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1. 发明授权

US4654418A Continuous removal of the catalyst from polyphenylene ethers 失效
标题翻译：从聚苯醚连续除去催化剂
公开(公告)号：US4654418A
公开(公告)日：1987-03-31
申请号：US627984
申请日：1984-07-05
申请人： Rosemarie Berger , Hermann Dreher , Juergen Hambrecht , Eduard Heil , Rudi W. Reffert , Johann Swoboda , Adolf Echte , Peter Siebel
发明人： Rosemarie Berger , Hermann Dreher , Juergen Hambrecht , Eduard Heil , Rudi W. Reffert , Johann Swoboda , Adolf Echte , Peter Siebel
IPC分类号： C08G65/46 , C08G65/42
CPC分类号： C08G65/46
摘要： The catalyst is removed in the preparation of high molecular weight polyphenylene ethers from monohydric phenols, which are alkyl-substituted at the two ortho-positions but not at the para-position and may or may not be alkyl-substituted at the meta-position, by an oxidative coupling reaction with oxygen at from 15.degree. to 50.degree. C. in the presence of a catalyst complex obtained from a copper salt and an organic amine, in the presence of from 1 to 20 parts by weight of a solvent per part by weight of the monomeric phenol, and in the presence or absence of an activator, and removal of the metal component of the catalyst from the polyphenylene ether solution with a complex-forming or chelate-forming compound in aqueous solution, in the presence or absence of reducing and stabilizing substances and assistants for accelerating the interphase reactions and for phase separation, by a method in which the continuous removal of the copper catalyst is carried out in one or more mixer-settler stages at a phase volume ratio of the organic phase to the aqueous phase of from 1:0.1 to 1:1.0, preferably from 1:0.4 to 1:0.6.
摘要翻译：在从一元酚制备高分子量聚苯醚时除去催化剂，该二元酚在两个邻位进行烷基取代，而不是在对位，在间位可以是或不是烷基取代的，在由铜盐和有机胺获得的催化剂配合物的存在下，在15〜50℃下，与氧气进行氧化偶合反应，每份由1〜20份重量的溶剂单体苯酚的重量，并且在存在或不存在活化剂的情况下，在存在或不存在复合物形成或螯合形成化合物的情况下，在聚苯醚溶液中除去催化剂的金属组分减少和稳定物质和辅助剂，用于加速相间反应和相分离，方法是连续除去铜催化剂的方法是在一个或多个混合沉淀器以有机相与水相的相体积比为1:0.1至1:1.0，优选1:0.4至1:0.6。

2. 发明授权

US4696996A Preparation of polyphenylene ethers, and an apparatus for this purpose 失效
标题翻译：聚苯醚的制备及其用途
公开(公告)号：US4696996A
公开(公告)日：1987-09-29
申请号：US797884
申请日：1985-11-14
申请人： Hermann Brandt , Hermann Fischer , Hermann Dreher , Eduard Heil , Juergen Hambrecht , Herbert Naarmann , Adolf Echte , Hermann Gausepohl , Peter Siebel , Johann Swoboda , Gerd Schwoebel , Albert Nikles
发明人： Hermann Brandt , Hermann Fischer , Hermann Dreher , Eduard Heil , Juergen Hambrecht , Herbert Naarmann , Adolf Echte , Hermann Gausepohl , Peter Siebel , Johann Swoboda , Gerd Schwoebel , Albert Nikles
IPC分类号： B01J10/00 , B01J19/18 , C08G65/44 , C08G65/38
CPC分类号： C08G65/44 , B01J19/1862 , B01J19/1881 , B01J2219/00094 , B01J2219/00103 , B01J2219/0011
摘要： Polyphenylene ethers are prepared from monohydric phenols, which possess alkyl substituents in the two ortho-positions and, if desired, in the meta-position, but not in the para-position, by an oxidative coupling reaction with oxygen at from 15.degree. to 50.degree. C. and under from 1 to 10 bar in the presence of a catalyst complex, of a solvent and, if required, of an activator, by a method in which the conversion of the phenols is carried out in two more reaction zones, in which some or all of the solvent, the catalyst complex and the phenols and, where relevant, the activator is initially taken and is circulated by means of a conveying unit, and about 60-100% of the stoichiometric amount of oxygen required for the oxidative coupling is introduced into the first reaction zone and from 0 to about 40% of the said stoichiometric amount is introduced into the second reaction zone.
摘要翻译：聚苯醚由单羟基苯酚制得，它们在两个邻位具有烷基取代基，如果需要，在间位，而不是在对位，通过与15至50的氧的氧化偶联反应，在催化剂配合物存在下，在溶剂和如果需要的情况下，活化剂存在下，在1至10巴下，通过酚的转化在两个更多的反应区中进行，在其中一些或全部溶剂，催化剂络合物和酚，并且在相关的情况下，活化剂最初被摄取并通过输送单元循环，并且约60-100％的化学计量量的氧化所需的氧将偶联引入第一反应区，并将0至约40％的所述化学计量量引入第二反应区。

3. 发明授权

US4436870A Production of molding materials containing polyphenylene ethers 失效
标题翻译：生产含聚苯醚的成型材料
公开(公告)号：US4436870A
公开(公告)日：1984-03-13
申请号：US400689
申请日：1982-07-22
申请人： Klaus Hinselmann , Herbert Naarmann , Adolf Echte , Eduard Heil , Albert Nikles , Rudi W. Reffert , Juergen Hambrecht
发明人： Klaus Hinselmann , Herbert Naarmann , Adolf Echte , Eduard Heil , Albert Nikles , Rudi W. Reffert , Juergen Hambrecht
IPC分类号： C08L7/00 , B29C35/00 , B29C45/00 , C08G65/46 , C08J3/00 , C08J3/20 , C08L21/00 , C08L23/00 , C08L33/00 , C08L33/02 , C08L71/00 , C08L71/12 , C08L101/00 , C08L71/04
CPC分类号： C08J3/005 , C08G65/46 , C08L71/12 , Y10S525/905
摘要： Molding materials containing high molecular weight polyphenylene ethers are produced by a process in which a solution of a polyphenylene ether in an organic solvent, together with another polymer, is freed of solvent by multi-stage evaporation.The solvent is preferably an aromatic compound from the class comprising the hydrocarbons, halohydrocarbons, ethers or esters, the ratio of the other polymer to the polyphenylene ether is advantageously from 99:1 to 20:80 parts by weight, the other polymer is, in particular, a homopolymer or copolymer of styrene or of a homolog thereof, which may be modified with rubber, and the multi-stage evaporation process preferably comprises not less than two and not more than four working up stages.The evaporation is carried out in general at from 120.degree. to 280.degree. C. and under a pressure of from 1 to 3,000 mbar, advantageously in the presence of assistants which reduce the partial pressure, eg. water and/or methanol.
摘要翻译：含有高分子量聚苯醚的成型材料是通过多层蒸发而将有机溶剂中的聚苯醚与其它聚合物一起溶解的方法而制得的。溶剂优选为包含烃类，卤代烃类，醚类或酯类的芳族化合物，另一种聚合物与聚苯醚的比率有利地为99:1至20:80重量份，另一个聚合物为特别是可以用橡胶改性的苯乙烯或其同系物的均聚物或共聚物，多级蒸发方法优选包括不少于2个且不超过4个加工阶段。蒸发通常在120℃至280℃和1至3,000毫巴的压力下进行，有利的是在有助于降低分压的助剂的存在下进行。水和/或甲醇。

4. 发明授权

US4540772A Continuous preparation of nylon from aqueous salt solution in precondensation zone having baffles 失效
标题翻译：从具有挡板的预缩合区域的盐水溶液中连续制备尼龙
公开(公告)号：US4540772A
公开(公告)日：1985-09-10
申请号：US620837
申请日：1984-06-15
申请人： Gunter Pipper , Franz Schmidt , Rainer Theysohn , Siegfried Riegger , Eduard Heil , Hermann Fischer , Richard Thoma , Paul Matthies
发明人： Gunter Pipper , Franz Schmidt , Rainer Theysohn , Siegfried Riegger , Eduard Heil , Hermann Fischer , Richard Thoma , Paul Matthies
IPC分类号： C08G69/00 , C08G69/26 , C08G69/28 , C08L77/00
CPC分类号： C08G69/28
摘要： Nylons are prepared by a continuous process in which, in a precondensation zone, an aqueous solution of a salt of a dicarboxylic acid of 6 to 18 carbon atoms and a diamine of 6 to 18 carbon atoms is heated to 250.degree.-300.degree. C. under superatmospheric pressure, with simultaneous vaporization of water and formation of a prepolymer, the prepolymer and the vapor are separated, and the former is fed into a polycondensation zone and condensed under superatmospheric pressure of from 1 to 10 bar and at from 250.degree. to 300.degree. C., wherein the aqueous salt solution is condensed under superatomspheric pressure of from 1 to 10 bar in the first third of the tubular precondensation zone provided with baffles, until the degree of conversion is not less than 93%, and the prepolymer and the vapor phase are brought into intimate contact with one another in the remaining two thirds of the precondensation zone.
摘要翻译：尼龙通过连续方法制备，其中在预缩合区中将6至18个碳原子的二羧酸盐和6至18个碳原子的二胺的水溶液加热至250-300℃。在超大气压下，同时蒸发水和形成预聚物，将预聚物和蒸气分离，将前者加入缩聚区，并在1至10巴和250至300的超大气压下冷凝 ℃，其中盐水溶液在具有挡板的管状预缩合区的第一三分之一中在1至10巴的超大体压力下冷凝，直到转化率不低于93％，并且预聚物和气相在预缩合区的剩余三分之二处彼此紧密接触。

5. 发明授权

US4060517A Continuous manufacture of polyamides 失效
公开(公告)号：US4060517A
公开(公告)日：1977-11-29
申请号：US559255
申请日：1975-03-17
申请人： Friedrich Mertes , Helmut Doerfel , Eduard Heil , Claus Cordes
发明人： Friedrich Mertes , Helmut Doerfel , Eduard Heil , Claus Cordes
IPC分类号： C08G69/00 , C08G69/04 , C08G69/28 , C08G69/36 , G01N30/91
CPC分类号： C08G69/28 , C08G69/04 , C08G69/36 , G01N30/91
摘要： An improved process for the continuous manufacture of polyamides by continuously conveying the aqueous solution of a salt of essentially equivalent amounts of a diamine, or of a mixture of several diamines, and of a dicarboxylic acid, or of a mixture of several dicarboxylic acids, or of mixtures of such salts with lactams and/or aminocarboxylic acids, through several reaction zones under polyamide-forming conditions, wherein the mixture of starting materials is heated, in a first reaction zone, to from 200.degree. to 300.degree. C, preferably from 220.degree. to 280.degree. C, at pressures which are above the corresponding saturation vapor pressure of water and prevent the formation of a vapor phase, the pressure action on the polycondensation mixture is released in a second reaction zone and condensation of the mixture, to form high molecular weight polyamides, is then completed in further reaction stages. According to the invention,A. the mixture of starting materials is heated, in the first reaction zone, until the polycondensation conversion is at least 80% and preferably 90%,B. in the second zone the pressure acting on the polycondensation mixture is released, adiabatically, to levels of not less than 3 atmospheres, preferably not less than 5 atmospheres, and not more than 20 atmospheres, preferably not more than 15 atmospheres, so as to reach temperatures below 215.degree. C, preferably 210.degree. C,c. the polycondensation mixture is then heated in a third reaction zone, comprising a heat exchanger consisting of heat exchange elements connected in parallel, to from 220.degree. to 330.degree. C, preferably from 250.degree. to 300.degree. C, in the course of less than 5 minutes and preferably less than 1 minute, the heating being carried out preferably in the presence of the water vapor formed during the adiabatic release of the pressure (in stage b), with application of heat and evaporation of the bulk of the water, at the pressure level to which the pressure has previously been released or at a lower pressure, andD. in further reaction stages, the condensation is completed, under the conditions prevailing at the end of the third reaction zone and, finally, by conventional methods, to form high molecular weight polyamides.

6. 发明授权

US4056514A Continuous manufacture of polybutylene terephthalates 失效
标题翻译：聚苯乙烯邻苯二甲酸酯的连续制造
公开(公告)号：US4056514A
公开(公告)日：1977-11-01
申请号：US668284
申请日：1976-03-18
申请人： Hugo Strehler , Ludwig Beer , Eduard Heil , Friedrich Urbanek , Hermann Fischer
发明人： Hugo Strehler , Ludwig Beer , Eduard Heil , Friedrich Urbanek , Hermann Fischer
IPC分类号： C08G63/00 , C08G63/78 , C08G63/85 , C08G63/16
CPC分类号： C08G63/78 , C08G63/85
摘要： A process for the continuous manufacture of linear, high molecular weight, polybutylene terephthalates, in which dimethyl terephthalate is trans-esterified with 1,4-butanediol, if desired in the presence of up to 40 mole% of other starting materials which form linear polyesters, in the molar ratio of from 1:1.2 to 1:1.5, in a plurality of successive stages at temperatures rising from 160.degree. to 230.degree. C, the mixture thus obtained is passed, at from 230.degree. to 270.degree. C and from 2 mm Hg to 20 mm Hg, upward through a bundle of stationary heated tubes, and immediately thereafter through a hold tank, with the proviso that the volume of the hold tank is at least 1/4 and at most 2.5 times the volume of the tube bundle and the mean residence time in the tube bundle and hold tank together is from 10 to 60 minutes, and the precondensate thus obtained is polycondensed at from 240.degree. to 260.degree. C and from 0.1 to 2 mm Hg. with continuous formation of thin films.The polybutylene terephthalates manufactured by the above process may be used for the manufacture of products such as fibers, films, sheeting and injection moldings.

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