公开(公告)号：US20080114195A1

公开(公告)日：2008-05-15

申请号：US11840302

申请日：2007-08-17

申请人： Saadat Hussain ,  Arthur G. Mack

发明人： Saadat Hussain ,  Arthur G. Mack

IPC分类号： C07C25/18 ,  C07C17/23

CPC分类号： C07C17/38 ,  C07C25/18 ,  C07C41/34 ,  C07C43/29 ,  C09K21/08

摘要： Solid-state highly brominated compounds such as solid brominated flame retardants with bromine contents of at least about 60 wt % often contain occluded bromine. Because of their high bromine contents, such compounds have relatively low solubility in common organic solvents. Despite this low solubility, the content of occluded bromine in such solid brominated compounds is effectively reduced by agitating a concentrated agitated slurry of the compound in an inert solvent at a suitable temperature for at least about 1 hour. Thereafter, solids with reduced content of occluded bromine are isolated or recovered from the slurry. Novel products having substantially reduced or eliminated occluded bromine contents and other very desirable characteristics are also provided.

摘要翻译： 固态高度溴化的化合物，例如溴含量至少约60wt％的固体溴化阻燃剂通常含有阻塞的溴。 由于溴含量高，所以这些化合物在常见的有机溶剂中的溶解度相对较低。 尽管这种低溶解度，但是通过在惰性溶剂中在合适的温度下搅拌化合物的浓缩的搅拌浆料至少约1小时，可以有效地降低这些固体溴化化合物中封闭的溴的含量。 此后，从浆液中分离或回收含有减少的阻塞溴含量的固体。 还提供了具有显着降低或消除了阻塞的溴含量和其它非常理想特性的新产品。

公开(公告)号：US20080227903A1

公开(公告)日：2008-09-18

申请号：US11840329

申请日：2007-08-17

申请人： Saadat Hussain ,  Arthur G. Mack

发明人： Saadat Hussain ,  Arthur G. Mack

IPC分类号： C07C25/02 ,  C08K5/03

CPC分类号： C07C1/26 ,  C07C17/10 ,  C07C2529/40 ,  C08K5/03 ,  C07C9/00 ,  C07C19/075

摘要： High assay, reaction-derived decabromodiphenylethane product is prepared by feeding (i) diphenylethane or (ii) partially brominated diphenylethane having an average bromine number less than about two, or (iii) both of (i) and (ii), into the liquid confines of a reaction mixture. Such reaction mixture is (a) formed from components comprised of excess liquid bromine and aluminum-based Lewis acid bromination catalyst, and (b) maintained at one or more elevated reaction temperatures of from about 45°-90° C., and at least when elevated pressure is needed to keep a liquid state in the reaction mixture at the temperature(s) used, the reaction mixture is at such an elevated pressure, whereby ar-bromination occurs. The feeding is conducted at a rate slow enough to form high assay reaction-derived decabromodiphenylethane product, which is an effective flame retardant.

摘要翻译： 通过将（i）平均溴数小于约2的（ii）二苯基乙烷或（ii）部分溴化的二苯基乙烷，或（iii）（i）和（ii）两者加入到液体中来制备高分离反应衍生的十溴二苯乙烷产物 反应混合物的限制。 这种反应混合物是（a）由过量的液态溴和铝基路易斯酸溴化催化剂组成的组分形成的，和（b）保持在一个或多个升高的​​反应温度为约45-90℃，至少 当需要提高压力以在反应混合物中使用的温度保持液体状态时，反应混合物处于这样一个升高的压力下，从而发生溴化。 饲料以足够慢的速度进行，以形成高分析反应衍生的十溴二苯乙烷产物，其是有效的阻燃剂。

公开(公告)号：US20080108855A1

公开(公告)日：2008-05-08

申请号：US11840307

申请日：2007-08-17

申请人： Arthur G. Mack ,  Saadat Hussain

发明人： Arthur G. Mack ,  Saadat Hussain

IPC分类号： C07C17/093

CPC分类号： C07C17/12 ,  C07C25/18

摘要： A process for producing reaction-derived decabromodiphenylalkane product, especially decabromodiphenylethane product, of high assay is described. Diphenylalkane, preferably diphenylethane, is brominated by introducing the selected diphenylalkane in the form of a mist or spray into a reaction zone containing a reaction mixture having a liquid phase comprised of excess bromine and Lewis acid bromination catalyst, so that mist or spray of diphenylalkane descends onto and contacts the liquid phase of the reaction mixture and bromination of the diphenylalkane occurs to produce reaction-derived decabromodiphenylalkane product of high assay. Preferably, the reaction mixture is maintained under reflux and optionally is also stirred.

摘要翻译： 描述了高分离反应衍生的十溴二苯基烷烃产物，特别是十溴二苯乙烷产物的方法。 将二苯基烷烃，优选二苯基乙烷通过将选择的以雾或喷雾形式的二苯基烷烃引入含有由过量的溴和路易斯酸溴化催化剂组成的液相的反应混合物的反应区中进行溴化，使得二苯基烷烃的雾或喷雾下降 发生和接触反应混合物的液相并发生二苯基链烷烃的溴化，以产生高分离反应的十溴二苯基烷烃产物。 优选地，将反应混合物保持回流并任选地还搅拌。

公开(公告)号：US20080058559A1

公开(公告)日：2008-03-06

申请号：US11843759

申请日：2007-08-23

申请人： Saadat Hussain ,  Arthur G. Mack

发明人： Saadat Hussain ,  Arthur G. Mack

IPC分类号： C07C41/22

CPC分类号： C07C41/22 ,  C07C43/29

摘要： Improvements are described in process technology for producing reaction-derived decabromodiphenyl oxide of high purity from (i) diphenyl oxide and/or partially brominated diphenyl oxide and (ii) bromine under specified conditions including substantially concurrently reducing the content of hydrogen bromide present in the reactor sufficiently so that reaction-derived decabromodiphenyl oxide of high purity is formed without requiring procedures such as recrystallization or chromatography to remove lower brominated species, especially nonabromodiphenyl oxide.

摘要翻译： 在（i）二苯基氧化物和/或部分溴化二苯基氧化物中制备高纯度的反应衍生的十溴二苯醚的方法技术中描述了改进，和（ii）溴在特定条件下包括基本上同时降低反应器中存在的溴化氢含量 足以使得形成高纯度的反应衍生的十溴二苯醚，而不需要诸如重结晶或色谱法的步骤以除去较低溴化物质，特别是非溴二苯基氧化物。

公开(公告)号：US08217207B2

公开(公告)日：2012-07-10

申请号：US13204146

申请日：2011-08-05

申请人： Saadat Hussain ,  Arthur G. Mack

发明人： Saadat Hussain ,  Arthur G. Mack

IPC分类号： C07C25/00

CPC分类号： C07C1/26 ,  C07C17/10 ,  C07C2529/40 ,  C08K5/03 ,  C07C9/00 ,  C07C19/075

摘要： High assay, reaction-derived decabromodiphenylethane product is prepared by feeding (i) diphenylethane or (ii) partially brominated diphenylethane having an average bromine number less than about two, or (iii) both of (i) and (ii), into the liquid confines of a reaction mixture. Such reaction mixture is (a) formed from components comprised of excess liquid bromine and aluminum-based Lewis acid bromination catalyst, and (b) maintained at one or more elevated reaction temperatures of from about 45°-90° C., and at least when elevated pressure is needed to keep a liquid state in the reaction mixture at the temperature(s) used, the reaction mixture is at such an elevated pressure, whereby ar-bromination occurs. The feeding is conducted at a rate slow enough to form high assay reaction-derived decabromodiphenylethane product, which is an effective flame retardant.

摘要翻译： 通过将（i）平均溴数小于约2的（ii）二苯基乙烷或（ii）部分溴化的二苯基乙烷，或（iii）（i）和（ii）两者加入到液体中来制备高分离反应衍生的十溴二苯乙烷产物 反应混合物的限制。 这种反应混合物是（a）由过量的液态溴和铝基路易斯酸溴化催化剂组成的组分形成的，和（b）保持在一个或多个升高的​​反应温度为约45-90℃，至少 当需要提高压力以在反应混合物中使用的温度保持液体状态时，反应混合物处于这样一个升高的压力下，从而发生溴化。 饲料以足够慢的速度进行，以形成高分析反应衍生的十溴二苯乙烷产物，其是有效的阻燃剂。

公开(公告)号：US08034986B2

公开(公告)日：2011-10-11

申请号：US11840302

申请日：2007-08-17

申请人： Saadat Hussain ,  Arthur G. Mack

发明人： Saadat Hussain ,  Arthur G. Mack

IPC分类号： C07C17/38 ,  C07C25/00 ,  C07C17/00

CPC分类号： C07C17/38 ,  C07C25/18 ,  C07C41/34 ,  C07C43/29 ,  C09K21/08

摘要： Solid-state highly brominated compounds such as solid brominated flame retardants with bromine contents of at least about 60 wt % often contain occluded bromine. Because of their high bromine contents, such compounds have relatively low solubility in common organic solvents. Despite this low solubility, the content of occluded bromine in such solid brominated compounds is effectively reduced by agitating a concentrated agitated slurry of the compound in an inert solvent at a suitable temperature for at least about 1 hour. Thereafter, solids with reduced content of occluded bromine are isolated or recovered from the slurry. Novel products having substantially reduced or eliminated occluded bromine contents and other very desirable characteristics are also provided.

摘要翻译： 固态高度溴化的化合物，例如溴含量至少约60wt％的固体溴化阻燃剂通常含有阻塞的溴。 由于溴含量高，所以这些化合物在常见的有机溶剂中的溶解度相对较低。 尽管这种低溶解度，但是通过在惰性溶剂中在合适的温度下搅拌化合物的浓缩的搅拌浆料至少约1小时，可以有效地降低这些固体溴化化合物中封闭的溴的含量。 此后，从浆液中分离或回收含有减少的阻塞溴含量的固体。 还提供了具有显着降低或消除了阻塞的溴含量和其它非常理想特性的新产品。

公开(公告)号：US20100268003A1

公开(公告)日：2010-10-21

申请号：US12745951

申请日：2008-11-24

申请人： Saadat Hussain ,  Arthur G. Mack

发明人： Saadat Hussain ,  Arthur G. Mack

IPC分类号： C07C17/00

CPC分类号： C07C41/22 ,  C07C17/12 ,  C09K21/08 ,  C07C25/18 ,  C07C43/29

摘要： Processes for preparing brominated aromatic flame retardant having a reduced content of occluded free bromine are described. The processes comprise subdividing, during bromination of an aromatic compound, solid particles that form in a bromination reaction mixture in which an excess of liquid bromine and a Lewis acid bromination catalyst are present, said subdividing taking place within the confines of said reaction mixture. Subdivision is effected by grinding, milling, or sonication.

摘要翻译： 描述了制备具有降低的阻塞游离溴含量的溴化芳族阻燃剂的方法。 这些方法包括在溴化芳族化合物的过程中，在存在过量的液态溴和路易斯酸溴化催化剂的溴化反应混合物中形成固体颗粒，所述细分发生在所述反应混合物的范围内。 通过研磨，研磨或超声处理实现细分。

公开(公告)号：US20080132743A1

公开(公告)日：2008-06-05

申请号：US11840318

申请日：2007-08-17

申请人： Arthur G. Mack ,  Saadat Hussain

发明人： Arthur G. Mack ,  Saadat Hussain

IPC分类号： C07C17/10

CPC分类号： C07C17/12 ,  C07C25/18

摘要： Reaction-derived decabromodiphenylalkane product, especially decabromodiphenylethane product, of high purity is formed by (A) maintaining in a loop reactor a circulating inventory comprising at least Lewis acid bromination catalyst and excess liquid bromine; (B) introducing diphenylalkane and/or partially brominated diphenylalkane into the reactor so that bromination can occur; and (C) after a period of travel in the reactor during which solids of reaction-derived decabromodiphenylalkane product of high purity is formed, removing such solids from the reactor.

摘要翻译： 通过（A）在环管反应器中保持包含至少路易斯酸溴化催化剂和过量液体溴的循环库存，形成高纯度的反应衍生的十溴二苯基烷烃产物，特别是十溴二苯基乙烷产物。 （B）将二苯基链烷烃和/或部分溴化二苯基烷烃引入反应器中以便发生溴化; 和（C）在反应器中经过一段时间后，形成高纯度的反应衍生的十溴二苯基烷烃产物的固体，从反应器中除去这些固体。

公开(公告)号：US20110288225A1

公开(公告)日：2011-11-24

申请号：US13204146

申请日：2011-08-05

申请人： Saadat Hussain ,  Arthur G. Mack

发明人： Saadat Hussain ,  Arthur G. Mack

IPC分类号： C08K5/03 ,  C07C25/02

CPC分类号： C07C1/26 ,  C07C17/10 ,  C07C2529/40 ,  C08K5/03 ,  C07C9/00 ,  C07C19/075

摘要： High assay, reaction-derived decabromodiphenylethane product is prepared by feeding (i) diphenylethane or (ii) partially brominated diphenylethane having an average bromine number less than about two, or (iii) both of (i) and (ii), into the liquid confines of a reaction mixture. Such reaction mixture is (a) formed from components comprised of excess liquid bromine and aluminum-based Lewis acid bromination catalyst, and (b) maintained at one or more elevated reaction temperatures of from about 45°-90° C., and at least when elevated pressure is needed to keep a liquid state in the reaction mixture at the temperature(s) used, the reaction mixture is at such an elevated pressure, whereby ar-bromination occurs. The feeding is conducted at a rate slow enough to form high assay reaction-derived decabromodiphenylethane product, which is an effective flame retardant.

摘要翻译： 通过将（i）平均溴数小于约2的（ii）二苯基乙烷或（ii）部分溴化的二苯基乙烷，或（iii）（i）和（ii）两者加入到液体中来制备高分离反应衍生的十溴二苯乙烷产物 反应混合物的限制。 这种反应混合物是（a）由过量的液态溴和铝基路易斯酸溴化催化剂组成的组分形成的，和（b）保持在一个或多个升高的​​反应温度为约45-90℃，至少 当需要提高压力以在反应混合物中使用的温度保持液体状态时，反应混合物处于这样一个升高的压力下，从而发生溴化。 饲料以足够慢的速度进行，以形成高分析反应衍生的十溴二苯乙烷产物，其是有效的阻燃剂。

公开(公告)号：US20080200573A1

公开(公告)日：2008-08-21

申请号：US11996852

申请日：2006-08-01

申请人： Kimberly A. Maxwell ,  Saadat Hussain ,  Dominique Fasbinder ,  Danielle F. Goossens ,  Govindarajulu Kumar ,  Arthur G. Mack ,  Paul F. Ranken

发明人： Kimberly A. Maxwell ,  Saadat Hussain ,  Dominique Fasbinder ,  Danielle F. Goossens ,  Govindarajulu Kumar ,  Arthur G. Mack ,  Paul F. Ranken

IPC分类号： C08J9/00

CPC分类号： C08J9/0019 ,  C08J9/16 ,  C08J2201/03 ,  C08J2201/034 ,  C08J2325/04 ,  C08K5/0066 ,  C08L9/00 ,  C08L19/006 ,  C08L25/04

摘要： Styrenic polymer foams, especially expanded and/or extruded styrenic polymer foams, are flame retarded by use of one or more flame retardant additives. These additives are i) a diether of tetrabromobisphenol-S, which ether groups do not contain bromine and wherein at least one of the ether groups is an allyl group; ii) a diether of tetrabromobisphenol-S, wherein at least one of the ether groups contains bromine; iii) a substituted benzene having a total of 6 substituents on the ring and wherein at least 3 of the substituents are bromine atoms and at least two of the substituents are C1-4 alkyl groups; iv) tribromoneopentyl alcohol; v) a tris(dibromoalkyl) benzenetricarboxylate in which each dibromoalkyl group contains, independently, 3 to 8 carbon atoms; vi) a brominated polybutadiene which is partially hydrogenated and/or aryl-terminated; vii) at least one brominated allyl ether of a novolac; viii) a brominated poly(1,3-cycloalkadiene); ix) a brominated poly(4-vinylphenol allyl ether); x) a brominated N,TSP-phenylenebismaleimide; xi) a brominated N,N′-(4,4′-methylenediphenyl)bismaleimide; xii) a brominated N,N′-ethylenebis-maleimide; xiii) ethylenebis(dibromonorbornane-dicarboxrmide); xiv) tetrabromobisphenol-A; or xv) a combination of any two or more of i) through xiv).

摘要翻译： 苯乙烯类聚合物泡沫，特别是膨胀和/或挤出的苯乙烯类聚合物泡沫，通过使用一种或多种阻燃添加剂来阻燃。 这些添加剂是i）四溴双酚-S的二醚，其醚基不含溴，其中至少一个醚基是烯丙基; ii）四溴双酚-S的二醚，其中至少一个醚基含有溴; iii）在环上总共具有6个取代基的取代的苯，其中至少3个取代基是溴原子，并且至少两个取代基是C 1-4烷基; iv）三溴新戊醇; v）三（二溴烷基）苯甲酸三甲酯，其中每个二溴烷基独立地含有3至8个碳原子; vi）被部分氢化和/或芳基终止的溴化聚丁二烯; vii）至少一种酚醛清漆的溴化烯丙基醚; viii）溴化聚（1,3-环烷二烯）; ix）溴化聚（4-乙烯基苯酚烯丙基醚）; x）溴化N，TSP-亚苯基双马来酰亚胺; xi）溴化N，N' - （4,4'-亚甲基二苯基）双马来酰亚胺; xii）溴化N，N'-亚乙基双马来酰亚胺; xiii）亚乙基双（二溴降冰片 - 二甲苯咪唑）; xiv）四溴双酚A; 或xv）i）至xiv中的任何两个或更多个的组合）。