazo dye; phthalocyanine dye; quinophthalone dye; methine dye;
- azine dye for example anionic azine dye, cationic phenazine dye
- triarylmethane dyes for example triphenyl-methane dye
- anthraquinone dye azo dye, disazo dye
- phthalocyanine dye quinophthalone dye
- methine dye methine dye
- hemicyanine dye azo/azomethine complex dye
- triphendioxazine dye or a mixture thereof azo/azomethine complex dye
- the dye is selected from the group consisting of Duasyn Acid Violet 4BN-IN (C.l. Acid Violet 17), Duasyn Violet SP-IN (C.l. Direct Violet 66), Duasyn Red N-6B-IN (C.l. Acid Violet 54), Duasyn Violet FBL-IN (C.l. Acid Violet 48), Duasyn Red Violet E2R-IN (C.l. Acid Violet 126) or mixtures of one or several of the afore mentioned dyes.
- Duasyn Acid Violet 4BN-IN C.l. Acid Violet 17
- Duasyn Violet SP-IN C.l. Direct Violet 66
- Duasyn Red N-6B-IN C.l. Acid Violet 54
- Duasyn Violet FBL-IN C.l. Acid Violet 48
- Duasyn Red Violet E2R-IN C.l. Acid Violet 126) or mixtures of one or several of the afore mentioned dyes.
- the silica is at least one selected from a silica gel, pyrogenic silica and precipitated silica.
- the precipitated silica is hydrophilic precipitated silica, hydrophobic precipitated silica or a mixture of both.
- Precipitated silica is typically produced by a precipitation of a sodium silicate with a mineral acid under neutral or slightly alkaline conditions.
- the filter cake of precipitated silica is dried and ground.
- Hydrophilic silica adsorbs water around the dye and hydrophobic silica does not allow water to get into touch with dye.
- the silica is hydrophilic precipitated silica.
- hydrophilic silica only consists of S1O2 and does not exhibit any surface modification and is wettable by water.
- the hydrophilic silica has a particle size d50 determined by laser diffraction of at least 50 pm, preferably at least 70 pm, mostly preferred at least 90 pm.
- the precipitated silica is selected from the group consisting of Sipernat ® 22;
- the precipitated silica of the inventive formulation is characterized by a high liquid absorption capacity, determined as DOA absorption number of at least 120 ml/100g, preferably at least 140 ml/100g, mostly preferred at least 160 ml/100g precipitated silica.
- DOA is the abbreviation for di-(2-ethylhexyl) adipate (CAS-number 103-23-1 ).
- the test method is based on ISO 19246 (“Rubber compounding ingredients- Silica - Oil absorption of precipitated silica”).
- Hydrophobic silica is not wettable by water and exhibits an organic surface modification created by chemical reactions with reactive alkylsilanes. The existence of such a surface modification can be proven by various analytical methods, e.g. the carbon content in an elemental analyzer following ISO 3262-19.
- the precipitated silica or one of the precipitated silica used in the formulations has a hydrophobic surface.
- the hydrophobic precipitated silica for the inventive formulation is characterized by a particle size d50 determined by laser diffraction (laser diffraction based on ISO 13320) of at least 5 pm, preferably at least 7 pm, mostly preferred at least 9 pm.
- hydrophilic silica is Sipernat ® D17 (d50 ⁇ 10 micron) or Sipernat ® D10 (particle size -d50 ⁇ 6.5 micron, free flowable) or combinations thereof.
- clay refers to both natural clays as well as modified clays. Modified clays in this context refers to natural clays which have been alkaline-activated or acid-activated. As used herein, the terms“clay minerals’ or “special clay minerals” refer to natural clays.
- the clay used in the present composition is selected from the group consisting of natural clays comprising bentonite, montmorillonite, beidellite, saponite, hectorite, stevensite, kerolite-saponite, kerolite, talc, pyrophyllite, attapulgite, sepiolite; a mixture of natural silica with a bentonite;any modified clays; and any mixtures thereof.
- the clay is bentonite.
- an encapsulated dye composition comprising:
- a carrier consisting of a mixture of silica and clay
- the dye is used in the amount in the range of 1 % to 30%, based on the total weight of the encapsulated dye composition, preferably 5% to 20%.
- the binder is used in the amount of 1 to 5% based on the total weight of the encapsulated dye composition.
- the silica is used in the amount of 30% to 75% based on the total weight of the encapsulated dye composition.
- the clay is used in the amount of 30% to 75 % based on the total weight of the encapsulated dye composition.
- the carrier has a silica to clay ratio of 1 :4 to 4:1.
- composition comprising:
- a carrier comprising 30% to 75% by weight of silica and 30% to 75% by weight of clay
- the clay consisting of a smectite like a bentonite, beidellite, saponite, hectorite, stevensite, kerolite-saponite,is employed in the natural Ca-form or in a soda activated form.
- natural sodium bentonite is used as clay.
- Especially preferred clays are montmorillonites in the natural or soda activated form or mixtures thereof.
- the clay used is bentonite having cation exchange capacity in the range of 10 meq/100 g to 140 meq/100g.
- the clay used is bentonite having cation exchange capacity in the range of 20 meq/100 g to 130 meq/100g, preferably between 30 meq/100 g to 120 meq/100 g.
- a special clay mineral which consists of a mixture of smectite clay and an amorphous silica phase.
- the clay material is homogenous on a macroscopic scale, i.e.it is an intimate mixture of both phases.
- the special clay mineral used has a very high silicon content which is well above the silicon content of e.g. bentonite.
- the clay mineral does not have such a well ordered structure as layered silicates, e.g. bentonite, but preferably comprises large amounts of amorphous material. Such amorphous material is believed to be formed by amorphous S1O2.
- the special clay mineral of the present invention comprises a continuous phase of amorphous silica into which are inserted small platelet-shaped smectite phases.
- the platelets of the smectite phase are homogeneously distributed in the continuous amorphous silica phase and are firmly fixed therein.
- the special clay mineral of the present invention comprises a matrix-like network of amorphous S1O2 into which very small clay particles are inserted and which may provide good protection of the dye to be encapsulated.
- the clay mineral of the present invention has a very high surface area in the range of 180 to 300 m 2 /g, preferably 185 to 280 m 2 /g, and more preferably 190 to 250 m 2 /g as determined by the BET method.
- the clay mineral of the present invention has high total pore volume of more than 0.5 ml/g.
- the clay mineral of the present invention has total pore volume of more than 0.55 ml/g, preferably more than 0.6 ml/g.
- the special clay mineral comprises a matrix of amorphous S1O2 into which are inserted small particles of smectite minerals.
- the smectite particles are delaminated to a high degree and therefore provide a very high surface area.
- the clay mineral used comprise a rigid, amorphous S1O2 matrix into which are inserted very small clay particles or platelets.
- the clay mineral used in the method according to the invention comprises an amorphous phase of at least 10 wt.% of the total clay mineral, preferably at least 20 wt.%, more preferably at least 30 wt.% .
- the amorphous phase forms less than 90 wt.% of the total clay mineral.
- the amorphous phase forms less than 80 wt.% of the clay mineral.
- the clay mineral used in the method of the invention preferably comprises a smectite phase.
- the clay mineral preferably comprises less than 60 wt.%, more preferred less than 50 wt.%, particularly preferred less than 40 wt.% of a smectite phase.
- the smectite phase forms at least 10 wt.%, according to a further embodiment at least 20 wt.% of the clay mineral.
- the ratio of smectite phase to amorphous phase preferably is within a range of 2 to 0.5, more preferred 1.2 to 0.8.
- amorphous phase and the smectite phase further minerals may be present in the clay mineral, preferably within a range of 0.5 to 40 wt.%, more preferred 1 to 30 wt.%, particularly preferred 3 to 20 wt.%.
- Exemplary side minerals are quartz, cristobalite, feldspar and calcite. Other side minerals may also be present.
- the matrix of the clay mineral preferably formed from silica gel dilutes the smectite phase which leads, depending on the fraction of the smectite phase, to a lowering of the signal-to-noise ratio of typical reflections of smectite minerals e.g. the small angle reflections of montmorillonite are effected by the periodic distance between layers of the montmorillonite structure.
- the clay particles fixed in the Si0 2 -matrix are delaminated to a very high degree leading to a strong broadening of the corresponding diffraction peak.
- the amount of amorphous silica phase and smectite clay phase present in the clay mineral can be determined by quantitative X-ray-diffraction analysis. Details of such method are described e.g. in "Hand Book of Clay Science", F. Bergaya, B.K.G. Therry, G. Lagaly (Eds.), Elsevier, Oxford, Amsterdam, 2006, Chapter 12.1 : I. Srodon, Identification and Quantitative Analysis of Clay Minerals; "X-Ray Diffraction and the Identification and Analysis of Clay Minerals", D.M. Moora and R.C. Reaynolds, Oxford University Press, New York, 1997, pp 765, included herein by reference.
- the XRD-diffractogram of the clay mineral of the present invention exhibit the reflexes which are hardly visible above noise.
- the signal to noise ratio for reflexes of the clay mineral, in particular the smectite phase is close to 1 , preferably in the range of 1 to 1.2.
- the sharp reflexes may be visible in the diffractogram originating from impurities in the clay mineral, e.g. quartz. Such reflexes are not considered for determination of the signal/noise ratio.
- the clay mineral of the present invention which does not or does hardly show a 001 reflection indicating the layer distance within the crystal structure of bentonite particles.
- Hardly visible means that the signal-to-noise ratio of the 001 reflection of the smectite particles is preferably less than 1.2, particularly preferred is within a range of 1.0 to 1.1.
- the clay mineral has a sediment volume in water after 1 hour of less than 15 ml/2g, more preferred of less than 10 ml/2g and most preferred of less than 7 ml/2g.
- the clay mineral of the present invention in particular when mined from a natural source, preferably has a cation exchange capacity of more than 40 meq/100 g, particularly preferred of more than 45 meq/100 g and is most preferred selected within a range of 44 to 120 meq/100 g.
- high activity bleaching earth obtained by extracting a clay mineral with boiling strong acid is characterized by a very low cation exchange capacity of usually less than 40 meq/100 g and in most cases of less than 30 meq/100g.
- the modified clay used in the method according to the invention therefore can clearly be distinguished from such high performance bleaching earth.
- the clay of the present invention is characterized by a high content of S1O2 determined after complete disintegration of the clay being above 62 wt.%, preferably above 64 wt.%, especially preferred above 66 wt.%.
- silicon other preferred metals or metal oxides may be contained in the clay. All percentages refer to a dry clay material dried to constant weight at 105°C.
- the clay preferably has a low aluminium content of, calculated as AI2O3, less than 15 wt.%, more preferred of less than 10 wt.%.
- the aluminium content, calculated as AI2O3, according to an embodiment is more than 2 wt.%, according to a further embodiment more than 4 wt.%.
- the clay contains magnesium, calculated as MgO, in an amount of less than 7 wt.%, preferably of less than 6 wt.%, particularly preferred less than 5 wt.%. In one embodiment, the magnesium content is at least 2 wt.%
- the clay contains iron, calculated as Fe 2 03, in amount of less than 8 wt.%.
- the iron content, calculated as Fe203 may be less than 6 wt.% and according to a still further embodiment may be less than 5 wt.%.
- the clay may contain iron, calculated as Fe203, in an amount of at least 1 wt.%, and according to a still further embodiment in an amount of at least 2 wt.%.
- the present invention provides encapsulation of shading dyes comprising forming an encapsulation matrix consisting of mixture of silica for example hydrophilic silica or hydrophobic silica, clay, dye and binding agent for example surfactant or polymers to obtain stable encapsulated dye composition.
- the present invention provides method for the preparation of the encapsulated dye composition.
- the method for preparation of encapsulated dye composition comprises
- the encapsulated dye composition can be in the powder form or in granular form.
- the coating of the granules with the binder can be carried out by the
- the dye is entrapped in the carrier matrix by simple physical mixing resulting in slightly powder material.
- granules are formed by compaction or granulation or by extrusion or by using fluidized bed processing.
- the granules thus formed have particle size -400 to 600 microns.
- the resulting particles can be treated in additional step with liquid barrier materials like surfactants, aqueous solution of thickening polymers etc.
- the resulting encapsulated dye matrix is not bleeding the dye in powder detergent. Thus, it is not impacting white powder detergent color.
- the encapsulated dye is released in water as desired during the washing cycle.
- composition comprises
- the process comprises encapsulation of shading dye Duasyn Acid Violet 4BN-IN (C.l. Acid Violet 17), Duasyn Violet SP-IN (C.l. Direct Violet 66), Duasyn Red N-6B-IN (C.l. Acid Violet 54), Duasyn Violet FBL-IN (C.l. Acid Violet 48), Duasyn Red Violet E2R-IN (C.l. Acid Violet 126) or mixtures of one or several of the afore mentioned dye.
- the dye is suspended in water or used as press cake and is blended or absorbed on silica and bentonite blends to achieve white dye encapsulated powder.
- the process for preparation of encapsulated dye composition comprises mixing about 5-20% of dye with binder for example 1 -5% of polymer or surfactant and blending this mixture with silica for example Sipernat ® D17 optionally followed by addition of about 5 to 30% of silica for example Ibersil ® D100P. The mixture is then blended thoroughly and the binder is added.
- the clay bentonites for example 20-40% of Laundrosil DGA and EXM 0242 is added to the blended mixture which will absorb on the shading dye loaded silica particles to give the encapsulated dye composition. This process involves manual/physical mixing of all the ingredients.
- the process for preparation of encapsulated dye composition comprises fluidized bed coating process to obtain encapsulated matrix of at least one suitable dye, silica, bentonite and binders which provides spherical particles having particle size of - 500 micron.
- dye is mixed with silica for example Sipernat ® 22 and clay in required composition, followed by addition of water to make dough. The dough is then extruded using extruder and spheronised to prepare granules.
- the spheronised granules are further coated using Fluidized Bed Processer with suitable binding or coating polymers such as Hydroxy Propyl Methyl Cellulose (HPMC), Carboxy methyl cellulolse (CMC), Polyvinyl alcohol (PVA), polyvinyl acetate (PVAc), and optionally T1O2 dispersion for whiteness.
- suitable binding or coating polymers such as Hydroxy Propyl Methyl Cellulose (HPMC), Carboxy methyl cellulolse (CMC), Polyvinyl alcohol (PVA), polyvinyl acetate (PVAc), and optionally T1O2 dispersion for whiteness.
- the encapsulated dye composition comprises a carrier consisting of a mixture of silica and clay, a dye encapsulated in the carrier and optionally a binder.
- the encapsulated dye of the present disclosure is found to be stable and did not leave stains on the fabric during the washing.
- the encapsulated dye composition when used in the detergent powder does not bleed into the powder and therefore it does not affect the white color of the detergent powder. Additionally, the encapsulated dye composition is released in water within few seconds with gentle stirring and can be easily shed off the clothes during washing.
- the present invention provides a detergent composition comprising encapsulated dye composition comprising:
- a carrier comprising 30% to 75% by weight of silica and 20% to 40% by weight of clay
- the present invention provides a method of laundering fabrics which includes a step of treating the fabrics with detergent composition comprising the encapsulated dye composition which comprising:
- a carrier comprising 30% to 75% by weight of silica and 20% to 40% by weight of clay
- the amount of water present in the clay material at a temperature of 105°C was determined according to DIN/ISO-787/2.
- the S1O2 was incinerated together with the filter paper and the residue was weighed.
- the filtrate was transferred into a calibrated flask and distilled water was added until the calibration mark.
- the amount of aluminium, iron, calcium and magnesium in the solution was determined by FAAS.
- a 500 mg sample was weighed in a platinum bowl with a precision of 0.1 mg.
- the sample was moistened with about 1 to 2 ml of distilled water and then four drops of concentrated sulphuric acid were added.
- About 10 to 20 ml of concentrated hydrofluoric acid was added and the liquid phase evaporated to dryness in a sand bath. This process was repeated three times.
- FI 2 SO 4 was added to the dry residue and the mixture was evaporated to dryness on an oven plate.
- the platinum bowl was calcined and, after cooling to room temperature, 40 ml of distilled water and 5 ml hydrochloric acid (18 %) was added to the residue and the mixture was heated to boiling.
- the solution was transferred into a calibrated 250 ml flask and water was added up to the calibration mark.
- the amount of sodium, potassium and lithium in the solution was determined by EAS.
- the clay material to be tested was dried at 150°C for two hours. Then the dried material was allowed to react under reflux with a large excess of aqueous NhUCI solution for 1 hour. After standing at room temperature for 16 hours, the material was filtered. The filter cake was washed, dried, and ground, and the NhU content in the clay material was determined by the Kjedahl method. The amount and kind of the exchanged metal ions was determined by ICP-spectroscopy.
- a graduated 100 ml glass cylinder was filled with 100 ml of distilled water or with an aqueous solution of 1 % sodium carbonate and 2 % trisodium polyphosphate. 2 g of the compound to be analyzed was placed on the water surface in portions of about 0.1 to 0.2 g. After sinking down of a portion, the next portion of the compound was added. After adding 2 g of
- the test of the clay material was performed in the same way as described for the test bentonite. On the basis of the spent methylene blue solution was calculated the inner surface of the clay material. According to this method 381 mg methylene blue/g clay correspond to a content of 100 %
- a vacuum cleaner connected with the sieve aspirates over a suction slit circling under the perforated sieve bottom all particles being finer than the inserted sieve being covered on top with an acrylic glass cover and leaves the coarser particles on the sieve.
- the experimental procedure was as follows: Depending on the product, between 5 and 25 g of air dried material was weighed in and was put on the sieve. Subsequently, the acrylic glass cover was put on the sieve and the machine was started. During air jet screening, the screening process can be facilitated by beating on the acrylic glass cover using the rubber hammer. Exhaustion time was between 1 and 5 minutes. The calculation of the dry screening residue in % is as follows: actual weight multiplied with 100 and divided by the initial weight.
- a calibrated 11 glass cylinder cut at the 1000 ml mark was weighed.
- the sample was poured into the cylinder in a single step such that the cylinder is completely filled and a cone was formed on top of the cylinder.
- the cone was removed with help of a ruler and material adhering to the outside of the cylinder was removed.
- the filled cylinder was weighed again and the apparent weight was obtained by subtracting the weight of the empty cylinder.
- Bentonite 1 Laundrosil ® DGA powder
- Bentonite 2 is produced from Bentonite 2 by alkaline activation
- Clay 3-5 (Clays with High content of S1O2/ Mixed phase of bentonite and natural Silica) is provided in below table. Clay 3 is sold under the brand name Tonsil ® Supreme 118 FF.
- the quantitative X-ray diffraction analysis shows presence of smectite clay in clay 1 and 2 which are used in the method according to the invention.
- various side minerals can be found, like sepiolite for clay 1 , orthoclase, plagioclase (other feldspars) and calcite.
- the X-ray diffraction shows the presence of more than 30 % of amorphous material for both clays.
- the amorphous phase is almost present in the same concentration as the smectite (ratio 100:95), whereas in clay 1 the ratio of smectite to amorphous material is 100:85.
- the dyes used for making encapsulated dye composition are listed in below table:
- silica used in the present invention having the properties as listed in the below table:
- the encapsulated dye composition was a violet color formulation comprising -10% Duasyn Acid Violet 4BN-IN. Comparative Example 2:
- the encapsulated dye composition was a violet color formulation comprising ⁇ 5% Duasyn Acid Violet 4BN-IN. Comparative Example 3:
- the dye composition was a violet color formulation comprising ⁇ 1.2 % Duasyn Acid Violet 4BN-IN. Comparative Example 4:
- Composition 1
- Composition 2 is a composition of Composition 2:
- the so obtained dye composition was a violet color formulation comprising 2% dye. It was observed that the color becomes more intense after storage at 45°C within a week. Formulation was found to release dye within few seconds in water with gentle stirring.
- Composition 3 is a composition of Composition 3:
- the so obtained dye composition was a white color formulation comprising -0.5% dye, which was found to be stable at room temperature (RT) and at 45°C on storage for 2 months. Formulation was found to release dye within few seconds in water with gentle stirring.
- RT room temperature
- Example 5
- Composition 5 is a composition of Composition 5:
- the so obtained dye composition was a white color formulation comprising ⁇ 6% dye, which was found to be stable at RT and at 45°C on storage for 2 months.
- Formulation was found to release dye within few seconds in water with gentle stirring.
- composition 6 is a composition of Composition 6:
- Formulation was found to release dye within few seconds in water with gentle stirring.
- Composition 7 is a composition of Composition 7:
- Formulation was found to release dye within few seconds in water with gentle stirring.
- Composition 8 is a composition of Composition 8:
- composition 9 is a composition of Composition 9:
- the so obtained dye composition was a white color formulation comprising ⁇ 7% dye, which was found to be stable at RT and at 45°C on storage for 2 months.
- Composition 10 is a composition of Composition 10:
- Formulation was found to release dye within few seconds in water with gentle stirring.
- Composition 11
- DGA powder ® (soda activated bentonite) to obtain the encapsulated dye composition.
- the so obtained dye composition was a white color formulation comprising -10% dye, which was found to be stable at RT and at 45°C upon storage for 2 months. Formulation was found to release dye within few seconds in water with gentle stirring.
- the same formulation could be prepared using Duasyn Violet FBL-IN, Duasyn Red Violet E2R-IN or mixtures of two or three dyes mentioned in this example.
- Composition 12 The encapsulated dye composition is prepared using Fluidized Bed Process.
- Dye premix containing 100g of Duasyn Acid Violet 4BN-IN dye in water was mixed with a mixture of 200g of Ibersil ® D 100 P (Silicon Dioxide, Hydrophilic Silica with bigger particle size, d (50): ⁇ 200micron), 100g of Clay 1 Laundrosil ® DGA-powder (soda activated bentonite) and 100g of Clay 2 EX ® 0242 (natural Ca-bentonite) in Stephen mixer to obtain a mixture/dough cake.
- the mixture/dough cake was extruded through an extruder to obtain extrudates.
- the extrudates were spheronized to obtain granules. Obtained granules were further dried at 45°C in oven to remove any moisture.
- the granules were coated with the binder to obtain the encapsulated dye composition.
- the above Table shows the final composition of the encapsulated dye composition 12.
- Example 13 Composition 13:
- the so obtained dye composition was found to be a white color formulation comprising -18% Dye.
- the mixing was done manually for encapsulation.
- the dye composition was found to be stable at RT and at 45°C on storage for 2 months.
- the formulation was found to release dye within few seconds in water with gentle stirring.
- the dye composition was found stable in strength testing.
- Duasyn Acid Violet 4BN-IN for the premix
- Duasyn Violet SP-IN, Duasyn Red N-6B-IN, Duasyn Violet FBL-IN or Duasyn Red Violet E2R-IN or a mixture of two or several of the afore mentioned dye can be used for the preparation of the formulation mentioned in this example.
- composition 14 is a composition of Composition 14:
- phase B dye premix containing Duasyn Violet SP-IN and HPMC
- Sipernat ® 22 Silicon Dioxide, Hydrophilic
- the dye composition was found to be violet colored granules, which were found to be stable at RT and at 45°C storage for 2 months.
- the formulation was found to release dye within few seconds in water with gentle stirring.
- the dye composition was found to be stable in strength testing and no dye staining on cloth piece after washing.
- Similar formulations can be prepared with the shading dyes Duasyn Acid Violet 4BN-IN, Duasyn Red N-6B-IN, Duasyn Violet FBL-IN, Duasyn Red Violet E2R-IN or a mixture of two or several of the afore mentioned dyes.
- Composition 15 The encapsulated dye composition is prepared using Fluidized Bed Process.
- Dye premix containing Duasyn Acid Violet 4BN-IN in water was mixed with a mixture of Ibersil ® D 100 P (Silicon Dioxide, Hydrophilic Silica with bigger particle size, d (50): ⁇ 200micron), Laundrosil DGA-powder and EXM 0242 (bentonite/Clay) in Stephen mixer to obtain a mixture/dough cake.
- Ibersil ® D 100 P Silicon Dioxide, Hydrophilic Silica with bigger particle size, d (50): ⁇ 200micron
- Laundrosil DGA-powder Laundrosil DGA-powder
- EXM 0242 bentonite/Clay
- the so obtained dye composition was off white color HPMC coated beads, which were found to be stable at RT and at 50°C on storage for 2 months.
- the formulation was found to release dye within few seconds in water with gentle stirring.
- Comparable Formulations can be prepared using Duasyn Violet SP-IN or Duasyn Red N-6B-IN, Duasyn Violet FBL-IN or Duasyn Red Violet E2R-IN or a mixture of two or several of the fore mentioned dyes.
- compositions of present invention are tested for their effects which are discussed as below.
- Open dish stability test was carried out to test the bleeding character of the encapsulated dye composition.
- the encapsulated dye composition was mixed with the white detergent powder and the resulting powder was kept in a petri dish and was left in the open environment for up to 2 months at room temperature and elevated temperature to check bleeding.
- the encapsulated dye compositions of the present invention prepared according to the above examples were used for the strength testing.
- the encapsulated sample was added to the powder detergent or components such as sodium sulfate.
- the sample was exposed to shear mimicking conditions of mixing dye with powder detergent.
- the sample was further observed after strength testing for migration of dye in powder detergent/sodium sulfate.
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Detergent Compositions (AREA)
- Cosmetics (AREA)
- Manufacturing Of Micro-Capsules (AREA)
Abstract
Description
Claims
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
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EP18211210.2A EP3666869A1 (en) | 2018-12-10 | 2018-12-10 | An encapsulated dye composition and a method for preparation thereof |
PCT/EP2019/083471 WO2020120225A1 (en) | 2018-12-10 | 2019-12-03 | An encapsulated dye composition and a method for preparation thereof |
Publications (2)
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EP3894532A1 true EP3894532A1 (en) | 2021-10-20 |
EP3894532B1 EP3894532B1 (en) | 2024-03-27 |
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Application Number | Title | Priority Date | Filing Date |
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EP18211210.2A Ceased EP3666869A1 (en) | 2018-12-10 | 2018-12-10 | An encapsulated dye composition and a method for preparation thereof |
EP19812786.2A Active EP3894532B1 (en) | 2018-12-10 | 2019-12-03 | An encapsulated dye composition and a method for preparation thereof |
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Application Number | Title | Priority Date | Filing Date |
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EP18211210.2A Ceased EP3666869A1 (en) | 2018-12-10 | 2018-12-10 | An encapsulated dye composition and a method for preparation thereof |
Country Status (4)
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EP (2) | EP3666869A1 (en) |
CN (1) | CN113166686A (en) |
BR (1) | BR112021011064A8 (en) |
WO (1) | WO2020120225A1 (en) |
Family Cites Families (13)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CA2327453A1 (en) * | 1999-12-04 | 2001-06-04 | Henkel Kommanditgesellschaft Auf Aktien | Laundry detergents and cleaning products |
US20040018955A1 (en) * | 2000-01-12 | 2004-01-29 | Jean Wevers | Pro-perfume composition |
GB0018774D0 (en) | 2000-07-31 | 2000-09-20 | Unilever Plc | Coloured speckle composition and particulate laundry detergent compositions containing it |
EP1352951A1 (en) * | 2002-04-11 | 2003-10-15 | The Procter & Gamble Company | Detergent granule comprising a nonionic surfactant and a hydrotrope |
CA2635974A1 (en) * | 2006-01-12 | 2007-07-19 | The Procter & Gamble Company | Cleaning implement with erodible foam substrate and controlled release system of active agent |
US20110143989A1 (en) * | 2006-04-14 | 2011-06-16 | Petkus Matthew M | Laundry article |
EP2245133B1 (en) * | 2008-01-10 | 2012-05-23 | Unilever Plc, A Company Registered In England And Wales under company no. 41424 of Unilever House | Granules |
US8535392B2 (en) * | 2008-11-25 | 2013-09-17 | Milliken & Company | Solid polymeric colorant compositions |
ES2378495T3 (en) * | 2009-07-17 | 2012-04-13 | Clariant Finance (Bvi) Limited | Cleaning composition that changes color |
US8318652B2 (en) | 2009-08-25 | 2012-11-27 | Milliken & Company | Colored speckles comprising a porous carrier and a releasing agent layer |
US8470760B2 (en) * | 2010-05-28 | 2013-06-25 | Milliken 7 Company | Colored speckles for use in granular detergents |
CN104769094B (en) * | 2012-06-08 | 2018-03-09 | 宝洁公司 | What can especially be applied in combination with powder or particulate composition has the visual contrast particle attractive in appearance of the water solubility improved |
US9889072B2 (en) * | 2014-10-02 | 2018-02-13 | Jgc Catalysts And Chemicals Ltd. | Porous silica particle, method for producing the same, and cleansing cosmetic containing the same |
-
2018
- 2018-12-10 EP EP18211210.2A patent/EP3666869A1/en not_active Ceased
-
2019
- 2019-12-03 CN CN201980081168.0A patent/CN113166686A/en active Pending
- 2019-12-03 WO PCT/EP2019/083471 patent/WO2020120225A1/en unknown
- 2019-12-03 BR BR112021011064A patent/BR112021011064A8/en unknown
- 2019-12-03 EP EP19812786.2A patent/EP3894532B1/en active Active
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BR112021011064A2 (en) | 2021-08-31 |
WO2020120225A1 (en) | 2020-06-18 |
EP3666869A1 (en) | 2020-06-17 |
CN113166686A (en) | 2021-07-23 |
EP3894532B1 (en) | 2024-03-27 |
BR112021011064A8 (en) | 2023-03-07 |
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