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    • 12. 发明授权
    • Higher molecular weight arylene sulfide resin and process for its
preparation
    • 较高分子量的亚芳基硫醚树脂及其制备方法
    • US5110901A
    • 1992-05-05
    • US580720
    • 1990-09-11
    • Kenneth C. HooverEarl Clark, Jr.Roy E. RegerLacey E. ScogginsAfif M. Nesheiwat
    • Kenneth C. HooverEarl Clark, Jr.Roy E. RegerLacey E. ScogginsAfif M. Nesheiwat
    • C08G75/02
    • C08G75/0259
    • In a first embodiment, arylene sulfide resins are provided by contacting, in a polymerization mixture, during a polymerization process, reactants comprising: an alkali metal sulfide, an organic amide, an alkali metal carboxylate, water and a monomer source which comprises at least one dihaloaromatic compound. The amount of alkali metal carboxylate present during the polymerization process ranges from about 0.01 to about 0.03 mole per each mole of sulfur present in the resulting arylene sulfide resin. The total amount of water present during the polymerization process ranges from about 1.02 to about 2.1 moles per each mole of sulfur present in the resulting arylene sulfide resin.In a second embodiment, arylene sulfide resins are provided by contacting, in a polymerization mixture, during a polymerization process, reactants comprising: an alkali metal sulfide, an organic amide, an alkali metal carboxylate, water and a monomer source which comprises a mixture of at least one dihaloaromatic compound and at least one polyhaloaromatic compound having more than two halogen substituents per molecule. The ranges of the amount of alkali metal carboxylate present during the polymerization process and the total amount of water present during the polymerization process are identical to those amounts disclosed in the first embodiment. The amount of polyhaloaromatic compound initially present ranges from about 0.0001 to about 0.01 mole per each mole of dihaloaromatic compound present prior to the initiation of the polymerization process.
    • 在第一个实施方案中,亚芳基硫醚树脂通过在聚合反应过程中使聚合反应中的反应物与碱金属硫化物,有机酰胺,碱金属羧酸盐,水和单体源接触来提供,所述反应物包括至少一种 二卤化合物。 在聚合过程中存在的碱金属羧酸盐的量为所得亚芳基硫醚树脂中存在的每摩尔硫的约0.01至约0.03摩尔。 在聚合过程中存在的水的总量范围为所得亚芳基硫醚树脂中存在的每摩尔硫的约1.02至约2.1摩尔。 在第二个实施方案中,亚芳基硫醚树脂是通过在聚合反应过程中使聚合反应中的反应物与碱金属硫化物,有机酰胺,碱金属羧酸盐,水和单体来源接触来提供的, 至少一种二卤代芳族化合物和每分子具有多于两个卤素取代基的至少一种多卤芳族化合物。 在聚合过程中存在的碱金属羧酸盐的量的范围和在聚合过程中存在的水的总量与第一实施方案中公开的量相同。 在开始聚合过程之前,存在的每摩尔二卤代芳族化合物最初存在的多卤代芳族化合物的量为约0.0001至约0.01摩尔。
    • 15. 发明授权
    • Preparation of branched polymers of arylene sulfide
    • 亚芳基硫醚支化聚合物的制备
    • US4282347A
    • 1981-08-04
    • US66584
    • 1979-08-14
    • Dale O. TieszenLacey E. Scoggins
    • Dale O. TieszenLacey E. Scoggins
    • D01F6/76C08G75/02C08G75/06C08G75/14C08G75/16
    • C08G75/0231C08G75/025
    • A process for the production of branched polymers of arylene sulfide in which a reaction mixture of (1) at least one p-dihalobenzene, (2) at least one alkali metal sulfide, (3) at least one organic amide, (4) water in an amount of about 1.0 mole to about 2.4 moles per mole of alkali metal sulfide, and (5) at least one alkali metal carboxylate is contacted under polymerization conditions for a time sufficient to form arylene sulfide polymer and the arylene sulfide polymer formed in said reaction mixture is contacted under polymerization conditions with a polyhaloaromatic compound having more than two halogen substituents per molecule for a time having a range of up to about 75 minutes before entering upon termination of the polymerization process. An embodiment of the process in which the alkali metal sulfide is produced in situ by the reaction of an excess of alkali metal hydroxide with alkali metal hydrosulfide. An embodiment in which carbon dioxide is contacted with arylene sulfide polymer formed in the reaction mixture to stabilize the polymer. A melt spun fiber that is the product of this reaction.
    • 一种制备亚芳基硫化物支化聚合物的方法,其中(1)至少一种对二卤代苯,(2)至少一种碱金属硫化物,(3)至少一种有机酰胺,(4)水 其量为每摩尔碱金属硫化物约1.0摩尔至约2.4摩尔,和(5)至少一种碱金属羧酸盐在聚合条件下接触足以形成亚芳基硫醚聚合物的时间,并且所述 反应混合物在聚合条件下与每个分子具有多于两个卤素取代基的多卤芳族化合物接触一段时间,在聚合过程终止之前达到约75分钟。 通过过量碱金属氢氧化物与碱金属氢硫化物的反应原位产生碱金属硫化物的方法的一个实施方案。 二氧化碳与反应混合物中形成的亚芳基硫醚聚合物接触以稳定聚合物的实施方案。 作为该反应的产物的熔纺纤维。
    • 16. 发明授权
    • Producing fiber grade polyamide from terephthalic acid and
5-methyl-1,9-nonanediamine
    • 由对苯二甲酸和5-甲基-1,9-壬二胺生产纤维级聚酰胺
    • US4172194A
    • 1979-10-23
    • US851328
    • 1977-11-14
    • Lacey E. ScogginsRobert W. Campbell
    • Lacey E. ScogginsRobert W. Campbell
    • C08G69/28
    • C08G69/28
    • Terephthalic acid and a diamine, always including 5-methyl-1,9-nonanediamine, and a lower fatty acid, e.g., acetic acid, are admixed with water, the water is evaporated, the concentrated mixture is heated (100.degree.-200.degree. C., 1/2-2 hrs.); then heated further (125.degree.-295.degree. C., 1/2-3 hrs., autogenous pressure up to 150-600 psig) with venting as needed; decompressed to atmospheric pressure (1/4-2 hrs., 245.degree.-295.degree. C.); and heated (270.degree.-295.degree. C., 1/2-2 hrs.) to produce a polyamide having good acid and basic dye receptivity, inherent viscosity, melt spinning and drawing characteristics. An isomeric mixture of diamines containing 5-methyl-1,9-nonanediamine, and 2,4-dimethyl-1,8-octanediamine, 2,4,6-trimethyl-1,7-heptanediamine and/or 4-isopropyl-1,7-heptanediamine can be the starting 5-methyl-1,9-nonanediamine-furnishing material. The diamine-furnishing material contains at least one principal diamine component having the formula H.sub.2 NRNH.sub.2, where R is selected from the group consisting of 5-methylnonamethylene, 2,4-dimethyloctamethylene, 2,4,6-trimethylheptamethylene, and 4-isopropylheptamethylene, the R in the formula of at least about 50 percent of the principal diamine component molecules initially present in the reaction being 5-methylnonamethylene. Other structural units, up to about 20 mole percent, can be present in the product which preferably will be at least 90 mole percent and up to about 98 mole percent and even up to about 100 mole percent derived from the foregoing recited terephthalic acid and diamines. Such other structural units are supplied by, e.g., other diamines, other dicarboxylic acids, amino acids and lactams.
    • 将对苯二甲酸和二胺(总是包括5-甲基-1,9-壬二胺)和低级脂肪酸(例如乙酸)与水混合,蒸发水,将浓缩的混合物加热(100-200℃) C.,1 / 2-2小时); 然后根据需要进一步加热(125°-295℃,1 / 2-3小时,自生压力至150-600psig) 减压至大气压(1 / 4-2小时,245℃-295℃); 加热(270°-295℃,1 / 2-2小时),得到具有良好的酸和碱性染料接受性,特性粘度,熔融纺丝和拉伸特性的聚酰胺。 含有5-甲基-1,9-壬二胺和2,4-二甲基-1,8-辛二胺,2,4,6-三甲基-1,7-庚二胺和/或4-异丙基-1的二胺的异构体混合物 ,7-庚二胺可以是起始的5-甲基-1,9-壬二胺装饰材料。 二胺家具材料含有至少一种具有式H2NRNH2的主要二胺组分,其中R选自5-甲基亚麻醇,2,4-二甲基八亚甲基,2,4,6-三甲基亚庚基和4-异丙基亚庚基, 式中最初存在于反应中的至少约50%的主要二胺组分分子中的R为5-甲基亚麻醇。 最高约20摩尔%的其它结构单元可以存在于产物中,其优选为前述对苯二甲酸和二胺衍生的至少90摩尔%和高达约98摩尔%,甚至高达约100摩尔% 。 这样的其它结构单元由例如其它二胺,其它二羧酸,氨基酸和内酰胺提供。