Process for the preparation of tetrabromobisphenol-A

    公开(公告)号:US06313355B1

    公开(公告)日:2001-11-06

    申请号:US09614819

    申请日:2000-07-12

    IPC分类号: C07C3916

    CPC分类号: C07C37/62 C07C39/367

    摘要: Tetrabromobisphenol-A is produced in a bromination process where no bromine or only a very small proportion of bromine is fed to the reactor. In the process aqueous hydrobromic acid, is the sole source or a major source of the bromine. In the process there are at least three concurrent continuous feeds to the reactor. One is composed of bisphenol-A and/or underbrominated bisphenol-A and a water-miscible organic solvent. The second is gaseous hydrogen bromide or preferably, aqueous hydrobromic acid, and the third is aqueous hydrogen peroxide. Optionally a small additional continuous feed of bromine can be employed. The feeds are proportioned to maintain a liquid phase containing (i) from above about 15 to about 85 wt % water, based upon the amount of water and water-miscible organic solvent in such liquid phase, and (ii) an amount of unreacted bromine that is in excess over the stoichiometric amount theoretically required to convert the bisphenol-A and/or underbrominated bisphenol-A to tetrabromobisphenol-A. The tetrabromobisphenol-A continuously forms as a solids phase in a yield of at least about 90% based on bisphenol-A and/or underbrominated bisphenol-A fed. The reaction mass is agitated and/or refluxed to maintain a substantially uniform slurry in the reactor. An amount of the slurry is continuously removed so that the volume of the contents of the reactor remains substantially constant.

    Process for producing tetrabromobisphenol-A
    2.
    发明授权
    Process for producing tetrabromobisphenol-A 有权
    生产四溴双酚A的方法

    公开(公告)号:US6147264A

    公开(公告)日:2000-11-14

    申请号:US288195

    申请日:1999-04-08

    IPC分类号: C07C37/62 C07C39/16

    CPC分类号: C07C37/62

    摘要: Bisphenol-A or preferably, a mixture of bisphenol-A and underbrominated bisphenol-A, is brominated in a liquid phase reaction medium in which tetrabromobisphenol-A is relatively insoluble, using a stoichiometric deficiency of bromine to thereby form in the reaction mass a precipitate (i.e., a solids phase) composed of 50-95 wt % of tetrabromobisphenol-A and 50-5 wt % of underbrominated bisphenol-A. The precipitate is separated from the reaction mass, preferably during the bromination, and tetrabromobisphenol-A is recovered from the precipitate. Preferably underbrominated bisphenol-A is recycled as feed to the bromination. The process technology of this invention has the capability of producing high quality tetrabromobisphenol-A (high purity, good color, low ionic halide content) with efficient raw material utilization, minimized waste product formation, and minimized waste disposal costs.

    摘要翻译: 双酚A或双酚A和未溴化双酚A的混合物在其中四溴双酚A相对不溶的液相反应介质中溴化,使用化学计量的溴缺乏,从而在反应物质中形成沉淀 (即,固体相),由50-95重量%的四溴双酚A和50-5重量%的未溴化双酚A组成。 将沉淀物与反应物质分离,优选在溴化期间,从沉淀物中回收四溴双酚-A。 优选将未溴化双酚-A作为进料进行溴化反应。 本发明的工艺技术具有生产高品质的四溴双酚A(高纯度,良好的颜色,低离子卤化物含量)的能力,具有高效的原料利用率,最大限度地减少废物产生形成和最小化废物处理成本。

    Process for the preparation of tetrabromobisphenol-A
    3.
    发明授权
    Process for the preparation of tetrabromobisphenol-A 有权
    制备四溴双酚A的方法

    公开(公告)号:US06235946B1

    公开(公告)日:2001-05-22

    申请号:US09416855

    申请日:1999-10-12

    IPC分类号: C07C3916

    CPC分类号: C07C37/62 C07C39/367

    摘要: Tetrabromobisphenol-A is produced in a bromination process where no bromine or only a very small proportion of bromine is fed to the reactor. In the process aqueous hydrobromic acid, is the sole source or a major source of the bromine. In the process there are at least three concurrent continuous feeds to the reactor. One is composed of bisphenol-A and/or underbrominated bisphenol-A and a water-miscible organic solvent. The second is gaseous hydrogen bromide or preferably, aqueous hydrobromic acid, and the third is aqueous hydrogen peroxide. Optionally a small additional continuous feed of bromine can be employed. The feeds are proportioned to maintain a liquid phase containing (i) from above about 15 to about 85 wt % water, based upon the amount of water and water-miscible organic solvent in such liquid phase, and (ii) an amount of unreacted bromine that is in excess over the stoichiometric amount theoretically required to convert the bisphenol-A and/or underbrominated bisphenol-A to tetrabromobisphenol-A. The tetrabromobisphenol-A continuously forms as a solids phase in a yield of at least about 90% based on bisphenol-A and/or underbrominated bisphenol-A fed. The reaction mass is agitated and/or refluxed to maintain a substantially uniform slurry in the reactor. An amount of the slurry is continuously removed so that the volume of the contents of the reactor remains substantially constant.

    摘要翻译: 在溴化过程中产生四溴双酚A,其中溴或仅很少比例的溴被加入到反应器中。 在该方法中,氢溴酸水溶液是溴的唯一来源或主要来源。 在该过程中,至少有三次同时连续进料到反应器中。 一种由双酚A和/或二溴双酚A和水混溶性有机溶剂组成。 第二种是气态溴化氢或优选氢溴酸水溶液,第三种是过氧化氢水溶液。 任选地,可以使用小的额外的连续进料的溴。 进料成比例以维持液相,其基于在这种液相中的水和水混溶性有机溶剂的量,含有(i)约15至约85重量%的水,和(ii)一定量的未反应的溴 这超过理论上将双酚A和/或未溴化双酚A转化为四溴双酚A所需的化学计量量。 基于双酚A和/或进料的未溴化双酚A,四溴双酚-A连续形成固体相,产率至少为约90%。 搅拌和/或回流反应物料以在反应器中保持基本均匀的浆料。 连续除去一定量的浆料,使得反应器内容物的体积保持基本恒定。

    Process for the preparation of tetrabromobisphenol-A
    4.
    发明授权
    Process for the preparation of tetrabromobisphenol-A 有权
    制备四溴双酚A的方法

    公开(公告)号:US06300527B1

    公开(公告)日:2001-10-09

    申请号:US09614818

    申请日:2000-07-12

    IPC分类号: C07C3916

    CPC分类号: C07C37/62 C07C39/367

    摘要: This invention relates, inter alia, to a process for the production of tetrabromobisphenol-A by the bromination of bisphenol-A and/or underbrominated bisphenol-A, which process features: a water and water-miscible organic solvent reaction medium; a relatively high reaction temperature; and the presence, in the reaction medium, of both (i) excess unreacted Br2 during the feed of bisphenol-A to the reactor, and (ii) sufficient HBr to protect the tetrabromobisphenol-A produced against undesirable color formation. Tetrabromobisphenol-A precipitates from the reaction mass and is easily recovered. Product of high purity (97% or more) and very low color (APHA of 50 or less) can be produced, even when using large excesses of bromine in the reaction.

    摘要翻译: 本发明尤其涉及通过双酚A和/或二溴双酚A的溴化生产四溴双酚A的方法,其特征在于:水和水可混溶的有机溶剂反应介质; 相对较高的反应温度; 以及在反应介质中存在(i)在将双酚-A进料到反应器中过量的未反应Br 2的存在,和(ii)足够的HBr以保护所产生的四溴双酚A而导致不希望的颜色形成。 四溴双酚A从反应物质中沉淀出来,容易回收。 即使在反应中使用大量过量的溴,也可以生产高纯度(97%以上)和非常低的颜色(APHA为50以下)的产品。

    Process for the preparation of tetrabromobisphenol-A
    5.
    发明授权
    Process for the preparation of tetrabromobisphenol-A 有权
    制备四溴双酚A的方法

    公开(公告)号:US06218584B1

    公开(公告)日:2001-04-17

    申请号:US09329374

    申请日:1999-06-10

    IPC分类号: C07C3916

    CPC分类号: C07C37/62 C07C39/367

    摘要: This invention relates, inter alia, to a process for the production of tetrabromobisphenol-A by the bromination of bisphenol-A and/or underbrominated bisphenol-A, which process features: a water and water-miscible organic solvent reaction medium; a relatively high reaction temperature; and the presence, in the reaction medium, of both (i) excess unreacted Br2 during the feed of bis-phenol-A to the reactor, and (ii) sufficient HBr to protect the tetrabromobisphenol-A produced against undesirable color formation. Tetrabromobisphenol-A precipitates from the reaction mass and is easily recovered. Product of high purity (97% or more) and very low color (APHA of 50 or less) can be produced, even when using large excesses of bromine in the reaction.

    摘要翻译: 本发明尤其涉及通过双酚A和/或二溴双酚A的溴化生产四溴双酚A的方法,其特征在于:水和水可混溶的有机溶剂反应介质; 相对较高的反应温度; 以及在反应介质中存在(i)在将双酚-A进料到反应器期间过量的未反应Br 2和(ii)足够的HBr以保护产生的四溴双酚A而导致不希望的颜色形成。 四溴双酚A从反应物质中沉淀出来,容易回收。 即使在反应中使用大量过量的溴,也可以生产高纯度(97%以上)和非常低的颜色(APHA为50以下)的产品。

    Methods and apparatus for calibrating a color display
    8.
    发明授权
    Methods and apparatus for calibrating a color display 有权
    用于校准彩色显示器的方法和装置

    公开(公告)号:US08009175B2

    公开(公告)日:2011-08-30

    申请号:US12661663

    申请日:2010-03-22

    申请人: Richard A. Holub

    发明人: Richard A. Holub

    IPC分类号: G09G5/02

    摘要: Improved methods are provided for calibrating color on a color display coupled to a computer, which are useful for obtaining calibrated data in a virtual proof network for enabling different color devices to render consistent color. Methods involve user interactions with screens on the display to set color display parameters. An apparatus is also provided for calibrating a sensor which may be used for measuring color of a display in one or more of these methods.

    摘要翻译: 提供了改进的方法来校准耦合到计算机的彩色显示器上的颜色,这对于在虚拟证明网络中获得校准数据是有用的,以使不同的颜色设备能够呈现一致的颜色。 方法涉及用户与显示器上的屏幕交互以设置彩色显示参数。 还提供了用于校准可以用于以这些方法中的一种或多种测量显示器的颜色的传感器的装置。

    Methods and apparatus for calibrating a color display
    10.
    发明授权
    Methods and apparatus for calibrating a color display 有权
    用于校准彩色显示器的方法和装置

    公开(公告)号:US07102648B1

    公开(公告)日:2006-09-05

    申请号:US09832553

    申请日:2001-04-11

    申请人: Richard A. Holub

    发明人: Richard A. Holub

    IPC分类号: G09G5/02

    摘要: Improved methods are provided for calibrating color on a color display coupled to a computer, which are useful for obtaining calibrated data in a virtual proof network for enabling different color devices to render consistent color. Methods involve user interactions with screens on the display to set color display parameters. An apparatus is also provided for calibrating a sensor which may be used for measuring color of a display in one or more of these methods.

    摘要翻译: 提供了改进的方法来校准耦合到计算机的彩色显示器上的颜色,这对于在虚拟证明网络中获得校准数据是有用的,以使不同的颜色设备能够呈现一致的颜色。 方法涉及用户与显示器上的屏幕交互以设置彩色显示参数。 还提供了用于校准可以用于以这些方法中的一种或多种测量显示器的颜色的传感器的装置。