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    • 2. 发明授权
    • Use of a colorant solution containing a stable, at least partially neutralized chromium (III) coordination compound for coloring unglazed ceramic
    • 使用含有稳定的,至少部分中和的铬(III)配位化合物的着色剂溶液用于着色无釉陶瓷
    • US06352587B1
    • 2002-03-05
    • US09323140
    • 1999-06-01
    • Thomas StaffelJürgen StraubThomas Klein
    • Thomas StaffelJürgen StraubThomas Klein
    • C09C134
    • C04B41/5033
    • A process for coloring an unglazed ceramic with an aqueous colorant solution containing a chromium (III) coordination compound which is at least partially neutralized and stable, including (a) dissolving a carboxylic acid selected from the group consisting of acetic acid, an organic dicarboxylic acid having a general formula (COOH)—(CH2)n—(COOH), where n ranges from 0 to 10, and an unsaturated, organic dicarboxylic acid in water at a temperature ranging from 40 to 60° C. to provide an aqueous solution of a carboxylic acid; (b) adding a chromium (III) compound to the aqueous solution of a carboxylic acid while stirring for a time and at a temperature effective for reaction to form an aqueous solution containing a chromium (III) coordination compound; (c) filtering the aqueous solution containing the chromium (III) coordination compound to provide a filtered aqueous solution; and (d) adjusting pH of the filtered aqueous solution to a pH ranging from 3 to 6.5 by addition of one of alkali hydroxide or ammonia to provide the aqueous colorant solution containing a chromium (III) coordination compound which is at least partially neutralized, which is stable, and which has a chromium content ranging from 5 to 10% by weight.
    • 一种用含有至少部分中和并稳定的铬(III)配位化合物的含水着色剂溶液着色无釉陶瓷的方法,包括(a)将选自乙酸,有机二羧酸 具有通式(COOH) - (CH 2)n - (COOH),其中n为0至10,以及在40至60℃的温度范围内的不饱和有机二羧酸在水中的溶液,以提供水溶液 的羧酸; (b)向羧酸水溶液中加入铬(III)化合物,同时搅拌一段时间并在有效反应的温度下形成含有(III)配位化合物的水溶液; (c)过滤含有铬(III)配位化合物的水溶液以提供过滤的水溶液; 和(d)通过加入碱金属氢氧化物或氨来调节过滤的水溶液的pH至3至6.5的pH,以提供含有至少部分中和的铬(III)配位化合物的含水着色剂溶液,其中 是稳定的,并且其铬含量为5至10重量%。
    • 5. 发明授权
    • Method for coloring ceramic surfaces
    • 陶瓷表面着色方法
    • US6114054A
    • 2000-09-05
    • US142824
    • 1998-12-15
    • Thomas KleinThomas StaffelJurgen StraubLysander Fischer
    • Thomas KleinThomas StaffelJurgen StraubLysander Fischer
    • C04B33/14C04B41/50C04B41/52C04B41/85C04B41/87C04B41/89B32B9/00B05D1/38B05D3/02
    • C04B41/009C04B33/14C04B41/5007C04B41/5027C04B41/52C04B41/85C04B41/87C04B41/89C04B2111/82
    • A method for coloring a surface of a ceramic mass to produce a colored ceramic body includes providing a host lattice material composed of a colorless metal oxide compound which crystallizes into one of a spinel lattice or a rutile lattice and which may be water soluble; providing an aqueous coloring solution containing water; a first water soluble compound including a metal ion which is one of a two-valent metal ion or a three-valent metal ion and which colors the host lattice material; and a second water soluble compound including a metal ion which is one of a five-valent metal ion or six-valent metal ion and which provides electrostatic balance; generating a mixed-phase pigment in the surface of the ceramic mass by one of (i.) working a fine powder of the colorless metal oxide into the ceramic mass and applying the aqueous coloring solution onto at least one surface of the ceramic mass, or (i.i.) adding a water soluble colorless metal oxide compound to the aqueous coloring solution in an amount effective to form a mixture having a preselected viscosity and applying this mixture to the surface of the ceramic mass; drying the solution; and firing the ceramic body at a temperature ranging from 300 to 1400.degree. C. for a duration ranging from 0.5 to 5 hours.
    • PCT No.PCT / EP98 / 00136 Sec。 371 1998年12月15日第 102(e)1998年12月15日日期PCT提交1998年1月13日PCT公布。 公开号WO98 / 31647 日期:1998年7月23日一种用于着色陶瓷块的表面以制备着色陶瓷体的方法包括提供由无色金属氧化物化合物构成的主晶格材料,其结晶成尖晶石晶格或金红石晶格之一,并且可以是 水溶性; 提供含有水的着色溶液; 包含作为2价金属离子或3价金属离子之一的金属离子的第1水溶性化合物,使主体晶格材料变色; 和包含五价金属离子或六价金属离子之一的金属离子并提供静电平衡的第二水溶性化合物; 通过(i)将无色金属氧化物的细粉末加工到陶瓷块中并将水性着色溶液施加到陶瓷块的至少一个表面上,或者在陶瓷块的表面中产生混合相颜料,或 (ii)以有效形成具有预选粘度的混合物的量将水溶性无色金属氧化物化合物加入到水性着色溶液中,并将该混合物施加到陶瓷体的表面; 干燥溶液; 并在300〜1400℃的温度下烧制陶瓷体,持续时间为0.5〜5小时。
    • 6. 发明授权
    • Aqueous ruthenium chloride solution for blackening ceramic surfaces
    • 用于使陶瓷表面变黑的氯化钌水溶液
    • US6042884A
    • 2000-03-28
    • US11898
    • 1998-04-30
    • Thomas KleinThomas StaffelLysander Fischer
    • Thomas KleinThomas StaffelLysander Fischer
    • C04B33/34C04B41/50C04B41/85C04B41/87B05D3/02
    • C04B41/009C04B33/34C04B41/5072C04B41/85C04B2111/82
    • An aqueous ruthenium chloride solution for blackening ceramic surfaces includes ruthenium chloride; water present in an amount effective to provide an aqueous solution of ruthenium chloride; and a buffer which is selected from the group consisting of sodium acetate, sodium propionate, potassium acetate, potassium propionate, and mixtures thereof, and which is present in an amount effective to provide the aqueous solution with a pH of at least 1.5. A method for dyeing a ceramic surface includes applying the aqueous solution of ruthenium chloride to a ceramic surface by at least one of spraying, dipping, painting and printing to provide a treated surface; drying and firing the treated surface at a temperature ranging from about 300 to about 1400.degree. C. for a period of time ranging from one half hour to five hours; and grinding and polishing the treated surface to even out the treated surface.
    • PCT No.PCT / EP97 / 03087第 371日期:1998年4月30日 102(e)日期1998年4月30日PCT提交1997年6月13日PCT公布。 公开号WO97 / 49650 PCT 日期1997年12月31日用于使陶瓷表面变黑的氯化钌水溶液包括氯化钌; 以有效提供氯化钌水溶液的量存在水; 和选自乙酸钠,丙酸钠,乙酸钾,丙酸钾及其混合物的缓冲剂,其以有效提供水溶液至少1.5的pH的量存在。 用于染色陶瓷表面的方法包括通过喷涂,浸涂,喷涂和印刷中的至少一种将氯化钌水溶液施加到陶瓷表面以提供经处理的表面; 在约300至约1400℃的温度下干燥和烧制经处理的表面一段时间为半小时至五小时; 并研磨和抛光经处理的表面以使经处理的表面均匀。
    • 9. 发明授权
    • Process for the preparation of ammonium polyphosphate
    • 制备聚对苯二甲酸一铵的方法
    • US5139758A
    • 1992-08-18
    • US731541
    • 1991-07-17
    • Thomas StaffelRenate Adrian
    • Thomas StaffelRenate Adrian
    • C01B25/40
    • C01B25/405
    • To prepare essentially water-insoluble, chain-form ammonium polyphosphate from equimolar amounts of di- ammonium phosphate and phosphorus pentoxide in the presence of ammonia at temperatures of from 170.degree. to 350.degree. C. with constant mixing, kneading and comminution, at least some of the diammonium phosphate and phosphorus pentoxide is replaced by partially ammoniated polyphosphoric acid.A plant for carrying out this process can comprise a sealed reactor (1) which is provided with metering devices (2, 3) and feed tubes (4, 5) for phosphorus pentoxide and diammonium orthophosphate, an ammonia feed tube (8), an ammonium polyphosphate discharge tube (9) and a line for offgas. Rotatable mixing, kneading and comminution elements are provided inside the reactor (1). Furthermore, a heatable stirred tank (11) which can be charged with polyphosphoric acid via a feed line (13) is provided and can be used to remore water vapor and ammonia from the offgas flowing from the reactor (1) via the line (20) and from which partially ammoniated polyphosphoric acid can be introduced into the reactor (1) via an outlet line (17).
    • 在氨存在下,在170〜350℃的温度下,从等摩尔量的磷酸二氢铵和五氧化二磷基本上制备水不溶性的链状多磷酸铵,同时进行不断的混合,捏和和粉碎 的磷酸氢二铵和五氧化二磷被部分氨化的多磷酸代替。 用于进行该方法的设备可以包括密封反应器(1),该反应器设置有用于五氧化二磷和正磷酸二铵的计量装置(2,3)和进料管(4,5),氨进料管(8), 多磷酸铵放电管(9)和废气管线。 在反应器(1)内设置可旋转混合,捏合和粉碎元件。 此外,提供了可以通过进料管线(13)装入多磷酸的可加热搅拌罐(11),并且可用于通过管线(20)从从反应器(1)流出的废气中再次蒸发水蒸气和氨 ),并且可以通过出口管线(17)将部分氨化的多磷酸从其中引入反应器(1)。
    • 10. 发明授权
    • Process for the preparation of alkali metal phosphate solutions
    • 制备碱金属磷酸盐溶液的方法
    • US5124137A
    • 1992-06-23
    • US676862
    • 1991-03-28
    • Gunther SchimmelThomas StaffelReinhard Gradl
    • Gunther SchimmelThomas StaffelReinhard Gradl
    • C01B25/30
    • C01B25/308
    • Alkali metal phosphate solutions having a fluorine content of less than 20 ppm, based on P.sub.2 O.sub.5, are prepared by first digesting crude phosphate using sulfuric acid, and separating the calcium sulfate from the crude phosphoric acid. An alkali metal compound is then added to the crude phosphoric acid, and the precipitated solid is filtered off. The prepurified crude phosphoric acid is neutralized to a pH of at least 7, and the solid produced during this operation is separated off. The resultant alkali metal phosphate solutions having a P.sub.2 O.sub.5 content of from 10 to 30% by weight are adjusted to a pH of between 4.8 and 6.0 using phosphoric acid. The solutions are heated to from 60.degree. to 120.degree. C., and from 1 to 6% by weight, based on the weight of the solution, of an alkaline earth metal oxygen compound are added to the alkali metal phosphate solutions with stirring. Finally, the precipitated solid is filtered off from the alkali metal phosphate solutions after a residence time of from 0.5 to 4 hours.
    • 通过首先使用硫酸消化粗磷酸酯,并从粗磷酸中分离硫酸钙,制备基于P 2 O 5的氟含量小于20ppm的碱金属磷酸盐溶液。 然后向粗磷酸中加入碱金属化合物,滤出沉淀的固体。 将预纯化的粗磷酸中和至至少7的pH,并且在该操作期间产生的固体被分离出来。 使用磷酸将所得的具有10-30重量%的P2O5含量的碱金属磷酸盐溶液调节至4.8至6.0的pH。 在搅拌下将溶液加热至60〜120℃,以溶液重量为1〜6重量%的碱土金属氧化合物加入到碱金属磷酸盐溶液中。 最后,在0.5-4小时的停留时间后,将沉淀的固体从碱金属磷酸盐溶液中滤出。