• 专利附录
  • 专利说明
  • 权利要求
  • 类似技术
  • 同族专利
  • 引用文献
  • 法律状态
  • 优先权
    • 专利摘要:
    THE METHOD FOR OBTAINING GRANULATED PIGMENT for the treatment of azphthalocyanine pigment or azolac by means of euhmcim followed by treatment with shneralic acid and further granule formation, which is similar to that, the pattern can be put on a pathway. rosin, disproportionating rosin, hydrogenated kaifol or a mixture of the latter, or the product of co-oxidant formaldehyde and rosin with softening temperature of 6073 ° C and k Synthesis No. 4 in the amount of 145-165 in the amount of 38-67 wt.% per granulate, and the treatment is carried out with 31% hydrochloric acid to a pH of 2-5 with the introduction of 0.2 to 2.0 wt. tetrakis 3-
    公开号:SU1145933A3
    申请号:SU813369303
    申请日:1981-10-20
    公开日:1985-03-15
    发明作者:Дойбель Райнхольд；Уде Криста；Маркс Вернер
    申请人:Хехст Аг (Фирма)；
    IPC主号:
    专利说明:

    The invention relates to the technology of injection forms and preparations of organsshish pigments and dyes, in particular, to a method for producing a granular pigment used in inks for high offset and gravure printing.
    The closest to the technical essence of the proposed method is a method of obtaining a granulated pigment by treating a suspension of azo or phthalocyanine pigment or aeolac in water or an organic solvent with a binder solution of a resin from the group of synthetic or natural polymers, for example polyacryl resins, and dextrin that is soluble in water, used by ush organic solvent, followed by treatment of the resulting mass of mineral, in particular, sulfuric acid, coprecipitation of the pigment and binder in the form of granules, szgshkoy at 90-120 C and the further extension of the granule tlj.
    The disadvantages of this method are the low color intensity and dispersibility of the granulate, as well as the complexity of the technological process associated with the additional stage of granulation of the powdered pigment.
    The purpose of the invention is to increase the color intensity and dispersibility of the granulate and simplify the process.
    Ukazayna object is achieved in that the process for producing a granular pigment by treating azoftalotsianynovogo pigment or azolaka binder followed by treatment with a mineral acid and further vscheleniem granulate, as a binder is used ka nifoL, disproportionated Kani Fol, hydrogenated rosin or a mixture of the latter, or a condensation product of formaldehyde and rosin with a softening temperature of 60-73 0 and an acid number of 145-165 in the amount of 38-67 wt.% per granulate, and the treatment is carried out with 31% hydrochloric acid about pH 2-5 with the introduction of 3,2 (3,5-di-tert-butyl-4-hydroxyphenyl) propionate into a mixture of 0.22, 0 wt.%, pentaerythrityl-tetrakis, carrying out the phpashing process at 70-90 C and additionally with steam treatment at,
    Natural and synthetic resins, which are soluble in an aqueous-alkaline medium, are used as resins; however, they are insoluble in the acidic pH region. Due to the wide compatibility with the usual binders for printing inks, as well as their low softening temperature, rosin, disproportionated or hydrogenated rosin, as well as rosin derivatives are used as resins in the proposed method. The amount of resin and temperature peKMvf is determined by the resin used in each case.
    To prevent thermal oxidation processes in the resins of highly dispersed pigment granules, antioxidants of 0.1-2 wt.%, In particular pentaerythrityl-tetrakis-3- (3, 5-ditert-butyl4-hydroxyphenyl) propionate, are used.
    The proposed method is carried out with conventional pigments, which are used mainly for printing inks, for example, azo pigments, lacophore azo pigments and phthalocyanine pigments.
    The granulate pigments obtained according to the invention are non-flammable and well dispensed. They can easily be dispersed in the medium used and, for example, in printing inks, they exhibit a very high crush capacity, good transparency and low viscosity.
    Compared to the known method of producing such granulates, the method is simple and it is carried out in the suspension formed during the synthesis of the pigment without the addition of solvents, organic acids or other auxiliary agents that need to be additionally removed or regenerated again. In the proposed method some organic matter can be used. solvents when using pigment suspensions that contain a known amount of such solvents, or if the alkaline solution of the resin with erzhit, for example, water-miscible solvent, such as low molecular weight alcohols or ketones which may act as mediators dissolution.
    The flushing process is carried out at a temperature up to, if possible, in an open vessel. It is advisable to heat the mixture by introducing steam.
    In the following examples, parts and percentages are by weight. The weight and volume parts are, respectively, kilograms and liters.
    Example 1. By combining with a pH of 5.5-5.7, a pigment suspension of 47 h, a yellow pigment, (azo pigment) (C, 1. 21090) is obtained in a final cupellation of 2100 h. The mass is neutralized with a dilute caustic solution soda and add 52 h, disproportionate rosin, not containing abietic acid and containing 45-554 dihydroabietic acid (softening temperature acid number 150) in the form of a 10% solution in caustic soda, as well as an antioxidant add 1 h, pentaerythritol 1-tetrakis-3- (3,5-ditretbu tyl-4-hydroxy-1) propionate. After that, 31% hydrochloric acid is added to and, with gentle stirring, 31% hydrochloric acid is added to obtain a pH of 4, and a granulate is formed in the flushing process. Upon subsequent heating by direct. Steam before this process ends. The product is filtered off at 6 ° C, washed with salt-free water, dried at 60 ° C in a chamber air circulation dryer. 99 parts of a granular granulate with a particle diameter of about 1-4 mm are obtained. This granulate is easily processed with standard varnish for high or offset printing into printing ink, which (apart from 53% resin components) with good transparency and good gloss gives a colored impression that is weaker than printing ink made with an equal amount of weight. the original pigment.
    Example 2. The method is carried out as in example 1, but instead of disproportionating rosin, an extraction rosin with a softening temperature of 75 ° C and an acid number of 165 is used. A well-formed granulate is obtained.
    Example 3 By coupling at pH 5.5-5.7, a pigment suspension of 60 parts of yellow pigment 13 (C, t, 21100) is obtained in a final cupellation volume of 1500 hours. Neutralized with a dilute sodium hydroxide solution and added at 39 including disproportionate rosin in the form of a solution in caustic soda solution. The mixture is then heated by directly introducing steam up to and over the pot at this temperature for 2 hours. After cooling the reaction mixture to 80 ° C, 1 hour of antioxidant used in Example 1 is added and, after addition of hydrochloric acid, processed into Example 1 into granulate (100 hours). If printing ink is obtained from equal weight amounts of the granulate and the initial pigment, then the color comparison shows approximately the same dyeing abilities, and the ink obtained from the granulate is higher in transparency and gloss.
    Example 4 A combination of 50 parts of a mixed product consisting of a 3,3-dichloro4, 4-diaminobiphenyl diazonium compound and a mixture of 0.4 mol 1 is obtained by combination at a pH of 5.5-5.7 and 20 ° C. -acetoacetyl-amino-2-methoxybenzene and 1.6 mol of acetoacetylamino-2,4-dimethylbenzene in the final cupellation of 1500 hours.
    Neutralized with a dilute sodium hydroxide solution and at 38 hours, the disproportionate rosin used in Example 1 (softening point 73 ° C, acid number 150) is added in the form of a 10% solution in caustic soda. After this, the mixture is heated by direct injection of steam until it is kept at this temperature for 2 hours.
    i
    After cooling the reaction mixture to 80 ° C, the antioxidant used in Example 1 was added 2 hours and with weak stirring, 31% hydrochloric acid was quickly added to pH 4, and a granulate was formed in the flushing process. pair up to 98s this process ends. The product is filtered off, washed with salt-free water, and when dried in a chamber circulation with air circulation. 99.5 hours are obtained, of a granulate with a particle diameter of about 2-5 mm. With equal initial amounts, it is possible to compare the coloring ability of the granulate (60 parts of a pigment) and 100% of the initial pigment. The granulate obtained has an increased dye capacity. Example 5. Corresponding to example 4, 55 parts of pigment were used for 44 hours, rosin from gum turpentine (melting point 6065 ° C, acid number 165) and addition of hydrochloric acid was carried out at 98 ° C. 95 hours of a well-formed granulate are obtained. Example 6. In accordance with example 4, 49 hours, 49 hours of the pigment, the condensation product of formaldehyde and rosin obtained by high-pressure reaction, 100 hours, the kapifoli of example 5 and 10 hours of paraformaldehyde with softening temperature and acid number 145, were used in ec 50% solution in toluene 24 mPaS. The addition of acid is carried out at. 97 hours of well-formed granulate are obtained. Example 7 By combining in a pH range, decreasing from 5.8 to 3.5, a pigment suspension is obtained from 40 parts of a mixed product of a combination consisting of about 1 mole of the diazonium compound 1-amino-2-methoxybenzene 5-phenoamide carboxylic acid consumed with 80 mol.% (2-hydroxy-3-naphthoylamino) -2-methyl-5-chlorobenzene and 20 mAb.% (2-hydroxy 3-naphtho-1-chloro) 2, 5-dimethoxy-4-chlorobenzene per volume cupellation equal to 1800 hours. Using a concentrated solution of caustic soda, set pH 12 and add 59.8 hours of disproportionate rosin of Example 1 in ide alkaline solution. Then heat up by introducing steam to 98 ° C and extinguish for 2 hours at this temperature. After cooling the reaction mixture, 0.2 hours was added to the antioxidant used in Example 1 and after adding hydrochloric acid, the process of Example 1 was carried out to form a granulate ( 99 hours). Example 8. By combining and then forming a lacquer with the power of a calcium chloride solution at a pH of 9 to 7.8, a pigment suspension of 32 parts of the red 57: 1 red pigment (C, 1. 15850: 1) is obtained in the final volume of lacquering equal to 3000 hours. After 30 minutes of heating to 80 ° C, 1 part of antioxidant according to example 1 and 67 hours is added, the disproportionate rosin according to receiving 1 is in the form of an alkaline solution, and with weak stirring, 31% hydrochloric acid is slowly added dropwise until pH 3 After heating until the formed granulate is processed, ak in Example 1. Example 9, 32 parts of a pigment suspension of red pigment 57: 1, prepared according to example 8, is filtered off with suction and washed with salt-free water. The wet residue after filtration is stirred in water to form a 15% pigment slurry and mixed with 1 part of the antioxidant used in Example 1. After that, 67 parts of the disproportionate rosin of Example 1 are added with and with weak stirring, 31% hydrochloric acid is slowly added dropwise to pH 3. After heating, the granulate is treated as described in Example 1. Example 10. 55 hours copper semi-chlorophthalocyanine (Blue pigment Blue 15: 1 (CI 74160) in the form of an aqueous 30% filter residue is shaken as in Example 1 in a 10% solution containing 44 hours of the resin of Example 1 in a solution of caustic soda and the reaction mixture is heated direct injection of steam up for 2 4v then the pigment The suspension is cooled to 80 ° C and diluted with water to a solid content of 3%. After the addition of 1 hour, the antioxidant specified in Example 1, with a fast feed of 31% hydrochloric acid to pH 4, and with slow permeation, the formation of granules begins one that ends after heating to, Example 11, By combining: in the pH range, decreasing from 5.5 to .4.5, a pigment suspension of 50 parts of yellow pigment 83 (C.1.21108) is obtained in the final Yef. Cow cupellation volume equal to 1900 h.
    The pigment suspension is additionally stirred for approximately 15 minutes and the pH is set to tO with 33% sodium hydroxide solution and combined with a 30% solution containing 50 hours of the resin specified in Example 1 in sodium hydroxide solution. As a result of the rapid nourishment of 31% hydrochloric acid in the pH range from 4 to 5, granulate is formed and, after 15 minutes of heating, direct steam is completed to a temperature of 98 ° C. After treatment with the disproportionate rosin in accordance with Example 1, 99.5 homogeneous, formed, granular granules are obtained.
    Example 12. By combining in the range of pI 5-7 and lacquering at pH 6.5, a pigment suspension of 55 parts of the red pigment Red 53: 1 (0.1.15585: 1) is obtained in the final lacquering volume equal to 4 1100 hours. by do6aiBKH diluted caustic soda solution pH 10 and the resin indicated in Example 1, 45 is added in the form of a 25% solution in caustic solution. With a PS (by adding a rapid addition of 31% hydrochloric acid at 80 s, with p 2, after heating to 98 ° and processing disproportionate rosin. Example 98, 98 hours of well-formed grains are obtained, KOTopi easily dissolves in paints for aysokOC, offset and deep pecha, t.
    Example 13. In Example 1, the half of the used resin was replaced with an equal amount of the resin used in Example 2, and then it was worked with a mixture of resin. A well-formed pigment in the form of a granulate is obtained.
    According to the proposed method, I obtain granulated pigment directly in the process of making pigment. The additional stage of the overall process, starting from the aqueous suspension of the pigment as a result of applying the process of a single evaporation, displaces water from the surface of the pigment through the molten resin. With this, pigment particles remain in the state of the finest comminution, which are not caked among themselves, as occurs during the processing of the pigment into relatively difficult to disperse agglomerates according to the prototype method. At the same time, the resulting granulated product during its subsequent processing, for example, when applying a printed pattern, is easily dispersible and even with a high resin content (for example, 50-60% by weight) ensures a staining intensity that can only be achieved using the prototype method. a part of 100% pygmy1 | comrade without recalculation for the same pigment content. Production of powdered pigments with the indicated quality of coloring in relation to its intensity is impossible with the prototype method.
    权利要求:
    Claims (4)
    [1]
    A METHOD FOR PRODUCING A GRANULATED PIGMENT by treating azoft-cyanine pigment or azo-lacquer with a binder followed by treatment with mineral acid and further isolating the granulate, characterized in that, in order to increase the coloring and dispersibility of the granulate, to simplify the process as a binder use rosin, a disproportionate rosin, hydrogenated rosin or a mixture of the latter, or a condensation product of formaldehyde and rosin with a softening point of 6073 ° C and acid number 145-165 in the amount of 38-67 May.
    [2]
    2 per granulate, and the treatment is carried out with 312 hydrochloric acid to a pH of 2-5 with the introduction of the mixture on 0.2-2.0 May. 2 pentaerythritol-tetrakis [
    [3]
    3- (3,5-ditret-butyl-
    [4]
    4-oksifenip) -propionataZ by conducting Flushing process at 9O-7D * C and an additional treatment with steam at 98 C.
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    引用文献:
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    GB240852A|1924-10-01|1926-04-01|Hoechst Ag|Manufacture of finely subdivided pigment dyes|
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    US4175979A|1974-08-21|1979-11-27|Ciba-Geigy Corporation|Process for the manufacture of a pigment composition in bead form|
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    DE2745679C2|1977-10-11|1981-12-17|Hoechst Ag, 6000 Frankfurt|Pigment preparations, their manufacture and use|
    CA1096712A|1977-12-19|1981-03-03|Douglas W.T. Beattie|Pigment compositions and methods of preparation|
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    US6051060A|1997-12-04|2000-04-18|Marconi Data Systems, Inc.|Method of making pigment with increased hydrophilic properties|
    IT1315251B1|1999-10-21|2003-02-03|Great Lakes Chemical Europ|MIXTURES OF ADDITIVES FOR ORGANIC POLYMERS IN GRANULAR FORM|
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    法律状态:
    优先权:
    申请号 | 申请日 | 专利标题
    DE19803039642|DE3039642A1|1980-10-21|1980-10-21|METHOD FOR PRODUCING FIGURE GRANULES AND THEIR USE|
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