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    • 1. 发明授权
    • Continuous removal of the catalyst from polyphenylene ethers
    • 从聚苯醚连续除去催化剂
    • US4654418A
    • 1987-03-31
    • US627984
    • 1984-07-05
    • Rosemarie BergerHermann DreherJuergen HambrechtEduard HeilRudi W. ReffertJohann SwobodaAdolf EchtePeter Siebel
    • Rosemarie BergerHermann DreherJuergen HambrechtEduard HeilRudi W. ReffertJohann SwobodaAdolf EchtePeter Siebel
    • C08G65/46C08G65/42
    • C08G65/46
    • 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.
    • 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。
    • 3. 发明授权
    • Stabilization of polyphenylene ether solutions
    • 聚苯醚溶液的稳定化
    • US4496679A
    • 1985-01-29
    • US531656
    • 1983-09-13
    • Juergen HambrechtRudi W. ReffertAdolf EchteJohann Swoboda
    • Juergen HambrechtRudi W. ReffertAdolf EchteJohann Swoboda
    • C08G65/46C08L71/04
    • C08G65/46
    • A process for the preparation of high molecular weight polyphenylene ethers from alkyl-substituted monohydric phenols by an oxidative coupling reaction with oxygen in the presence of a catalyst complex of a copper salt and an organic amine, subsequent stopping of the reaction and removal of the metal component of the catalyst by addition of chelating and/or salt-forming agents, wherein the polymer solution is treated with a compound having the general structure: ##STR1## where R.sup.2 and R.sup.3 can be identical or different and each is OH, NH.sub.2, NHR.sup.5, where R.sup.5 is alkyl or cycloalkyl, or SH, and where R.sup.1 and R.sup.4 are identical or different, being hydrogen, alkyl, cycloalkyl, aryl, carbonyl, carboxyl, carboxyalkyl or nitrile, and can be linked to form a ring, advantageously in an amount of from 0.1 to 100 mmoles and advantageously in from 1 to 20% strength aqueous solutions.
    • 在铜盐和有机胺的催化剂络合物存在下,通过与氧的氧化偶联反应从烷基取代的一元酚制备高分子量聚苯醚的方法,随后停止反应和除去金属 通过加入螯合和/或成盐剂的催化剂组分,其中聚合物溶液用具有以下通式结构的化合物处理:其中R 2和R 3可以相同或不同,并且各自为OH,NH 2,NHR 5 ,其中R 5是烷基或环烷基或SH,并且其中R 1和R 4相同或不同,是氢,烷基,环烷基,芳基,羰基,羧基,羧基烷基或腈,并且可以连接形成环,有利地在 量为0.1至100毫摩尔,有利地为1至20%强度的水溶液。
    • 4. 发明授权
    • Removal of the catalyst from polyphenylene ethers
    • 从聚苯醚中除去催化剂
    • US4482705A
    • 1984-11-13
    • US518612
    • 1983-07-29
    • Juergen HambrechtRudi W. ReffertVolker MuenchAdolf EchteJohann Swoboda
    • Juergen HambrechtRudi W. ReffertVolker MuenchAdolf EchteJohann Swoboda
    • C08G65/46
    • C08G65/46
    • High molecular weight polyphenylene ethers are prepared from monohydric phenols by an oxidative coupling reaction with oxygen in the presence of a catalyst complex obtained from a copper salt and an organic amine by a method wherein the metal component of the catalyst is separated off, after the polymerization, by the addition of a polymeric polycarboxylic acid which is essentially composed of unsaturated monofunctional or difunctional carboxylic acids and/or their anhydrides.Advantageously, the polymeric polycarboxylic acids used are homopolymers or copolymers of (a) from 50 to 100% by weight of one or more unsaturated monofunctional acids of 3 to 10 carbon atoms and/or one or more difunctional acids or their anhydrides of 4 to 6 carbon atoms and from 0 to 50% by weight of one or more monomers which do not possess an acid function and can be copolymerized with (a).
    • 在由铜盐和有机胺得到的催化剂配合物的存在下,通过与氧的氧化偶合反应,通过催化剂的金属组分在聚合后分离的方法,由一元酚制备高分子量聚苯醚 通过加入基本上由不饱和单官能或双官能羧酸和/或它们的酸酐组成的聚合多元羧酸。 有利地,所使用的聚合多元羧酸是(a)50至100重量%的一种或多种3至10个碳原子的不饱和单官能酸和/或一种或多种双官能酸或其酸酐4至6的均聚物或共聚物 碳原子和0至50重量%的一种或多种不具有酸官能并可与(a)共聚的单体。
    • 6. 发明授权
    • Treatment of (Co)polymers to remove residual monomers
    • (Co)聚合物的处理以除去残留的单体
    • US4503219A
    • 1985-03-05
    • US489558
    • 1983-04-28
    • Rudi W. ReffertJuergen HambrechtRudolf H. JungAdolf Echte
    • Rudi W. ReffertJuergen HambrechtRudolf H. JungAdolf Echte
    • C08F6/00C08G6/00C08J3/00
    • C08F6/006
    • (Co)polymers which are composed of one or more monomers from the group comprising(a) the vinyl-aromatic monomers and(b) the ethylenically unsaturated monomersand furthermore contain one or more monomer components (a) or (b), or (a) and (b), as unreacted residual monomers are treated at above the glass temperature of the (co)polymer and in the presence of one or more assistants, which have been added to the (co)polymer. The assistant used is a bicyclic compound of the general formula I ##STR1## where X is a methylene, ethylene, 1,1-ethenyl, 1,2-ethenyl, carbonyl, azo, amino, ether or thioether group which is unsubstituted or substituted by halogen, alkyl, alkenyl, cycloalkyl, aryl, carboxyl, carboxyalkyl, an ether group or a thioether group, R.sup.1, R.sup.2, R.sup.3 and R.sup.4 are each hydrogen, halogen, alkyl, alkenyl, cycloalkyl, aryl, carboxyalkyl or nitrile, R.sup.5 and R.sup.6 are each hydrogen, halogen, alkyl or carboxyalkyl, and R.sup.7 and R.sup.8 are each hydrogen, halogen, alkyl, alkenyl, aryl, carboxyalkyl, carboxyl or nitrile.
    • (a)乙烯基芳族单体和(b)烯键式不饱和单体并且还含有一种或多种单体组分(a)或(b)或(a)的单体组分 a)和(b)中,作为未反应的残余单体在(共)聚合物的玻璃化温度以上和在已加入到(共))聚合物中的一种或多种助剂的存在下进行处理。 使用的助剂是通式I的双环化合物,其中X是未取代或取代的亚甲基,亚乙基,1,1-乙烯基,1,2-乙烯基,羰基,偶氮,氨基,醚或硫醚基 卤素,烷基,烯基,环烷基,芳基,羧基,羧基烷基,醚基或硫醚基,R1,R2,R3和R4各自为氢,卤素,烷基,烯基,环烷基,芳基,羧烷基或腈,R5和 R 6各自为氢,卤素,烷基或羧基烷基,R 7和R 8各自为氢,卤素,烷基,烯基,芳基,羧基烷基,羧基或腈。
    • 8. 发明授权
    • Process and apparatus for removing vaporizable constituents from viscous
solutions or melts of thermoplastics
    • 从热塑性塑料的粘稠溶液或熔体中除去可挥发成分的方法和设备
    • US4153501A
    • 1979-05-08
    • US768636
    • 1977-02-14
    • Peter FinkHans WildJohann ZizlspergerRudi W. ReffertGunter Thielen
    • Peter FinkHans WildJohann ZizlspergerRudi W. ReffertGunter Thielen
    • B01D1/22B01D19/00B29B13/02C08F6/10F28F7/02
    • C08F6/10B01D1/22B01D19/0021B29B13/02F28F7/02Y10S159/10
    • A process for removing vaporizable constituents from high-viscosity solutions or melts of thermoplastics by continuous evaporation along a heated devolatilization zone and separation of the vapor phase from the liquid phase in a downstream separating vessel. The plastic solution or melt is first heated stepwise in increments, in the devolatilization zone, while the product is in the form of thin layers from about 0.5 to 4 mm, so as to maintain a temperature difference of less than 50.degree. C. between the heat transfer medium and the plastic solution or melt until the devolatilization temperature is reached, the distribution of the solution or melt to form thin layers of product taking place while the temperature conditions still correspond to those of the feed of solution or melt, after which the vaporizable constituents are evaporated so as to form a two-phase system of vapor and melt, and the heat of evaporation absorbed is substantially returned to the product during the evaporation along the devolatilization zone. The process permits the removal of vaporizable constituents under mild conditions.
    • 通过沿着加热的脱挥发分区连续蒸发并在下游分离容器中将液相从液相中分离出来,从热塑性塑料的高粘度溶液或熔体中除去可挥发成分的方法。 首先在脱挥发区中逐步逐渐加热塑料溶液或熔体,同时产物为0.5〜4mm的薄层形式,以保持温度差在50℃以下 传热介质和塑料溶液或熔体,直到达到脱挥发分温度,溶液或熔体的分布形成薄层产品,同时温度条件仍然对应于溶液或熔体进料的温度条件,之后 可蒸发的成分被蒸发以形成蒸气和熔体的两相体系,并且在沿着脱挥发分区的蒸发期间吸收的蒸发热量基本上返回到产物中。 该方法允许在温和条件下除去可汽化组分。