公开(公告)号：US4705572A

公开(公告)日：1987-11-10

申请号：US872542

申请日：1986-06-09

申请人： Ernst Spietschka ,  Manfred Urban

发明人： Ernst Spietschka ,  Manfred Urban

IPC分类号： C09B3/60 ,  C09B67/10 ,  C09B67/54 ,  C08K5/08

CPC分类号： C09B67/0014 ,  C09B3/60

摘要： Process for the preparation of pigments of the anthanthrone series of the formula ##STR1## in which R.sub.1 and R.sub.2 denote chlorine, bromine or iodine atoms or C.sub.1 -C.sub.4 -alkoxy groups, having valuable properties, which comprises first converting the anthanthrones of the formula mentioned, in the form of the crude pigment, in an aqueous alkaline medium and at a pH>10, into the leucoform, precipitating the latter by adding inorganic or organic acids, reoxidizing the aqueous suspension of the leuco-form to give the anthanthrones and subjecting the resulting finely divided pre-pigments of the formula mentioned to a solvent finish.

摘要翻译： 制备式“IMAGE”的蒽醌系列颜料的方法，其中R1和R2表示氯，溴或碘原子或具有有价值性质的C1-C4-烷氧基，其包括首先将所述式的蒽醌转化 以粗颜料的形式，在碱性水溶液中并且在pH> 10的情况下，加入到无色或无机酸中，通过加入无机酸或有机酸沉淀后者，再次将无色形式的水悬浮液再氧化，得到蒽醌并经受 得到的所分配的细分前述颜料与溶剂完成。

公开(公告)号：US4614803A

公开(公告)日：1986-09-30

申请号：US738577

申请日：1985-05-28

申请人： Ernst Spietschka ,  Manfred Urban

发明人： Ernst Spietschka ,  Manfred Urban

IPC分类号： C07D221/14 ,  C07D221/04

CPC分类号： C07D221/14

摘要： Process for the preparation of dry alkali metal salts of 1,8-naphthalimide, which comprises allowing concentrated alkali metal hydroxide solutions to run into solid 1,8-naphthalimide in a molar ratio, at a rate corresponding to the degree of reaction, with vigorous stirring in vacuo at an elevated internal temperature, and then carrying out drying without intermediate isolation of the alkali metal salt formed.

摘要翻译： 制备1,8-萘二甲酰亚胺的干碱金属盐的方法，其包括使浓缩的碱金属氢氧化物溶液以相当于反应程度的摩尔比以强烈的摩尔比进入固体1,8-萘二甲酰亚胺 在升高的内部温度下在真空中搅拌，然后进行干燥而不中间分离形成的碱金属盐。

公开(公告)号：US4588814A

公开(公告)日：1986-05-13

申请号：US601862

申请日：1984-04-19

申请人： Ernst Spietschka ,  Manfred Urban

发明人： Ernst Spietschka ,  Manfred Urban

IPC分类号： C07D471/06 ,  C09B5/62 ,  C07D221/14

CPC分类号： C07D471/06 ,  C09B5/62

摘要： Preparation of 3,4,9,10-perylenetetracarboxylic acid diimide by fusing naphthalene-1,8-dicarboxylic acid imide with potassium hydroxide and sodium acetate to give the alkali metal salt of the leuko compound of 3,4,9,10-perylenetetracarboxylic acid diimide, diluting the melt with water when the reaction has ended and oxidizing the leuko form to give the 3,4,9,10-perylenetetracarboxylic acid diimide, by a procedure which comprises(a) applying a vacuum of less than 100 mm Hg before the naphthalene-1,8-dicarboxylic acid imide is introduced into the potassium hydroxide/sodium acetate melt, heating the potassium hydroxide/sodium acetate mixture to 200.degree.-300.degree. C. and dehydrating it such that the melt is still stirrable at 200.degree.-220.degree. C., and then introducing the naphthalene-1,8-dicarboxylic acid imide or its sodium or potassium salt into the melt at 200.degree.-220.degree. C. under normal pressure and heating the mixture at 250.degree.-300.degree. C. in the absence of atmospheric oxygen, or(b) applying a vacuum of less than 100 mm Hg after the naphthalene-1,8-dicarboxylic acid imide or its sodium or potassium salt has been introduced into the potassium hydroxide/sodium acetate melt at 200.degree.-220.degree. C. under normal pressure, heating the mixture to 200.degree.-250.degree. C. and dehydrating it such that the melt is still stirrable at 200.degree.-220.degree. C., and then heating the melt at 250.degree.-300.degree. C. in the absence of atmospheric oxygen, or(c) introducing the sodium or potassium salt of naphthalene-1,8-dicarboxylic acid imide into the potassium hydroxide/sodium acetate melt at 200.degree.-220.degree. C. under normal pressure and heating the melt at 250.degree.-300.degree. C. in the absence of atmospheric oxygen.

摘要翻译： 通过将萘-1,8-二羧酸酰亚胺与氢氧化钾和乙酸钠混合制备3,4,9,10-苝四羧酸二酰亚胺，得到3,4,9,10-苝四羧酸的白化合物的碱金属盐 酸二酰亚胺，当反应结束时用水稀释熔体，并通过包括（a）施加小于100mm Hg的真空的方法氧化白细胞形式得到3,4,9,10-苝四羧酸二酰亚胺 在将萘-1,8-二羧酸酰亚胺引入氢氧化钾/乙酸钠熔体中之前，将氢氧化钾/乙酸钠混合物加热到200-300℃，并将其脱水，使得熔体在200℃仍然可搅拌 ℃-220℃，然后在常压下在200-220℃下将萘-1,8-二羧酸酰亚胺或其钠或钾盐引入熔体中，并在250-300℃下加热该混合物 在没有大气氧的情况下，或（b） 在萘-1,8-二羧酸酰亚胺或其钠或钾盐在常压下在200-220℃下加入到氢氧化钾/乙酸钠熔体中，施加小于100mm Hg的真空，加热 该混合物在200-250℃下脱水，使得熔体仍然在200-220℃下搅拌，然后在不存在大气氧的条件下在250-300℃下加热熔体，或 （c）在常压下在200-220℃下将萘-1,8-二羧酸酰亚胺的钠盐或钾盐引入氢氧化钾/乙酸钠熔体中，并在250-300℃加热熔融物。 在没有大气氧气的情况下。

公开(公告)号：US4431806A

公开(公告)日：1984-02-14

申请号：US261927

申请日：1981-05-08

申请人： Ernst Spietschka ,  Manfred Urban

发明人： Ernst Spietschka ,  Manfred Urban

IPC分类号： C09B5/62 ,  C07D471/06 ,  C09B67/04 ,  C09B67/14 ,  C09B67/20 ,  D06P1/44 ,  C09B3/14 ,  C09B67/00

CPC分类号： C09B67/0017 ,  C09B67/0002

摘要： Very pure, transparent pigments of high color strength, of the formula ##STR1## in which R is hydrogen or alkyl having 1 to 4 C atoms, X is chlorine and/or bromine and n is a number from 0 to 4 are obtained by converting the corresponding crude pigment to the sulfate, isolating the sulfate, liberating the pure product from the sulfate by hydrolysis, separating off the pure product and dry milling the anhydrous material, with or without additives and with or without subsequent solvent finishing. These pigments are suitable for coloring paints and plastic compositions, especially for pigmenting metallic paints.

摘要翻译： 具有高着色强度的非常纯的透明颜料，其中R为氢或具有1至4个C原子的烷基，X为氯和/或溴，n为0至4的数的式“IMAGE”通过转化 将相应的粗颜料与硫酸盐分离，分离出硫酸盐，通过水解从硫酸盐中释出纯产物，分离纯产物，并干燥研磨无水材料，加入或不添加添加剂，并进行或不进行后续溶剂整理。 这些颜料适用于着色油漆和塑料组合物，特别是用于着色金属涂料。

公开(公告)号：US4229583A

公开(公告)日：1980-10-21

申请号：US959446

申请日：1978-11-13

申请人： Ernst Spietschka ,  Manfred Urban

发明人： Ernst Spietschka ,  Manfred Urban

IPC分类号： C09B7/10 ,  C09B7/00

CPC分类号： C09B7/10

摘要： Thioindigo and its derivatives are obtained in high yield and excellent purity by oxidizing corresponding 3-hydroxythionaphthenes with peroxo-disulfate in an aqueous alkaline solution.

摘要翻译： 通过在碱性水溶液中氧化相应的3-羟基硫茚与过氧二硫酸盐，可以高产率和高纯度获得硫靛及其衍生物。

公开(公告)号：US4689087A

公开(公告)日：1987-08-25

申请号：US796514

申请日：1985-11-08

申请人： Ernst Spietschka ,  Manfred Urban

发明人： Ernst Spietschka ,  Manfred Urban

IPC分类号： C09B67/10 ,  C09B7/00

CPC分类号： C09B67/0014

摘要： A process for the preparation of 4,4',7,7'-tetrachloro-thioindigo pigment which comprises treating a finely divided crude 4,4',7,7'-tetrachloro-thioindigo pigment in anhydrous form at temperatures of from 50.degree. to 180.degree. C. with a nitroaromatic substance which is volatile in steam and has a melting point of 50.degree. C. or below under normal conditions.

摘要翻译： 一种制备4,4'，7,7'-四氯硫代靛蓝颜料的方法，该方法包括在50℃的温度下处理无水形式的细碎的4,4'，7,7'-四氯硫靛红颜料 与硝基芳族物质在蒸气中挥发，在正常条件下具有50℃或更低的熔点。

公开(公告)号：US4650879A

公开(公告)日：1987-03-17

申请号：US872127

申请日：1986-06-09

申请人： Ernst Spietschka ,  Manfred Urban

发明人： Ernst Spietschka ,  Manfred Urban

IPC分类号： C07D493/06 ,  C07C51/54 ,  C07C51/56 ,  C07D311/78

CPC分类号： C07C51/54 ,  C07C51/56

摘要： Process for the preparation of perylene-3,4,9,10-tetracarboxylic dianhydride of high purity and in a very good yield in an ecologically unobjectionable manner, which comprises saponifying perylene-3,4,9,10-tetracarboxylic acid diimide with a 2.5-fold to 6-fold amount by weight of 92.5% to 97.5% strength sulfuric acid at temperatures of 210.degree. to 230.degree. C., washing the resulting mixture of perylene-3,4,9,10-tetracarboxylic dianhydride and perylene-3,4,9,10-tetracarboxylic acid monoanhydride-monoimide with a 0-fold to 4-fold amount by weight of 80-95% strength sulfuric acid, and then washing it with water until it is neutral, converting the compounds present in the mixture into their potassium salts by means of potassium hydroxide, after removing the perylene-3,4,9,10-tetracarboxylic acid monoanhydride-monoimide, adding to the solution of the tetrapotassium salt of perylene-3,4,9,10-tetracarboxylic acid, under nitrogen and with the exclusion of air and light, a salt of iron, nickel, calcium, magnesium, aluminum, tin, copper, lead, zinc or manganese, suspended or dissolved in water, and allowing this salt to act at a pH>10 and at temperatures from 0.degree. to 100.degree. C., then clarifying the mixture and converting the tetrapotassium salt of perylene-3,4,9,10-tetracarboxylic acid by acidification into perylene-3,4,9,10-tetracarboxylic dianhydride and isolating the latter in a customary manner.

摘要翻译： 以生态无损的方式制备高纯度和非常好的收率的苝-3,4,9,10-四羧酸二酐的方法，其包括将苝-3,4,9,10-四羧酸二酰亚胺皂化 在210-230℃的温度下，硫酸浓度为2.5倍至6倍重量的92.5％至97.5％的硫酸，洗涤得到的苝-3,4,9,10-四羧酸二酐和苝 - 3,4,9,10-四羧酸单酐，具有0-至4倍重量的80-95％强度的硫酸，然后用水洗涤直到其为中性，将存在于 在除去苝-3,4,9,10-四羧酸单酐之后，通过氢氧化钾将其混合成它们的钾盐，加入苝-3,4,9,10-四羧酸四钾盐的溶液， 四羧酸，在氮气下，排除空气和光，铁，镍，钙的盐 铁，镁，铝，锡，铜，铅，锌或锰，悬浮或溶解在水中，并使该盐在pH> 10和0℃至100℃的温度下起作用，然后澄清混合物和 通过酸化将苝-3,4,9,10-四羧酸的四钾盐转化成苝-3,4,9,10-四羧酸二酐，并以常规方式分离后者。

公开(公告)号：US4655845A

公开(公告)日：1987-04-07

申请号：US770698

申请日：1985-08-29

申请人： Ernst Spietschka ,  Manfred Urban

发明人： Ernst Spietschka ,  Manfred Urban

IPC分类号： C09B67/14 ,  C04B14/00

CPC分类号： C09B67/0017

摘要： Process for preparing organic pigments having excellent application properties, which comprises treating finely divided crude pigments of the anthanthrone, pyranthrone, isoviolanthrone, azo, quinacridone, flavanthrone, indanthrone, naphthaldazine, indigo, thioindigo, tetracarboximide, dioxazine, isoindolinone, perylene, anthrapyrimidine, acylanthraquinone, dianthraquinonyl, azoanthraquinone, azomethineanthraquinone and phthalocyanine series at temperatures of 0.degree. C. to 100.degree. C., with acid esters of polyphosphoric acid and a primary, secondary or tertiary alkanol of 1 to 8 carbon atoms, a glycol, glycol ether or phenol, then hydrolyzing the polyphosphate ester used, heating the resultant aqueous mixture to temperatures of 20.degree. C. to 150.degree. C., and isolating the pigment in conventional manner.

摘要翻译： 用于制备具有优异应用性能的有机颜料的方法，其包括处理蒽醌，吡喃酮，异喹喔酮，偶氮，喹吖啶酮，黄烷酮，阴丹酮，萘并嗪，靛蓝，硫靛，四甲酰亚胺，二恶嗪，异吲哚啉酮，苝，蒽吡啶，酰基蒽醌 ，蒽醌，偶氮蒽醌，偶氮甲蒽醌和酞菁系列，在0℃至100℃的温度下，与多磷酸的酸酯和1至8个碳原子的伯，仲或叔烷醇，二醇，二醇醚或苯酚 然后水解所使用的多磷酸酯，将所得含水混合物加热至20℃至150℃的温度，并以常规方式分离颜料。

公开(公告)号：US4460410A

公开(公告)日：1984-07-17

申请号：US451822

申请日：1982-12-21

申请人： Ernst Spietschka ,  Manfred Urban

发明人： Ernst Spietschka ,  Manfred Urban

IPC分类号： C09D5/38 ,  C09B3/18 ,  C09B67/10 ,  C04B31/00 ,  C07D311/02 ,  C09D11/00

CPC分类号： C09B67/0014 ,  C09B3/18

摘要： A perylene-3,4,9,10-tetracarboxylic acid dianhydride pigment, useful as a varnish pigment, made by adding an aqueous solution of an alkali metal salt of perylene-3,4,9,10-tetracarboxylic acid and a surfactant to an acid at a pH below 3, at 0.degree. C. to 90.degree. C., and then heating the suspension so obtained at 50.degree. C. to 150.degree. C.

摘要翻译： 通过将苝-3,4,9,10-四羧酸的碱金属盐的水溶液和表面活性剂加入到作为清漆颜料的苝-3,4,9,10-四羧酸二酐颜料 在0℃〜90℃下，pH低于3的酸，然后将在50℃至150℃下得到的悬浮液加热。

公开(公告)号：US4617403A

公开(公告)日：1986-10-14

申请号：US627770

申请日：1984-07-05

申请人： Ernst Spietschka ,  Manfred Urban

发明人： Ernst Spietschka ,  Manfred Urban

IPC分类号： C09B7/00 ,  C09B7/10 ,  C07D333/64 ,  C07D409/04

CPC分类号： C09B7/10

摘要： Process for preparing a strong, non-flocking and rheologically excellent 4,4',7,7'-tetrachlorothioindigo pigment in high yields and high purity, which comprises(a) reacting 2,5 -dichlorophenylthioglycoloyl chloride with Friedel-Crafts catalysts in inorganic acyl halides of medium oxidation state as diluent as temperatures of -20.degree. to +50.degree. C. to 4,7-dichloro-3-oxythionaphthene,(b) oxidizing the resulting 4,7-dichloro-3-oxythionaphthene in a conventional manner to crude 4,4',7,7'-tetrachlorothioindigo, and(c) treating the crude 4,4',7,7'-tetrachlorothioindigo obtained in moist form with an aromatic solvent at 80.degree. to 180.degree. C. in the presence of an aqueous alkali solution and a surface-active compound.

摘要翻译： 以高产率和高纯度制备强的非植绒和流变学优异的4,4'，7,7'-四氯硫靛素颜料的方法，其包括（a）使2,5-二氯苯硫基乙酰氯与Friedel-Crafts催化剂在无机 作为稀释剂的中等氧化态的酰基卤作为-20℃至+ 50℃至4,7-二氯-3-氧代硫茚的温度，（b）以常规方式氧化所得的4,7-二氯-3-氧硫羰 到粗品4,4'，7,7'-四氯硫靛素，和（c）在80-180℃下，用芳族溶剂处理湿润形式的粗品4,4'，7,7'-四氯硫靛素， 存在碱性水溶液和表面活性化合物。