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11. 发明授权

US4705572A Process for the preparation of pigments of the anthanthrone series 失效
标题翻译：制备蒽醌系列颜料的方法
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。

12. 发明授权

US4614803A Process for the preparation of dry alkali metal salts of 1,8-naphthalimide 失效
标题翻译：制备1,8-萘二甲酰亚胺的干碱金属盐的方法
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。

13. 发明授权

US4588814A Process for the preparation of 3,4,9,10-perylenetetracarboxylic acid diimide 失效
标题翻译：制备3,4,9,10-苝四羧酸二酰亚胺的方法
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。

14. 发明授权

US4431806A Process for the preparation of pigments of the perylene-3,4,9,10-tetracarboxylic acid diimide series, and their use 失效
标题翻译：苝-3,4,9,10-四羧酸二酰亚胺系列颜料的制备方法及其用途
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。

15. 发明授权

US4229583A Process for preparing thio-indigo dyestuffs 失效
标题翻译：制备硫靛蓝染料的方法
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。

16. 发明授权

US4689087A Process for the preparation of an organic pigment on the basis of 4,4',7,7'-tetrachloro-thio-indigo 失效
标题翻译：基于4,4'，7,7'-四氯硫代靛蓝制备有机颜料的方法
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。

17. 发明授权

US4650879A Process for the preparation of perylene-3,4,9,10-tetracarboxylic dianhydride 失效
标题翻译：制备苝-3,4,9,10-四羧酸二酐的方法
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。

18. 发明授权

US4009180A Continuous process for preparing copper phthalocyanine 失效
标题翻译：制备铜酞菁的连续工艺
公开(公告)号：US4009180A
公开(公告)日：1977-02-22
申请号：US415633
申请日：1973-11-14
申请人： Walter Deucker , Ernst Spietschka , Dieter Steidl
发明人： Walter Deucker , Ernst Spietschka , Dieter Steidl
IPC分类号： C09B47/067 , C09B67/00 , C09B47/04
CPC分类号： C09B67/0032 , C09B47/067
摘要： A continuous process for preparing copper phthalocyanines by caking a mixture of phthalodinitrile, and a copper salt which comprises carrying out the reaction in a continuously working, heatable, tubular vibration mill, which contains iron or steel bars in the grinding room.In comparison with the continuous processes hitherto known this process requires a considerably smaller amount of thermal energy from outside, since the amount of heat formed in the strongly exothermic condensation process is, to a considerable extent conducted away from the reaction zone, with the aid of heat-conducting grinding bars, and is used in order to heat up the freshly introduced starting product to room temperature.
摘要翻译：通过结合酞腈和铜盐的混合物制备铜酞菁的连续方法，其包括在连续加工的可加热的管式振动研磨机中进行反应，该研磨机在研磨室中含有铁棒或钢棒。

19. 发明授权

US4732618A Powdered pigments with improved rheological properties, processes for their preparation and their use with a content of at least 5% of unsubstituted quinacridone 失效
标题翻译：具有改善流变性能的粉末颜料，其制备方法及其用量至少5％未取代喹吖啶酮
公开(公告)号：US4732618A
公开(公告)日：1988-03-22
申请号：US902444
申请日：1986-08-11
申请人： Ernst Spietschka , Adolf Kroh , Otmar Hafner
发明人： Ernst Spietschka , Adolf Kroh , Otmar Hafner
IPC分类号： B05D7/24 , C08J3/22 , C08K9/04 , C08K9/10 , C09B67/00 , C09B67/08 , C09B67/20 , C09D7/12 , C09D17/00
CPC分类号： C09D17/003 , C09B67/0004 , C09B67/0063
摘要： Powdered pigments which contain at least 5% of unsubstituted quinacridone and have improved rheological properties for use in paint systems on an alkyd/melamine, acrylic/melamine, acrylate/isocyanate or polyester/isocyanate basis, both of a conventional nature and also of a modern nature of the "high solids" type, onto which--as appropriate before, during or after finishing--1 to 20% by weight of the active substance of a paint additive, prepared by reacting polyisocyanurates which still carry free isocyanate groups and are based on tolylene diisocyanate, hexamethylene diisocyanate or mixtures thereof, with (1) aliphatic mono- or poly-(hydroxycarboxylic acid) C.sub.1 -C.sub.20 -alkyl esters (degree of polymerization 2-50), (2) polyethylene glycols (molecular weight 500-1,500) and (3) 5- or 6-membered, saturated or unsaturated heterocyclic compounds which contain at least 1 nitrogen atom in the ring and reactive amino or hydroxy-C.sub.1 -C.sub.6 -alkyl groups, until isocyanate groups are no longer detectable, has/have been applied, processes for their preparation and their use for pigmenting polymeric materials and for coloring paint systems.
摘要翻译： PCT No.PCT / EP85 / 00700 Sec。 371日期：1986年8月11日 102（e）日期1986年8月11日PCT提交1985年12月12日PCT公布。公开号WO86 / 03763 日期：1986年7月3日。含有至少5％的未取代喹吖啶酮并具有改善的流变性能的粉末颜料，用于在醇酸/三聚氰胺，丙烯酸/三聚氰胺，丙烯酸酯/异氰酸酯或聚酯/异氰酸酯基础上的涂料体系中常规性质以及“高固体”类型的现代性质，其中适当的是在整理之前，之中或之后 - 将1-20重量％的仍然携带的聚异氰脲酸酯制备的涂料添加剂活性物质游离异氰酸酯基团，基于甲苯二异氰酸酯，六亚甲基二异氰酸酯或其混合物与（1）脂族单 - 或聚 - （羟基羧酸）C 1 -C 20烷基酯（聚合度2-50），（2）聚乙二醇（分子量500-1,500）和（3）5-或6-元饱和或不饱和的杂环化合物，其在环中含有至少1个氮原子，反应性氨基或羟基-C 1 -C 6 - 烷基直到异氰酸酯基为没有喔更高可检测，已经被应用，它们的制备方法以及它们用于着色聚合物材料和着色涂料体系的用途。

20. 发明授权

US4693753A Pigments of the quinacridonequinone series, process for their preparation and their use 失效
标题翻译：喹吖啶酮系列的颜料，其制备方法及其用途
公开(公告)号：US4693753A
公开(公告)日：1987-09-15
申请号：US905672
申请日：1986-09-09
申请人： Ernst Spietschka , Frank Prokschy
发明人： Ernst Spietschka , Frank Prokschy
IPC分类号： C09B67/20 , C09B67/22 , C04B14/00
CPC分类号： C09B67/0036
摘要： Pigments of the quinacridonequinone series comprising 99-30 mole percent of a quinacridonequinone of the formula (1) ##STR1## in which R denotes a hydrogen or chlorine atom or a methyl group, 0-60 mole percent of a quinacridone of the formula (2) ##STR2## in which R has the above-mentioned meaning, and 1-10 mole percent of a 7,15-dihydro-pyrido-(2,1-b)-(1',2'; 1,2)-pyrimido-(4,5-g)-quinazoline-7,15-dione of the formula (3) ##STR3## in which R has the above-mentioned meaning, the added compounds of the formulae (2) and (3) being present in the crystal lattice of the quinacridonequinone of the formula (1), process for their preparation and their use for coloring plastic materials and for preparing automotive paints for metallic coatings.
摘要翻译：喹吖啶酮醌系颜料，其包含99-30摩尔的式（1）的喹吖啶酮醌其中R表示氢或氯原子或甲基，0-60摩尔％的式（2）的喹吖啶酮）（2）其中R具有上述含义，并且1-10摩尔％的7,15-二氢 - 吡啶并 - （2,1-b） - （1'，2'; 1' 2） - 嘧啶并 - （4,5-g） - 喹唑啉-7,15-二酮，其中R具有上述含义，加入式（2）的化合物）和（3）存在于式（1）的喹吖啶酮的晶格中，其制备方法及其用于着色塑料材料和用于制备金属涂料的汽车漆。

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