CS245098B1 - Method of pigments' surface treatment for polyolefins' mass-dyeing - Google Patents
Method of pigments' surface treatment for polyolefins' mass-dyeing Download PDFInfo
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- CS245098B1 CS245098B1 CS852894A CS289485A CS245098B1 CS 245098 B1 CS245098 B1 CS 245098B1 CS 852894 A CS852894 A CS 852894A CS 289485 A CS289485 A CS 289485A CS 245098 B1 CS245098 B1 CS 245098B1
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- pigment
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- 239000000049 pigment Substances 0.000 title claims abstract description 39
- 229920000098 polyolefin Polymers 0.000 title claims abstract description 14
- 238000000034 method Methods 0.000 title claims description 6
- 238000004381 surface treatment Methods 0.000 title abstract description 7
- 238000004043 dyeing Methods 0.000 title abstract description 3
- 239000000203 mixture Substances 0.000 claims abstract description 15
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical compound C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000004040 coloring Methods 0.000 claims abstract description 7
- 238000000227 grinding Methods 0.000 claims abstract description 7
- GOOHAUXETOMSMM-UHFFFAOYSA-N Propylene oxide Chemical compound CC1CO1 GOOHAUXETOMSMM-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229920001577 copolymer Polymers 0.000 claims abstract description 6
- 229920001451 polypropylene glycol Polymers 0.000 claims abstract description 5
- 150000001298 alcohols Chemical class 0.000 claims abstract description 4
- -1 esters carboxylic acids Chemical class 0.000 claims description 10
- 239000000843 powder Substances 0.000 claims description 5
- 239000012736 aqueous medium Substances 0.000 claims description 3
- 150000002148 esters Chemical class 0.000 claims description 2
- 150000002170 ethers Chemical class 0.000 claims description 2
- 238000000926 separation method Methods 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 20
- 238000000265 homogenisation Methods 0.000 abstract description 4
- 150000001735 carboxylic acids Chemical class 0.000 abstract 1
- 229920005606 polypropylene copolymer Polymers 0.000 abstract 1
- 239000006185 dispersion Substances 0.000 description 15
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 6
- 239000012141 concentrate Substances 0.000 description 5
- 239000002270 dispersing agent Substances 0.000 description 4
- 229920000642 polymer Polymers 0.000 description 4
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 3
- 239000004743 Polypropylene Substances 0.000 description 3
- 239000012065 filter cake Substances 0.000 description 3
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 3
- 229920001155 polypropylene Polymers 0.000 description 3
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 description 2
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 description 2
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 description 2
- 239000005642 Oleic acid Substances 0.000 description 2
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 description 2
- 239000004698 Polyethylene Substances 0.000 description 2
- 239000011324 bead Substances 0.000 description 2
- 150000002334 glycols Chemical class 0.000 description 2
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 229920000573 polyethylene Polymers 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 150000001733 carboxylic acid esters Chemical class 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000009967 direct dyeing Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000003801 milling Methods 0.000 description 1
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 description 1
- 239000012860 organic pigment Substances 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
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- Pigments, Carbon Blacks, Or Wood Stains (AREA)
Abstract
Riešenie sa týká povrchovej úpravy pigmentov pre farbenie polyolefínov v hmotě. Povrchová úprava pigmentov pre farbenie polyolefínov v hmotě podfa riešenia spočívá v tom, že pigment sa po mletí vo vodnom prostředí zhomogenizuje s polyoxypropylénglykolom alebo vo vodě nerozpustným kopolymérom etylénoxidu a propýlénoxidu s molekulovou hmotnostou 600 až 10 000. Okrem toho· sa na povrchovú úpravu možu použit tiež deriváty polypropylénoxidu a kopolyméru etylénoxidu a propýlénoxidu s vyššími alkoholmi a karboxylovými kyselinami. K zmesi sa može přidat tiež práškový polyolefín. Po homogenizácii sa pigment oddělí a vysuší.The solution relates to the surface treatment of pigments for coloring polyolefins in the mass. Surface treatment of pigments for dyeing polyolefins in the mass of the solution lies in that the pigment is ground after grinding the environment homogenizes with polyoxypropylene glycol or water insoluble copolymer of ethylene oxide and propylene oxide with a molecular weight of 600 to 10,000. In addition, it can be used for surface treatment polypropylene oxide and copolymer derivatives are also used ethylene oxide and propylene oxide s higher alcohols and carboxylic acids. Powdered can also be added to the mixture polyolefin. After homogenization, the pigment is separated and dried.
Description
Vynález sa týká povrchovej úpravy pigmentov pre farbenie polyolefínov v hmotě.The invention relates to the surface treatment of pigments for coloring polyolefins in a mass.
Farebná výdatnosť pigmentov- používaných pre farbenie polyolefínov v hmotě je funkciou ich kvality, najma schopnosti dispergácie do· vysokého stupňa v polymérnej tavenine. Vysoký stupeň disperzity pigmentov v polyolefínoch je možné získat prídavkom vhodných dispergátorov (AO 195 089, AO 220 955, AO 220 957). Tieto látky ovplyvňujú často aj ďalšie vlastnosti polymérnej taveniny, ako například zníženie elektrostatického náboja, zlepšenie reologických vlastností a spracovatefnostl. Aj pri použití dispergačných přísad sa však nedosiahne optimálny stupeň disperzity pigmentov pri využití komerčných dispergačných zariadení.The color yield of pigments used for coloring polyolefins in the mass is a function of their quality, in particular the ability to disperse to a high degree in the polymer melt. A high degree of pigment dispersion in polyolefins can be obtained by adding suitable dispersants (AO 195 089, AO 220 955, AO 220 957). These substances often also influence other properties of the polymer melt, such as reducing electrostatic charge, improving rheological properties and processability. However, even with the use of dispersants, the optimum degree of pigment dispersion is not achieved when using commercial dispersing devices.
Maximálny alebo optimálny stupeň disperzity organických pigmentov pre farbenie polyolefínov v hmotě je možné dosiahnúť len špeciálnymi postupmi pri mletí v prostředí kvapalín s viskozitou okolo 1 Pas (NSR pat. 126 136, US pat. 3 755 244). Princip týchto postupov spočívá v mletí pigmentov vo vodnom prostředí za, alebo bez přítomnosti polyolefínov a za přídavku špeciálneho dispergátora, rozpuštěného vo vodě v závislosti od pH, ako organické) fázy, ktorá sa po mletí spolu s pigmentem vyzráža znížením teploty a změnou pH prostredia.The maximum or optimal degree of dispersion of organic pigments for coloring polyolefins in the mass can only be achieved by special grinding procedures in liquids with a viscosity of about 1 Pas (US Pat. 126 136, US Pat. 3,755,244). The principle of these processes consists in grinding the pigments in an aqueous medium with or without the presence of polyolefins and with the addition of a special dispersant dissolved in water depending on the pH (organic) phase which precipitates after grinding together with the pigment.
Predmetom vynálezu je sposob povrchové] úpravy pigmentov pre farbenie polyolefínov v hmotě, ktorý sa vyznačuje tým, že sa pigment po mletí vo vodnom prostředí homogenizuje s polyoxypropylénglykolom alebo- vo vodě nerozpustným kopolymérom etylénoxidu a propylénoxidu s molekulovou hmotnosťou 600 až 10 000, alebo ich étermi s vyššími alkoholmi, alebo s estermi s karboxylovými kyselinami s počtom uhlíkov Cs až C20, alebo ich zmesami, bez alebo za přítomnosti práškového polyolefinů, pri teplote 20 až 100 °C a po separácii sa upravený pigment vysuší. Ochladením disperzie alebo přidáním studenej vody do disperzie vznikne lahkodispergovatefná konzistencia disperze.The present invention relates to a process for the surface treatment of polyolefin coloring pigments in a mass, characterized in that the pigment, after grinding in aqueous medium, is homogenized with polyoxypropylene glycol or a water-insoluble copolymer of ethylene oxide and propylene oxide of molecular weight 600-10,000 or ethers thereof. with higher alcohols or with carboxylic acid esters having a carbon number of C8 to C20, or mixtures thereof, in the presence or absence of polyolefins at a temperature of 20 to 100 DEG C. and after separation, the treated pigment is dried. Cooling the dispersion or adding cold water to the dispersion produces a dispersible dispersion consistency.
Ako povrchovoaktívne látky pri mletí pigmentu sa použijú iónogenné alebo neiónogenné látky, ak-o< napr. polyoxyetylénglykoly -a ich vo vodě rozpustné deriváty v koncentrácii do 30 % hmot. Koncentrácia pigmentu pri mletí vo vodnom prostředí je 4 až 40 % hmot.Ionogenic or non-ionic substances are used as surfactants in the milling of the pigment, e.g. polyoxyethylene glycols and their water-soluble derivatives in a concentration of up to 30% by weight; The pigment concentration for aqueous grinding is 4 to 40% by weight.
Organický dispergátor na báze vo vodě nerozpustných derivátov p-olyoxyalkylénglykolov, kopolymérov- etylénoxidu a propylénoxidu alebo ich zmesi sa pri povrchovej úpravě přidá v množstve 20 — 150 % hmot. na pigment, výhodné 30 — 50 % hmot. na pigment.The organic dispersant based on the water-insoluble derivatives of p-olyloxyalkylene glycols, copolymers-ethylene oxide and propylene oxide or mixtures thereof is added in an amount of 20-150% by weight in the surface treatment. % to pigment, preferably 30-50 wt. for pigment.
P-ovrchovoupravený pigment sa v ďalšom použije na přípravu koncentrovaných f-arebných disperzií alebo- na priame farbenie polyolefínov v hmotě.The β-superficial pigment is further used for the preparation of concentrated phosphate dispersions or for direct dyeing of polyolefins in the mass.
K výhodám uvedeného postupu přípravy povrchovo upravených pigmentov patří vznik pigmentu vo formě čiastočiek s priemero-m pod 0,1 mm s podstatným znížením prašnosti, vysokým stupňom preddispergovatefnosti pigmentu s následným zvýšením jeho farbiace) sily o 20 — 30 °/o, najmá pri ťažk-odispergovatefných typoch, a dobrá miešatefnosť a hom-ogenizácia so základným práškovým polymérom, resp. v tavenlne polyméru.Advantages of said process for the preparation of surface-treated pigments include the formation of pigment particles in the diameter of less than 0.1 mm with a significant reduction in dustiness, a high degree of pigment pre-dispersibility with subsequent increase in its coloring strength by 20-30 ° / o. dispersible types, and good miscibility and homogenization with the base powder polymer, respectively. in a polymer melt.
Nižšie uvedené příklady ilustrujú predmet vynálezu.The examples below illustrate the subject matter of the invention.
Příklad 1Example 1
100 dielov hmot. pigmentu yellow 95 vo formě filtračného koláča obsahujúceho 20 dielov čistého pigmentu a 80 dielov vody sa v planetové) miešačke zriedi s dalšími 100 dielmi vody obsahujúcej 20 % hmot. poly-o-xyetylénglyikolu 600 a 6 000 v pomere 1 : 1. Po zhomogenizovaní sa disperzie melie v kontinuálně pracujúcom perlovom mlýne pri 2 000 otáčkách a 70 °C s 5-násobným prechodom. Disperzia sa potom prenesie dovysokootáčkového h-omogenizéra a přidá sa k nej 8 dielov kopolymerů etylénoxidu a propylénoxidu 1 : 4 s molekulovou hmotnosťou 3 000 a zmes sa potom homogenizuje počas 10 minút. N-akoniec sa přidá ešte 100 dielov studenej vody. V disperzii sa vytvoria částice povrchovoupraveného pigmentu. Tieto sa odfiltrujú, premyjú vodou a vysušia pri 60 °C do konstantně]' hmotnosti.100 parts by weight Pigment yellow 95 in the form of a filter cake containing 20 parts pure pigment and 80 parts water is diluted in a planetary mixer with an additional 100 parts water containing 20 wt. poly-o-xyethylene glycol 600 and 6,000 in a 1: 1 ratio. After homogenization, the dispersion is ground in a continuously operating bead mill at 2000 rpm and 70 ° C with a 5-fold passage. The dispersion is then transferred to a high-speed h-omogenizer and 8 parts of a 1: 4 ethylene oxide / propylene oxide copolymer with a molecular weight of 3,000 are added and the mixture is then homogenized for 10 minutes. 100 parts of cold water are added at the end. The surface-treated pigment particles are formed in the dispersion. These are filtered off, washed with water and dried at 60 ° C to constant weight.
Příklad 2 dielov hmot. pigmentu red 147 sa zmieša so 180 dielmi vody obsahujúcej 20 ιθ/ο hmot. esteru polyoxyetylénglykolu 600 a kyseliny olejovej. Po zhomogenizo-vaní sa disperzia melie v kontinuálnem perlovom mlýne 4 hod. Po tomto čase sa disperzia prenesie do rýchlootáčkového ho-mogenizéra. K disperzii sa přidá 100 dielov éteru polypropylénoxidu a oktylalkoholu s molekulovou hmotnosťou 2 500. Disperzia sa pri teplote 50 C zhomogenizuje pri 2 000 otáčkách a potom ochladí přidáním dalších 100 dielov studenej vody. Vzniknutá obalená disperzia sa odfiltruje, premyje vodou a vysuší pri tepl-ote 60 °C.Example 2 parts by weight. Pigment Red 147 was mixed with 180 parts water containing 20 ιθ / ο weight. polyoxyethylene glycol 600 ester and oleic acid. After homogenization, the dispersion is ground in a continuous bead mill for 4 hours. After this time, the dispersion is transferred to a high speed homogenizer. 100 parts of polypropylene ether-octyl alcohol having a molecular weight of 2500 are added to the dispersion. The dispersion is homogenized at 2,000 rpm at 50 ° C and then cooled by adding an additional 100 parts of cold water. The resulting coated dispersion was filtered off, washed with water and dried at 60 ° C.
Příklad 3Example 3
K 50 dielom práškového- polyetylénu sa přidá 20 dielov kopolymerů etylénoxidu a propylénoxidu 1: 5 o- molekulové] hmotnosti 2 000 a zmes sa zhomogenizuje na rýchlomiešačke pri normálnej teplote. K zmesi sa potom přidá 500 dielov vody a 100 dielov filtračného koláča mletého pigmentu yellow 145 obsahujúceho 50 % vody. Zmes sa znova zhomogenizuje na rýchl-omiešačke za čas 10 minút. Potom sa přidá dalších ,2 45 09 8To 50 parts of polyethylene powder are added 20 parts of a 1: 5 o-molecular weight ethylene oxide / propylene oxide copolymer of 2,000 weight and the mixture is homogenized on a rapid mixer at normal temperature. 500 parts of water and 100 parts of yellow 145 ground pigment filter cake containing 50% water are then added to the mixture. The mixture was again homogenized on a rapid mixer for 10 minutes. Then add another 45 45 8
150 dielov vody, upravený pigment sa odfiltruje a vysuší pri 70 °C za vakua.150 parts water, the treated pigment is filtered off and dried at 70 ° C under vacuum.
Příklad 4Example 4
K 50 dielom práškového polyetylénu sa přidá 30 dielov polyoxypropylénglykolu o molekulovej hmotnosti 2 500 a zmes sa zhomogenizuje na rýehlomiešačke za čas 5 minút. K zmesi sa přidá 100 dielov filtračného koláča pigmentu black 7 obsahujúceho· 50 proč. vody a 500 dielov vody. Zmes sa znova homogenizuje 15 min. pri teplote 40 CC na rýehlomiešačke a po přidaní dalších 200 dielov studenej vody sa upravený pigment odfiltruje a vysuší za vakua pri 70 °C. Příklad 5To 50 parts of powdered polyethylene was added 30 parts of polyoxypropylene glycol having a molecular weight of 2,500 and the mixture was homogenized on a mixer for 5 minutes. To the mixture was added 100 parts of a black 7 pigment filter cake containing · 50 why. water and 500 parts water. The mixture is again homogenized for 15 min. at 40 ° C in a quencher and after addition of another 200 parts of cold water, the treated pigment is filtered and dried under vacuum at 70 ° C. Example 5
K 50 dielom práškového degradovaného polypropylénu s indexom toku 150 g/10 min. sa přidá 20 dielov zmesi 1: 1 kopolyméru etylénoxidu a propylénoxidu 1 : 4 o molekulovej hmotnosti 4 500 a esteru kyseliny olejovej s polyoxyetylénglykolom 600 a zhomogenizuje pri 60 °C. Přidá sa 100 dielov filtračného koláča pigmentu red 147 obsahujúceho 50 % vody a dalej sa přidá 400 dielov vody. Celá zmes sa zhomogenizuje na rýehlomiešačke za čas 10 minút. Po přidaní 200 dielov studenej vody sa upravený pigment odstředí a vysuší.To 50 parts degraded polypropylene powder with a flow index of 150 g / 10 min. 20 parts of a 1: 4 mixture of ethylene oxide and propylene oxide 1: 4 having a molecular weight of 4,500 and an oleic acid ester of polyoxyethylene glycol 600 are added and homogenized at 60 ° C. Add 100 parts of the red 147 pigment cake containing 50% water and add 400 parts of water. The whole mixture is homogenized on a stirrer for 10 minutes. After adding 200 parts of cold water, the treated pigment is centrifuged and dried.
Příklad 6Example 6
K 50 dielom práškového polypropylénu sa přidá 30 dielov 2-etylhexyléteru kopolyméru etylénoxidu a propylénoxidu 1:4 o· molekulovej hmotnosti 3 500 a zmes sa zhomogenizuje na rýehlomiešačke pri normálnej teplote počas 5 minút. K tomu sa přidá 100 dielov filtračného koláča pigmentu yellow 145, obsahujúceho 40 % vody a zmes sa znova zhomogenizuje počas 15 min. na rýchlomiešačke a vysuší pri 70 °C za vákua.To 50 parts of polypropylene powder is added 30 parts of a 1: 4 ethylene oxide / propylene oxide copolymer of 3,500 molecular weight of 3,500 and the mixture is homogenized on a mixer at normal temperature for 5 minutes. To this was added 100 parts of a yellow 145 pigment cake containing 40% water and the mixture was again homogenized for 15 min. on a rapid mixer and dried at 70 ° C under vacuum.
Zvýšenie farbiacej sily (RFS) koncentrátov připravených z upravených pigmentov oproti koncentrátom vyrábaným klasickými sposobmi, stanovené] na základe merania remisie vlákien vyrábaných z uvedených koncentrátov.The increase in dyeing strength (RFS) of the concentrates prepared from the treated pigments over the concentrates produced by conventional methods, determined by measuring the remission of the fibers produced from said concentrates.
RFS koncentrátov z upraveného pigmentu oproti klasickýmRFS concentrates of treated pigment versus conventional
Číslo koncentorátom z tých istých příkladu pigmentovConcentrate number from the same pigment examples
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