CS267060B1 - Method of pigments' surface treatment for polyolefins - Google Patents

Method of pigments' surface treatment for polyolefins Download PDF

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CS267060B1
CS267060B1 CS863830A CS383086A CS267060B1 CS 267060 B1 CS267060 B1 CS 267060B1 CS 863830 A CS863830 A CS 863830A CS 383086 A CS383086 A CS 383086A CS 267060 B1 CS267060 B1 CS 267060B1
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polyolefins
molecular weight
pigment
pigments
surface treatment
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CS863830A
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Slovak (sk)
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CS383086A1 (en
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Anton Ing Csc Marcincin
Koloman Ing Csc Ondrejmiska
Elena Ing Csc Zemanova
Jozef Prof Ing Drsc Beniska
Tatiana Ing Marcincinova
Miroslav Ing Csc Necas
Jozef Samuhel
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Marcincin Anton
Ondrejmiska Koloman
Zemanova Elena
Beniksa Jozef
Tatiana Ing Marcincinova
Necas Miroslav
Jozef Samuhel
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Priority to CS863830A priority Critical patent/CS267060B1/en
Publication of CS383086A1 publication Critical patent/CS383086A1/en
Publication of CS267060B1 publication Critical patent/CS267060B1/en

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Abstract

Riešenie sa týká povrchovej úpravy pigmentov pre polyolefíny. Podstata spósobu úpravy pigmentov podlá riešenia spočívá v tom, že pigment sa melie vo vodnom prostředí a homogenizuje pri teplote 70 až 100 °C s roztavenou trojzložkovou zmesou vysokomolekulového polyolefinů s molekulovou hmotnostou 2 000 až 50 000, dialkylftalátu s počtom uhlíkov v alkylreťazci 4 až 8 alebo neprchavého alkylderivátu fenolu alebo benzofenónu s počtom uhlíkov v alkylreťazci 4 až 35, a nízkomolekulového polyolefinů s molekulovou hmotnosťou 600 až 1 500, v pomere od 2,3: :0,7:2 do 2:2:1 hmot. dielov.The solution relates to surface treatment pigments for polyolefins. The nature of the method the treatment of the pigments according to the solution lies in that the pigment is ground in an aqueous medium and homogenized at 70-100 ° C s molten three component high molecular weight blend polyolefins with molecular weight From 2,000 to 50,000, dialkyl phthalate in number carbon atoms in the alkyl chain of 4 to 8 or non-volatile a phenol or benzophenone alkyl derivative with carbon numbers in the alkyl chains of 4 to 35, and molecular weight low molecular weight polyolefins with a weight of 600 to 1500, in a ratio of 2.3: : 0.7: 2 to 2: 2: 1 wt. parts.

Description

Vynález sa týká spósobu povrchovéj úpravy pigmentov pre polyolefíny.The invention relates to a process for the surface treatment of pigments for polyolefins.

Farebná sila pigmentov používaných pre farbenie polyolefínov v hmotě závisí od velkosti častíc pigmentu, a teda najmá od schopnosti ich dispergácie v tavenine polyméru. Stupeň disperzity pigmentov je možné zvýšit dispergačnými přísadami (AO 195 089, AO 220 955, AO 220 957), alebo povrchovou úpravou pigmentov (NSR pat. 126 136, US pat. 3 755 244). Najma povrchová úprava pigmentov rieši ich stupeň disperzity v polyolefínoch, pri optimálnych podmienkach mletia na maximálněj úrovni, so zvýšením ich farebnej sily až o 30 %.The color strength of the pigments used for dyeing polyolefins in the mass depends on the size of the pigment particles, and thus in particular on the ability to disperse them in the polymer melt. The degree of dispersion of the pigments can be increased by dispersing additives (AO 195 089, AO 220 955, AO 220 957) or by surface treatment of the pigments (NSR pat. 126 136, U.S. Pat. No. 3,755,244). In particular, the surface treatment of pigments solves their degree of dispersity in polyolefins, under optimal grinding conditions at the maximum level, with an increase in their color strength by up to 30%.

Okrem zvýšenia farebnej sily pigmentu povrchová úprava rieši tiež niektoré áalšie otázky, a to najma ulahčenie separácie pigmentov z vodnej fázy, zlepšenie podmienok pri sušení a tiež umožňuje netradičnú aplikáciu týchto pigmentov pre priame farbenie (až 50 % disperziami) polyolefínov bez predbežnej přípravy koncentrátov. Povrchová úpravu pigmentov vo vodě nerozpustnými dispergátormi na báze polyoxyalkylénglykolov, ich kopolymérov a derivátov viacmocných alkoholov a karboxylových kyselin riešia AO 245 098, AO 245 096. Aj ked sa pri týchto postupoch dosahujú dobré výsledky z hladiska farebnej výdatnosti pigmentov, nevýhodou týchto postupov je nie celkom uspokojivá separácia pigmentov z vodnej fázy a v niektorých prípadoch plastický charakter upravenéj zmesi, ktorou je na súčasných zariadeniach obtiažná manipulácia.In addition to increasing the color strength of the pigment, the surface treatment also addresses some other issues, in particular facilitating the separation of pigments from the aqueous phase, improving drying conditions and also allowing non-traditional application of these pigments for direct dyeing (up to 50% dispersions) of polyolefins without prior preparation of concentrates. Surface treatment of pigments with water-insoluble dispersants based on polyoxyalkylene glycols, their copolymers and derivatives of polyhydric alcohols and carboxylic acids is solved by AO 245 098, AO 245 096. Although good results are obtained in these processes in terms of color yield of pigments, the disadvantage of these processes is not quite satisfactory separation of pigments from the aqueous phase and in some cases the plastic nature of the treated mixture, which is difficult to handle on current equipment.

Podstata spósobu povrchovej úpravy pigmentov pre polyolefíny podlá vynálezu spočívá v tom, že pigment sa melie vo vodnom prostředí a homogenizuje pri teplote 70 až 100 °C s roztavenou trojzložkovou zmesou vysokomolekulového polyolefínu s molekulovou hmotnosťou 2 000 až 50 000, dialkylftalátu s počtom uhlíkov v alkylreťazci 4 až 8 alebo neprchavého alkylderivátu fenolu alebo benzofenónu s počtom uhlíkov v alkylreťazci 4 až 35 a nízkomolekulového polyolefínu s molekulovou hmotnosťou 600 až 1 500, v pomere od 2,3:0,7:2 do 2:2:1 hmot, dielov. Po ochladení vznikne jemná granulovaná disperzia pigmentu, ktorá sa oddělí a vysuší za zníženého tlaku do konštantnej hmotnosti.The process for the surface treatment of pigments for polyolefins according to the invention is that the pigment is ground in an aqueous medium and homogenized at 70 to 100 ° C with a molten three-component mixture of a high molecular weight polyolefin having a molecular weight of 2,000 to 50,000, dialkyl phthalate with carbon number in the alkyl chain. 4 to 8 or a non-volatile alkyl derivative of phenol or benzophenone having a carbon number in the alkyl chain of 4 to 35 and a low molecular weight polyolefin having a molecular weight of 600 to 1,500, in a ratio of 2.3: 0.7: 2 to 2: 2: 1 parts by weight. After cooling, a fine granular pigment dispersion is formed, which is separated and dried under reduced pressure to constant weight.

Namiesto dialkylftalátu je možné použiť aj iné aromatické deriváty, ako alkylované fenoly, napr. 2,5-ditercbutylfenol, alebo alkylované benzofenóny, napr. 1-hydroxy-4-oktoxybenzofenón, ktoré sú miešatelné vo vysokom zastúpení s polyolefínom a majú schopnost znižovať jeho maximálnu teplotu krystalizácie alebo teplotu topenia, pričom sa vylučujú prchavé aromatické rozpúšťadlá, napr. xylén a jeho deriváty. 'Instead of dialkyl phthalate, it is also possible to use other aromatic derivatives, such as alkylated phenols, e.g. 2,5-ditert-butylphenol, or alkylated benzophenones, e.g. 1-hydroxy-4-octoxybenzophenone, which are miscible in high proportion with the polyolefin and have the ability to lower its maximum crystallization temperature or melting point, while excluding volatile aromatic solvents, e.g. xylene and its derivatives. '

Ako povrchovoaktívne látky sa pri mletí pigmentu použijú neiónogenné látky například polyoxyalkylonglykoly a ich deriváty v koncentrácii do 20 % hmot. Koncentrácia pigmentu sa pri mletí vo vodnom prostředí je 4 až 40 í hmot.Nonionic substances, for example polyoxyalkylene glycols and their derivatives, are used as surfactants in the grinding of the pigment in a concentration of up to 20% by weight. The concentration of the pigment when grinding in an aqueous medium is 4 to 40% by weight.

K výhodám uvedeného postupu patří vznik povrchovo upraveného pigmentu s odstránenou prašnosťou, vo forme jemných hydrofóbnych granuliek s priemerom pod 1 mm, s velmi vhodnou konzistenciou na přípravu farebných koncentrátov so zvýšenou farebnou silou a dobrou dispergovatelnosťou v polyolefínoch. postup je zvlášť vhodný pre diazokondenzačné a antrachinónové pigmenty. Povrchovo upravený pigment je možné aplikovat pri farbení polyolefínov v hmotě, pri príprave farebných koncentrátov bez alebo s použitím dispergátorov alebo použiť na priame farbenie bez přípravy koncentrovaných aisperzií.The advantages of this process include the formation of a surface-treated pigment with dust removal, in the form of fine hydrophobic granules with a diameter below 1 mm, with a very suitable consistency for the preparation of color concentrates with increased color strength and good dispersibility in polyolefins. the process is particularly suitable for diazocondensation and anthraquinone pigments. The surface-treated pigment can be applied in the dyeing of polyolefins in bulk, in the preparation of color concentrates without or with the use of dispersants or used for direct dyeing without the preparation of concentrated dispersions.

Nižšie uvedené příklady ilustrujú predmet vynálezu.The following examples illustrate the subject matter of the invention.

Příklad 1Example 1

100 dielov hmot, pigmentu yellow 95 vo forme filtračného koláča, obsahujúceho 40 dielov čistého pigmentu a 60 dielov vody, sa zriedi dalšími 100 dielmi vody obsahujúcej 10 % hmot, polyoxyetylénglykolu 6 000. Po zhomogenizovaní sa disperzia melie v kontinuálně pracujúcom perlovom mlýne pri 2 000 otáčkach/min a teplote 20 °C za čas 2 h. Disperzia sa potom zohreje100 parts by weight of yellow 95 pigment in the form of a filter cake containing 40 parts of pure pigment and 60 parts of water are diluted with a further 100 parts of water containing 10% by weight of polyoxyethylene glycol 6,000. rpm and 20 ° C for 2 h. The dispersion is then heated

CS 267 060 Bl do varu, prenesie do vysokootáčkového homogenizéra a přidá sa k nej 40 dielov roztavenej zmesi polyetylénu Bralen SA 200, dioktyIftalátu 2:1:2 o teplote 130 °C. Celá disperzia sa potom čas 5 min. Vytvoria sa jemné granulky povrchovo vodnej fázy. Po ochladeni sa pigment odfiltruje Pigment sa vyznačuje zvýšenou farbiacou výdatno: úpravou.CS 267 060 B1 to boiling, transferred to a high-speed homogenizer and 40 parts of a molten mixture of polyethylene Bralen SA 200, dioctyl phthalate 2: 1: 2 at 130 ° C are added. The whole dispersion is then taken for 5 minutes. Fine granules of the surface aqueous phase are formed. After cooling, the pigment is filtered off. The pigment is characterized by an increased coloring abundance: treatment.

a polypropylénového oleja K 1000 v pomere zhomogenizuje pri vysokých otáčkách za upraveného pigmentu, ktoré sa oddelia od a vysuší pri 60 °C do konstantněj hmotnosti. ;ťou pri farbení polyolefínov a neprášivouand polypropylene oil K 1000 are homogenized in proportion at high speed with the treated pigment, which are separated from and dried at 60 ° C to constant weight. in dyeing polyolefins and non-dusting

Příklad 2 dielov mletého pigmentu yellow 147 vo forme 40 %-nej pasty sa zriedi vodou tak, aby jeho koncentrácia v disperzii bola 10 % hmot. Zmes sa zahřeje do varu, prenesie do mixéra a přidá sa k nej 20 dielov hmot, roztavenej zmesi polyetylénu Liten GO 62, dibutylftalátu a polypropylénového oleja K 1000 v pomere 1,5:1,5:2 o teplote 140 °C. Disperzia sa potom zhomogenizuje v mixéri pri vysokých otáčkách za čas 7 min. Vznikne povrchovo upravený pigment vo forme jemných granuliek, ktoré sa po ochladení odfiltrujú a vysušia za vákua pri teplote 70 °C. Povrchovo upravený pigment má zvýšenú farebnú silu a neprášivú úpravu. 'Example 2 parts of ground pigment yellow 147 in the form of a 40% paste are diluted with water so that its concentration in the dispersion is 10% by weight. The mixture is heated to boiling, transferred to a mixer and 20 parts by weight of a molten mixture of polyethylene Liten GO 62, dibutyl phthalate and polypropylene oil K 1000 in a ratio of 1.5: 1.5: 2 at a temperature of 140 ° C are added. The dispersion is then homogenized in a mixer at high speed for 7 minutes. A surface-treated pigment is formed in the form of fine granules which, after cooling, are filtered off and dried under vacuum at 70 ° C. The surface-treated pigment has an increased color strength and a dust-free finish. '

Příklad 3Example 3

K 50 dielom filtračného koláča pigmentu red 177 s obsahom 40 %-nej sušiny sa přidá 50 dielov vody obsahujúcej vo vodě rozpustný ester polyoxyetylénglykolu a kyseliny olejovej. Pri normálnej teplote sa disperzia melie v perlovom mlýne za čas 2 h. Potom sa disperzia zahřeje na 100 °C, prenesie do vysokootáčkového homogenizéra a zhomogenizuje s následné přidanou roztavenou zmesou termicky degradovaného polypropylénu s indexom toku 100 g/10 minút, l-hydroxy-4-(2)-etylhexoxybenzofenónu a polypropylénového oleja K 1000 v pomere 1,5:1,5:2 v množstve 20 dielov. Vznikne jemná disperzia povrchovo upraveného pigmentu v neprášivej úpravě a granulovanej forme, vhodná na farbenie polyolefínov, v hmotě priamo, alebo na přípravu koncentrovaných disperzii.50 parts of water containing a water-soluble ester of polyoxyethylene glycol and oleic acid are added to 50 parts of a filter cake of pigment 177 with a dry matter content of 40%. At normal temperature, the dispersion is ground in a bead mill for 2 hours. The dispersion is then heated to 100 DEG C., transferred to a high-speed homogenizer and homogenized, followed by the addition of a molten mixture of thermally degraded polypropylene with a flow index of 100 g / 10 minutes, 1-hydroxy-4- (2) -ethylhexoxybenzophenone and polypropylene oil K 1000 in a ratio of 1.5: 1.5: 2 in an amount of 20 parts. A fine dispersion of the surface-treated pigment in a non-dusting and granular form is obtained, suitable for dyeing polyolefins, directly in the mass, or for preparing concentrated dispersions.

Příklad 4Example 4

Připraví sa disperzia pigmentu yellow 95 vo vodě podlá příkladu 1 s obsahom 5 % hmot, zmesi polyoxyetylénglykolu 600 a 6 000 1:1 a melie sa v perlovom mlýne za čas 2 h. Disperzia sa potom zahřeje na 95 °C, prenesie do vysokootáčkového homogenizéra a přidá sa k nej roztavená zmes polyetylénu Bralen SA 200, stabilizátor AO 49 a polyetylénový olej v pomere 2:2:1. Po zhomogenizovaní, ochladení a separácii sa získá povrchovo upravený pigment, ktorý po vysušení za vákua vykazuje zvýšenú farebnú silu.A dispersion of yellow 95 pigment in water according to Example 1 containing 5% by weight, a mixture of polyoxyethylene glycol 600 and 6,000 1: 1 was prepared and ground in a bead mill for 2 hours. The dispersion is then heated to 95 ° C, transferred to a high speed homogenizer and a molten mixture of Bralen SA 200 polyethylene, AO 49 stabilizer and polyethylene oil in a ratio of 2: 2: 1 is added. After homogenization, cooling and separation, a surface-treated pigment is obtained which, after drying under vacuum, shows an increased color strength.

Příklad 5Example 5

K 20 dielom mletého pigmentu yellow 147 vo forme 1 %-nej vodnej disperzie sa pri teplote 40 °C přidá 20 dielov roztavenej zmesi polyetylénu Bralen SA 200, dioktylftalátu a polypropylénového oleja K 1000 v pomere 2:1:2. Zmes sa potom homogenizuje pri vysokých otáčkách 5 min. Po vytvoření jemných granuliek povrchovo upravený pigment sa odfiltruje a vysuší pri 60 °C do konštantnej hmotnosti. Upravený pigment sa vyznačuje vyššou farebnou silou.To 20 parts of ground pigment yellow 147 in the form of a 1% aqueous dispersion is added at 40 DEG C. 20 parts of a molten mixture of polyethylene Bralen SA 200, dioctyl phthalate and polypropylene oil K 1000 in a ratio of 2: 1: 2. The mixture is then homogenized at high speed for 5 minutes. After the formation of fine granules, the surface-treated pigment is filtered off and dried at 60 ° C to constant weight. The modified pigment is characterized by a higher color strength.

CS 267 060 BlCS 267 060 Bl

Postupom ako v příklade 5, s tým rozdielom, že sa pre povrchová úpravu použije pigment yellow 95 vo forme 1 %-nej disperzie o teplote 25 °C. Pigment sa vyznačuje zlepšenou filtroPříklad 6 vatelnosťou v tavenine polyméru a vyššou farebnou silou.By the procedure as in Example 5, except that pigment yellow 95 in the form of a 1% dispersion at 25 DEG C. is used for the surface treatment. The pigment is characterized by improved filterability of the polymer melt and a higher color strength.

Claims (1)

’ PREDMET VYNÁLEZUOBJECT OF THE INVENTION SpSsob povrchovej úpravy pigmentov pre polyolefíny vyznačujúci sa tým, že pigment sa melie vo vodnom prostředí a homogenizuje pri teplote 70 až 100 °C s roztavenou trojzložko.vou zmesou vysokomolekulového polyolefinů s molekulovou hmotnosťou 2 000 až 50 000, dialkylftalátu s počtom uhlíkov v alkylreťazci 4 až 8 alebo neprchavého alkylderivátu fenolu alebo benzofenónu s počtom uhlíkov v alkylreťazci 4 až 35, a nízkomolekulového polyolefinů s molekulovou hmotnosťou 600 až 1 500, v pomere od 2,3:0,7:2 do 2:2:1 hmot, dielov.Method for coating pigments for polyolefins, characterized in that the pigment is ground in an aqueous medium and homogenized at a temperature of 70 to 100 ° C with a molten three-component mixture of high molecular weight polyolefins with a molecular weight of 2,000 to 50,000, dialkyl phthalate with carbon number in the alkyl chain. to 8 or a non-volatile alkyl derivative of phenol or benzophenone having a carbon number in the alkyl chain of 4 to 35, and low molecular weight polyolefins having a molecular weight of 600 to 1,500, in a ratio of from 2.3: 0.7: 2 to 2: 2: 1 by weight.
CS863830A 1986-05-26 1986-05-26 Method of pigments' surface treatment for polyolefins CS267060B1 (en)

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