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公开(公告)号：US5087373A
公开(公告)日：1992-02-11
申请号：US707122
申请日：1991-05-29
CPC分类号： C02F9/00 , B01J39/04 , C23C22/34 , C23C22/86 , C02F1/66 , C02F2001/427 , C02F2101/14 , C02F2101/20 , C02F2101/303 , C02F2103/16 , C02F2209/06
摘要： In a process of removing complexly bound titanium and/or zirconium from acid aqueous solutions the solution which contains the complexly bound titanium and/or zirconium is conditioned in that its pH value is raised to at least 8, any precipitate thus formed is removed and the solution thus treated is passed through an ion exchange plant comprising a cation exchange material and an anion exchange material. The solution is preferably passed through an ion exchange plant which contains the cation exchange material in the H.sup.+ form and the anion exchange material in the OH.sup.- form. The process is particularly intended for the treatment of solutions obtained by the chemical treatment of surfaces preferably of metals, which solutions contain titanium and/or zirconium in the form of fluoro complexes.
摘要翻译： 在从酸性水溶液中除去复合结合的钛和/或锆的方法中，将含有复合结合的钛和/或锆的溶液调节为其pH值升至至少8，除去任何形成的沉淀物， 如此处理的溶液通过包含阳离子交换材料和阴离子交换材料的离子交换设备。 该溶液优选通过含有H +形式的阳离子交换材料和OH-型阴离子交换材料的离子交换设备。 该方法特别用于处理通过化学处理优选金属的表面所获得的溶液，该溶液含有氟络合物形式的钛和/或锆。
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公开(公告)号：US4897128A
公开(公告)日：1990-01-30
申请号：US178183
申请日：1988-04-06
申请人： Heinz Dosch , Dieter Hauffe , Horst Gehmecker
发明人： Heinz Dosch , Dieter Hauffe , Horst Gehmecker
CPC分类号： C23C22/77 , G01N31/164
摘要： Described is a process for determining the zinc content of an acid aqueous phosphating bath. A bath sample is titrated at a pH value between 1.2 and 1.7 in the presence of ethylenediaminetetraacetic acid, hexamethylenetetramine and alkalihexacyanoferrate (III) with an alkalihexacyanoferrate(II) until the potential at an oxidation-reduction electrode immersed into the bath sample reaches an inflection point.Any content of nitrite and/or iron(II) ions must be removed by an addition of nitrite-destroying substances and by an oxidation to iron(III) ions at a pH value above 8.The process is particularly suitable for determining the zinc concentration of phosphating baths which contain 0.4 to 2.0 g/l Zn. The presence in phosphating baths of additional cations such as manganese and/or calcium and/or nickel and/or magnesium does not interfere with the process. The analysis can be automatic and may directly be used to control a metering device for supplying make-up concentrates to the phosphating bath.
摘要翻译： 描述了确定酸性磷酸氢盐浴的锌含量的方法。 在乙二胺四乙酸六亚甲基四胺和碱金属氰化铁酸盐（III）与碱金属氰化铁酸盐（II）的存在下，在1.2至1.7的pH值下滴定浴样品，直到浸入浴液样品中的氧化还原电极的电位达到拐点 。 亚硝酸根和/或铁（II）离子的任何含量必须通过加入亚硝酸盐破坏物质和通过氧化成铁（III）离子在pH值高于8处去除。该方法特别适用于测定锌浓度 的含有0.4〜2.0g / l Zn的磷化浴。 存在附加阳离子如锰和/或钙和/或镍和/或镁的磷化浴不会妨碍该方法。 分析可以是自动的，并且可以直接用于控制用于向磷化浴提供补充浓缩物的计量装置。
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公开(公告)号：US06168674A
公开(公告)日：2001-01-02
申请号：US09468282
申请日：1999-12-20
IPC分类号： C23C2207
CPC分类号： C23C22/17 , C23C22/182
摘要： In a process of phosphatizing metal surfaces, which at least partly consist of iron or steel, in accordance with the low-zinc technology, the metal surfaces are brought in contact with aqueous acid phosphatizing solutions at a temperature of 30 to 65° C. for a period of 1 to 8 min, which solutions contain 0.4 to 2.0 g/l Zn 7 to 25 g/l P2O5 0.005 to 0.5 g/l peroxide (calc. as H2O2) 0.01 to 10 g/l formate (calc. as formate ion), are free from chlorate and added nitrite, and in which the weight ratio of free P2O5 to total P2O5 has been adjusted to a value in the range from 0.03 to 0.20, and the content of free acid has been adjusted to a value in the range from 0.5 to 2.5. After contact with the phosphatizing solution, the workpiece is rerinsed with water, which has been adjusted with mineral acid to a pH of from 3.6 to 5.0. The phosphatizing solutions may contain in addition up to 30 g/l nitrate as well as manganese, magnesium, calcium, lithium, tungstate, vanadate, molybdate or combinations thereof, possibly also nickel and/or cobalt, each in an amount of up to 3 g/l, possibly also up to 0.030 g/l copper. The weight ratios Mn:Zn, Mg:Zn, Ca:Zn and possibly (Ni and/or Co):Zn should each be not more than 2:1.
摘要翻译： 在根据低锌技术将至少部分由铁或钢组成的金属表面磷化的过程中，在30至65℃的温度下使金属表面与酸性磷酸盐水溶液接触， 时间为1至8分钟，该溶液含有0.4至2.0g / l Zn7至25g / l P2O50.005至0.5g / l过氧化物（按H 2 O 2计算）0.01至10g / l甲酸盐（计算为 甲酸根离子）不含氯酸盐和加入的亚硝酸盐，其中游离P 2 O 5与总P 2 O 5的重量比已经调节到0.03至0.20的范围内，并且游离酸的含量已被调节到一个值 在0.5至2.5的范围内。 在与磷酸盐溶液接触后，将工件重新吸收水，该水已经用无机酸调节至3.6至5.0的pH。 磷酸盐溶液还可以含有高达30g / l的硝酸盐以及锰，镁，钙，锂，钨酸盐，钒酸盐，钼酸盐或其组合，可能还含有镍和/或钴，其量最多为3 g / l，也可能达到0.030g / l铜。 重量比Mn：Zn，Mg：Zn，Ca：Zn以及可能的（Ni和/或Co）：Zn应不大于2：1。
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公开(公告)号：US5203930A
公开(公告)日：1993-04-20
申请号：US570350
申请日：1990-08-21
申请人： Georg Blumlhuber , Horst Gehmecker , Dieter Hauffe , Lothar Kaul , Thomas Nitschke , Werner Rausch , Hardy Wietzoreck
发明人： Georg Blumlhuber , Horst Gehmecker , Dieter Hauffe , Lothar Kaul , Thomas Nitschke , Werner Rausch , Hardy Wietzoreck
CPC分类号： C23C22/184 , C23C22/13 , C23C22/22 , C23C22/362 , C23C22/73
摘要： A process for forming phosphate coatings on metal surfaces is provided which comprises the steps of contacting said metal surface with an Fe(II)-containing phosphating solution comprising0.4 to 30 g/l Zn4 to 30 g/l P.sub.2 O.sub.55 to 50 g/l NO.sub.3up to 10 g/l Fe(II) ; andup to 0.3 g/l (Fe(III)wherein the weight ratio of free P.sub.2 O.sub.5 to total P.sub.2 O.sub.5 is (0.04 to 0.50):1 and, replenishing said phosphating solution with Zn, NO.sub.3 and P.sub.2 O.sub.5 in a weight ratio ofZn:NO.sub. 3 P.sub.2 O.sub.5 =(0.60 to 0.30):(0.2 to 0.4):1.wherein the Fe(II) content is adjusted by oxidation with nitrate or nitrite derived from nitrate optionally employed with an oxygen-containing gas, H.sub.2 O.sub.2 and/or nitrous gases; and rinsing said metal surface with a cascade of at least two aqueous rinsing baths in the opposite direction of travel of said metal surface wherein water having a low salt content or no salt content derived from the phosphating bath is fed to the last rinsing bath and the overflowing water from said rinsing bath is fed to the next preceding rinsing bath and ultimately to the phosphating bath, and wherein the low salt content rinse water derived from the phosphating bath is withdrawn therefrom as a rate effective to permit the addition of phosphate-enriched rinsing water from the cascade of rinsing water to the phosphating bath while maintaining the desired species concentration in said phosphating bath.
摘要翻译： 提供一种在金属表面上形成磷酸盐涂层的方法，其包括以下步骤：使所述金属表面与含有0.4至30g / l Zn 4至30g / l P 2 O 5的含Fe（II）的磷酸盐溶液接触5至50g / l NO3高达10g / l Fe（II）; 和高达0.3g / l（Fe（III），其中游离P 2 O 5与总P 2 O 5的重量比为（0.04-0.50）：1，并用Zn，NO 3和P 2 O 5以Zn:Nn的重量比补充所述磷酸盐溶液 3 P 2 O 5 =（0.60〜0.30）：（0.2〜0.4）：1，其中Fe（II）含量通过硝酸盐或亚硝酸盐氧化而调节，硝酸盐或硝酸盐任选地与含氧气体，H 2 O 2和/或亚硝酸气体 并且在所述金属表面的相反行进方向上用级联的至少两个水性漂洗浴冲洗所述金属表面，其中具有低盐含量或不含有来自磷酸盐的盐含量的水被供给到最后的冲洗浴中， 将来自所述冲洗浴的溢出水进料到下一个先前的漂洗浴并最终送入磷化浴，并且其中从磷化浴中得到的低盐含量的漂洗水从其中提取出来，其速率可以有效地添加富含磷酸盐 从级联漂洗水 e向磷化浴中冲洗水，同时保持所述磷化浴中所需的物质浓度。
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公开(公告)号：US4950339A
公开(公告)日：1990-08-21
申请号：US305214
申请日：1989-02-01
申请人： Horst Gehmecker , Werner Rausch , Peter Jorns
发明人： Horst Gehmecker , Werner Rausch , Peter Jorns
CPC分类号： C23C22/362 , C23C22/78
摘要： A process to form phosphate coatings on individual parts of metal which at least on part of their surface consists of iron or steel. The individual parts are contacted at a temperature in the range of from 60 to 100 degrees centigrade for 3 to 30 seconds with an aqueous phosphating solution which contains 10 to 80 g/l zinc, 12 to 80 g/l phosphate (calculated as P.sub.2 O.sub.5), 40 to 150 g/l nitrate and, in addition 0.1 to 10 g/l fluoride, 0.01 to 10 g/l nickel, 0.0001 to 0.1 g/l copper, and may also contain tartaric acid, citric acid and/or manganese and in which the ratio of free acid to total acid has been adjusted to (0.1 to 0.3):1 and which contains at least 80 points of total acid and is virtually free of iron(II) ions. Prior to phosphating treatment, the individual parts may be cleaned and may optionally be treated to remove rust, scale and phosphate layers and/or be activated. After the phosphating treatment they may be passivated with an after-rinse solution. Each of said process steps is carried out for 3 to 30 seconds.
摘要翻译： 在金属的单个部分上形成磷酸盐涂层的方法，其至少部分表面由铁或钢组成。 使用含有10至80g / l锌，12至80g / l磷酸盐（以P2O5计算）的磷酸盐水溶液将各个部件在60至100摄氏度的温度范围内接触3至30秒， ，40〜150g / l的硝酸盐，以及0.1〜10g / l的氟化物，0.01〜10g / l的镍，0.0001〜0.1g / l的铜，也可以含有酒石酸，柠檬酸和/或锰， 其中游离酸与总酸的比例已经被调节到（0.1〜0.3）：1，并且其含有至少80个总酸，实际上没有铁（II）离子。 在磷化处理之前，可以清洁各个部件，并且可以任选地处理以除去锈，鳞屑和磷酸盐层和/或被活化。 在磷化处理后，可以用冲洗液进行钝化。 每个所述处理步骤进行3至30秒。
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公开(公告)号：US5294266A
公开(公告)日：1994-03-15
申请号：US978193
申请日：1992-11-18
申请人： Dieter Hauffe , Thomas Kolberg , Gerhard Muller , Horst Gehmecker , Werner Rausch , Peter Schubach , Thomas Wendel
发明人： Dieter Hauffe , Thomas Kolberg , Gerhard Muller , Horst Gehmecker , Werner Rausch , Peter Schubach , Thomas Wendel
CPC分类号： C23C22/73 , C23C22/34 , C23C22/361 , C23C22/60 , C23C22/83
摘要： The invention is in a composition and process for the chromium free passivating postrinsing of conversion layers on metals before the application of a paint or adhesive. The conversion layers can be on the bases of phosphate layers, at least two polyvalent metal ions with complex formers, titanium, zirconium and/or hafnium. The postrinsing agent is an aqueous solution which has been adjusted to a pH value of up to 5 and which contains an aluminum fluorozirconate having an Al:Zr:F mole ratio of (0.15 to 8.0):1:(5 to 52), and in which solutions the total concentration of Al+Zr+F is 0.1 to 8.0 g/l. The postrinsing solutions may additionally contain at least one of the anions benzoate, caprylate, ethyl hexoate, salicylate in a total concentration of 0.05 to 0.5 g/1 and may preferably be adjusted to the required pH value with cations of volatile bases, such as ammonium, ethanolammonium and di- and triethanolammonium. The paint is subsequently applied suitably by cathodic electrocoating or powder coating or from a low-solvent high-solids paint.The rinsing treatment is over a period of 1 to 120 seconds at temperatures of 20.degree. to 80.degree. C. The invention is used as a pretreatment to the application of a paint coating, film coating or adhesive coating.
摘要翻译： 本发明是用于在施加涂料或粘合剂之前的金属上的转化层的无铬钝化的组合物和方法。 转化层可以在磷酸盐层，至少两种具有复合成型剂的多价金属离子，钛，锆和/或铪的基础上。 postrinsing剂是一种水溶液，其pH值调至5以下，并含有Al：Zr：F摩尔比为（0.15〜8.0）：1：（5〜52）的氟锆酸铝， 其中Al + Zr + F的总浓度为0.1〜8.0g / l。 postrinsing溶液还可以含有至少一种阴离子苯甲酸酯，辛酸酯，己酸乙酯，水杨酸酯，总浓度为0.05至0.5g / l，并且可优选用挥发性碱如铵的阳离子调节至所需的pH值 ，乙醇铵和二乙醇胺和三乙醇铵。 随后通过阴极电涂或粉末涂料或低溶剂高固体涂料适当地施涂涂料。 在20〜80℃的温度下，漂洗处理时间为1〜120秒。本发明用作涂料涂料，薄膜包衣或粘合剂涂料的预处理。
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公开(公告)号：US5268041A
公开(公告)日：1993-12-07
申请号：US949349
申请日：1992-09-22
申请人： Horst Gehmecker , Werner Rausch , Peter Schubach
发明人： Horst Gehmecker , Werner Rausch , Peter Schubach
CPC分类号： C23C22/83 , C23C22/186 , C23C22/188 , C23C22/368
摘要： In a process of phosphating metal surfaces phosphating solutions are employed which are substantially free of nickel and contain______________________________________ 0.3 to 1.7 g/l Zn 0.2 to 4.0 g/l Mn 0.001 to 0.030 (preferably 0.003 to 0.020) g/l Cu 5 to 30 g/l phosphate (calculated as P.sub.2 O.sub.5) ______________________________________ in which by oxygen and/or other equivalent oxidizers the concentration of Fe(II) is kept below 0.1 g/1 and which are adjusted to a pH value from 3.0 to 3.8. The weight ratio of Cu to P.sub.2 O.sub.5 is preferably adjusted to I: (170 to 30,000) and Cu and P.sub.2 O.sub.5 are preferably replenished in a weight ratio of 1 : (5 to 2000). The phosphating solutions should contain 0.3 to 1.0 g/1 Zn if they are applied by spraying and should contain 0.9 to 1.7 g/1 Zn if they are applied by spraying/dipping operations or by a dipping operation. The process serves particularly for the pretreatment of metal surfaces for a succeeding painting, particularly by electro-dipcoating, and for the phosphating of steel, galvanized steel, zinc alloy-plated steel, aluminum and its alloys.
摘要翻译： 在磷化金属表面的过程中，使用基本上不含镍的磷酸盐溶液，并且含有-0.3至1.7g / l的Zn-0.2至4.0g / l的Mn-0.001至0.030（优选0.003至-0.20）g / l的Cu -5至30g / l磷酸盐（计算为P 2 O 5） - 其中通过氧气和/或其它等效氧化剂将Fe（II）的浓度保持在0.1g / l以下，并将其调节至pH值为3.0至 3.8。 优选将Cu与P 2 O 5的重量比调整为I：（170〜30,000），优选以1：（5〜2000）的重量比补充Cu和P2O5。 如果通过喷涂施用，磷酸盐溶液应含有0.3至1.0 g / l的Zn，如果通过喷涂/浸渍操作或浸渍操作施加，则应含有0.9至1.7 g / l的Zn。 该方法特别用于后续涂漆的金属表面的预处理，特别是通过电沉积，以及用于钢，镀锌钢，镀锌钢，铝及其合金的磷化。
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公开(公告)号：US5135583A
公开(公告)日：1992-08-04
申请号：US749191
申请日：1991-08-23
申请人： Horst Gehmecker , Thomas Kolberg , Dirk Meyer , Gerhard Muller
发明人： Horst Gehmecker , Thomas Kolberg , Dirk Meyer , Gerhard Muller
CPC分类号： C23C22/362 , C23C22/86
摘要： For phosphating metal surfaces which consist at least in part of aluminum, by means of phosphating solutions which contain zinc, phosphate and fluoride, any titanium which has entered the phosphating solution and would disturb the formation of the layer is precipitated by an addition of SiO-containing compounds and after the precipitate has been removed, the content of free fluoride is readjusted to the required concentration. Particularly suitable compounds which contain SiO, consist of alkali metasilicate, alkali orthosilicate and/or alkali disilicate, preferably used in an amount of 0.05 to 1 g/l of the phosphating solution, or of silica, which is preferably used in an amount of 0.5 to 10 g per liter of the phosphating solution (calc. as Si).
摘要翻译： 对于至少部分由铝组成的磷化金属表面，通过含有锌，磷酸盐和氟化物的磷化溶液，已经进入磷化溶液并且将扰乱层的形成的任何钛通过加入SiO- 在除去沉淀物之后，将游离氟化物的含量重新调节至所需浓度。 含有SiO的特别合适的化合物由偏硅酸碱，原硅酸碱和/或碱二硅酸盐组成，优选以0.05至1g / l的磷酸盐溶液或二氧化硅的量使用，其优选以0.5的量使用 至10g每升磷酸盐溶液（计算为Si）。
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