公开(公告)号：US4454067A

公开(公告)日：1984-06-12

申请号：US82977

申请日：1979-10-09

申请人： Hartmut Behringer ,  Kurt Karrenbauer ,  Heinrich Rehberg

发明人： Hartmut Behringer ,  Kurt Karrenbauer ,  Heinrich Rehberg

IPC分类号： C09B41/00

CPC分类号： C09B41/007 ,  Y10S534/07

摘要： The invention relates to a process for the continuous manufacture of azo pigments, wherein a coupling component is reacted, inside a reaction zone filled with a previously produced suspension of the azo pigment to be made, with an aqueous solution of a diazo component at 10.degree. to 60.degree. C. and over periods of 0.2 to 4 hours. To this end, an aqueous suspension or solution of the coupling component is passed in substantially laminar flow upwardly through a cylindrical reaction zone arranged in upright position; the aqueous solution of the diazo component is introduced through 2 to 50 serially arranged inlets opening laterally into the reaction zone, the diazo component being admitted in quantities decreasing from below to above and the stoichiometric end point of the coupling reaction being established at the upper most inlet opening into the reaction zone; the pH-value typical of each reaction is established by introducing dilute alkali liquor through 2 to 50 serially arranged inlets opening laterally into the reaction zone, the respective diazo component and alkali liquor inlets being arranged at different levels with respect to each other.

摘要翻译： 本发明涉及连续制造偶氮颜料的方法，其中偶联组分在填充有预先制备的待制备的偶氮颜料的悬浮液的反应区内与10℃的重氮组分的水溶液反应 至60℃，超过0.2-4小时。 为此，耦合组分的水性悬浮液或溶液基本上层流通过布置在直立位置的圆柱形反应区域; 重氮组分的水溶液通过横向开放到反应区中的2至50个连续排列的入口引入，重氮组分以从下至上的量减少，并且偶联反应的化学计量的终点建立在最高 入口进入反应区; 每个反应的典型pH值是通过将稀碱液通过2至50个连续排列的入口侧向进入反应区而形成的，相应的重氮组分和碱液入口被设置在彼此不同的水平。

公开(公告)号：US4920205A

公开(公告)日：1990-04-24

申请号：US329647

申请日：1989-03-28

申请人： Heinrich Rehberg ,  Hartmut Behringer

发明人： Heinrich Rehberg ,  Hartmut Behringer

IPC分类号： C09B41/00

CPC分类号： C09B41/006

摘要： Azo pigments are made by subjecting a diazo component to an azo coupling reaction with the equivalent quantity of a coupling component difficultly soluble at less than 65.degree. C. in the aqueous/acid and aqueous/netural pH-ranges. More specifically, an aqueous/alkaline solution of the coupling component is continuously mixed in a first reaction step with an aqueous solution of acetic acid, boric acid, phosphoric acid, hydrochloric acid or sulfuric acid at a temperature lower than 65.degree. C. within a period of less than 1 minute, during which the coupling component commenences precipitating at least partially as reactive matter; next, the suspension obtained is continuously mixed, in a second reaction step immediately following the first reaction step, with an aqueous/acid solution of the diazo component at a temperature of less than 65.degree. C. within a period of less than 1 minute, and a predetermined pH between 2 and 9 is established by controlling the flow of the mass streams of diazo component and coupling component whereby a portion of the coupling component is caused to undergo immediate reaction to the azo pigment to be made; the balance portion of the coupling component is ultimately reacted in a postreaction phase with unreacted diazo component to the azo pigment to be made.

摘要翻译： 偶氮颜料是通过使重氮组分与等量的偶联组分在低于65℃在水/酸和水/ pH值范围内难溶的偶氮偶联反应来制备的。 更具体地说，将偶联成分的水溶液/碱性溶液在第一反应步骤中与乙酸，硼酸，磷酸，盐酸或硫酸的水溶液在低于65℃的温度下在 时间小于1分钟，在此期间耦合组分至少部分地作为反应性物质沉淀; 接下来，在第一反应步骤之后的第二反应步骤中，将所得悬浮液与小于65℃的重氮组分的水溶液/酸溶液在小于1分钟的时间内连续混合， 并且通过控制重氮组分和偶联组分的质量流的流动来建立在2和9之间的预定pH，由此使得一部分偶合组分与待制备的偶氮颜料立即反应; 偶联组分的平衡部分最终在后反应阶段与未反应的重氮组分反应至待制备的偶氮颜料。

公开(公告)号：US4439361A

公开(公告)日：1984-03-27

申请号：US344487

申请日：1982-02-01

申请人： Kurt Karrenbauer ,  Hartmut Behringer ,  Heinrich Rehberg

发明人： Kurt Karrenbauer ,  Hartmut Behringer ,  Heinrich Rehberg

IPC分类号： C07C245/20 ,  C07C67/00 ,  C07C241/00 ,  C09B41/00 ,  C07C113/04

CPC分类号： C09B41/007

摘要： The disclosure relates to a process for controlling diazotization reactions. To this end, a reaction batch containing an aromatic amine and nitrous acid is vigorously agitated so as to continuously renew the surface area of the batch. The air above said surface area is exhausted at a constant rate and tested for its content of nitrous gases originating from partially decomposed nitrous acid. Nitrous acid or dissolved matter forming it under the reaction conditions is supplied to the feed amine in the proportions necessary to provide for a content between 5 and 300 ppm nitrous gases in the exhausted air.

摘要翻译： 本公开涉及控制重氮化反应的方法。 为此，剧烈搅拌含有芳族胺和亚硝酸的反应批料，以连续更新批料的表面积。 所述表面积之上的空气以恒定速率排出，并测试其源自部分分解的亚硝酸的亚硝气的含量。 将在反应条件下形成的亚硝酸或其溶解物质以必需的比例供给至进料胺，以提供在排出空气中的5至300ppm的亚硝酸气体的含量。

公开(公告)号：US4268437A

公开(公告)日：1981-05-19

申请号：US47698

申请日：1979-06-12

申请人： Hartmut Behringer ,  Kurt Karrenbauer

发明人： Hartmut Behringer ,  Kurt Karrenbauer

IPC分类号： C07C245/20 ,  C07C20060101 ,  C07C67/00 ,  C07C241/00 ,  C07C113/04

CPC分类号： C07C245/20

摘要： The invention provides a process for the continuous diazotization of primary aromatic amines by reacting an aqueous solution or suspension of the amine in a mineral acid with an aqueous sodium nitrite solution. To this end, the lower portion of a cylindrical diazotization vessel placed in upright position is fed continuously with an aqueous mineral acid solution or suspension of a diazotizable primary aromatic amine. At the same time, the vessel is fed, via one or more inlets arranged one above the other so as to open laterally thereinto, with an aqueous sodium nitrite solution, the amine and nitrite being used in stoichiometric proportions, or the nitrite being used in a stoichiometric deficiency and the acid being used in an excess of about 1 to 3 equivalents per amine equivalent in the mineral acid solution. The resulting mixture is reacted while producing a laminar flow of liquid matter at temperatures of about 5.degree. to 30.degree. C. Next, reaction mixture is removed, in accordance with the diazotization velocity of the particular amine used, from the upper portion of the diazotization vessel at a place where the reaction mixture is substantially free from nitrous acid, said place being situated in the vessel at a level which is the higher the lower the diazotization velocity of the amine used. The reaction mixture removed is finally filtered and diazonium salt-containing solution is delivered to a sojourn zone.

摘要翻译： 本发明提供了通过使无机酸中的胺的水溶液或悬浮液与亚硝酸钠水溶液反应来连续重氮化伯芳香胺的方法。 为此，放置在直立位置的圆柱形重氮化容器的下部连续地与无机酸水溶液或可重氮化的伯芳族胺的悬浮液一起进料。 同时，通过一个或多个一个在另一个上方排列的入口将容器进料，以横向打开，用亚硝酸钠水溶液，胺和亚硝酸盐以化学计量比使用，或亚硝酸盐用于 化学计量不足，酸在无机酸溶液中的胺当量超过约1〜3当量。 使所得混合物反应，同时在约5℃至30℃的温度下产生液体物质的层流。接下来，根据所用特定胺的重氮化速度，从重氮化的上部除去反应混合物 容器在反应混合物基本上不含有亚硝酸的地方，所述位置位于所用容器中所用胺的重氮化速度越低的水平。 将除去的反应混合物最后过滤，并将含重氮盐的溶液输送至住宅区。

公开(公告)号：US5531075A

公开(公告)日：1996-07-02

申请号：US358247

申请日：1994-12-19

申请人： Hartmut Behringer ,  Siegfried Pottkamper ,  Hans-Werner Stephan ,  Gerrit Marcks

发明人： Hartmut Behringer ,  Siegfried Pottkamper ,  Hans-Werner Stephan ,  Gerrit Marcks

IPC分类号： B01J19/16 ,  C10L3/02 ,  C10L3/04 ,  F17C11/00 ,  F17C13/12

CPC分类号： B01J19/16 ,  C10L3/02 ,  C10L3/04 ,  F17C11/002 ,  F17C13/123 ,  Y10S220/901

摘要： In a process to transport acetylene which is dissolved in a solvent in a pressurized, insulated tank, the acetylene-to-solvent mass ratio of the solution is 0.30 at the maximum, whereby the solution has a temperature of up to -55.degree. C. [-67.degree. F.]. The surface of the solution in the tank is covered by a multilayer configuration consisting of pieces of floating material.

摘要翻译： 在加压绝缘槽中溶解在溶剂中的乙炔的方法中，溶液的乙炔与溶剂的质量比最大为0.30，由此溶液的温度高达-55℃。 [-67°F]。 罐中的溶液的表面被由浮动材料片组成的多层结构覆盖。

公开(公告)号：US4920206A

公开(公告)日：1990-04-24

申请号：US329953

申请日：1989-03-29

申请人： Hartmut Behringer ,  Heinrich Rehberg

发明人： Hartmut Behringer ,  Heinrich Rehberg

IPC分类号： C09B41/00

CPC分类号： C09B41/006

摘要： Azo Pigments are made by subjecting a diazo component to an azo coupling reaction with the equivalent quantity of a coupling component difficultly soluble at less than 65.degree. C. in the aqueous/acid and aqueous/neutral pH-ranges. More specifically, an aqueous/acid-solution of the diazo component is continuously mixed at a temperature of less than 65.degree. C. within a period of less than 1 minute with the aqueous/alkaline solution of the coupling component and a predetermined pH between 2 and 9 is established by controlling the flow of the mass streams of diazo component and coupling component; in this way a portion of the coupling component is caused to undergo immediate reaction to the azo pigment to be made whereas the balance portion of the coupling component simultaneously commences precipitating as finely crystalline reactive matter, which is reacted in a post-reaction phase with unreacted diazo component to give the azo pigment to be made.

摘要翻译： 偶氮颜料是通过在水/酸和水/中性pH范围内将重氮组分与等当量的难溶于低于65℃的偶联组分偶氮偶联反应制得的。 更具体地说，重氮组分的水溶液/酸溶液在小于65℃的温度下，在偶联组分的水/碱溶液和2分钟内的预定pH下在小于1分钟的时间内连续混合 并通过控制重氮组分和耦合组分的质量流的流动来建立9; 以这种方式使偶联组分的一部分立即反应到待制备的偶氮颜料，而偶联组分的平衡部分同时开始沉淀，作为精细结晶的反应性物质，其在反应后阶段与未反应的 重氮组分，得到偶氮颜料。