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    Catalytic process for the preparation of phosphazene polymers
    4.
    发明授权
    Catalytic process for the preparation of phosphazene polymers 失效
    用于制备磷腈聚合物的催化方法

    公开(公告)号：US4124567A

    公开(公告)日：1978-11-07

    申请号：US895259

    申请日：1978-04-10

    申请人： Ronald L. Dieck ,  Alan B. Magnusson

    发明人： Ronald L. Dieck ,  Alan B. Magnusson

    IPC分类号： C08F299/00 ,  C01B21/098 ,  C08F290/00 ,  C08G79/00 ,  C08G79/02 ,  C08J9/04 ,  C08J9/06 ,  C08L85/02

    CPC分类号： C08J9/06 ,  C08G79/025 ,  C08L85/02 ,  C08J2385/02 ,  Y10S260/24

    摘要： A process is disclosed for the catalytically-induced preparation of phosphazene polymers. Cyclic halophosphazenes are polymerized in the presence of a catalytically sufficient amount of a compound having the formula M(OR').sub.x where M is an alkali metal or alkaline earth metal, x is equal to the valence of the metal and R' is C.sub.1 to C.sub.10 linear or branched alkyl, C.sub.1 to C.sub.10 substituted linear or branched alkyl, the substituent selected from the group consisting of nitro, C.sub.1 to C.sub.10 alkyl, C.sub.1 to C.sub.10 alkoxy, C.sub.6 to C.sub.10 aryl and C.sub.6 to C.sub.10 aryloxy, or N.sub.3 P.sub.3 Cl.sub.z (OR').sub.6-z wherein R' is as defined above and z equals 0 to 5.

    摘要翻译： 公开了催化诱导的磷腈聚合物的制备方法。 在催化足够量的具有式M（OR'）x的化合物的存在下，环状卤代膦腈聚合，其中M是碱金属或碱土金属，x等于金属的化合价，R'为C1至 C10直链或支链烷基，C1至C10取代的直链或支链烷基，选自硝基，C1至C10烷基，C1至C10烷氧基，C6至C10芳基和C6至C10芳氧基的取代基，或N3P3Clz（OR' ）6-z其中R'如上定义，z等于0至5。

    Poly(dialkylaminoaryloxyphosphazene) polymers and foams
    6.
    发明授权
    Poly(dialkylaminoaryloxyphosphazene) polymers and foams 失效
    聚（二烷基氨基氧基磷腈）聚合物和泡沫

    公开(公告)号：US4055523A

    公开(公告)日：1977-10-25

    申请号：US714526

    申请日：1976-08-16

    申请人： Ronald L. Dieck ,  Alan B. Magnusson ,  Edwin J. Quinn

    发明人： Ronald L. Dieck ,  Alan B. Magnusson ,  Edwin J. Quinn

    IPC分类号： C08L85/00 ,  C08G79/00 ,  C08G79/02 ,  C08J9/04 ,  C08L85/02

    CPC分类号： C08L85/02 ,  C08G79/025 ,  Y10S260/24

    摘要： Poly(aryloxyphosphazene) polymers and foams thereof having di(C.sub.1 -C.sub.10)alkylaminophenoxy groups are described. The polymers consist of the units which occur in a nonregular fashion and are represented by the following general formula: ##STR1## wherein R.sub.1 and R.sub.2 are the same or different and are C.sub.1 -C.sub.10 linear or branched alkyl radical. Copolymeric dialkylaminoaryloxy-aryloxyphosphazenes are disclosed represented by units of the general formula: ##STR2## wherein R.sub.1 and R.sub.2 are defined above and R represents hydrogen, halogen, C.sub.1 -C.sub.10 linear or branched alkyl radical, or C.sub.1 -C.sub.4 linear or branched alkoxy radical substituted on any sterically permissible position on the other phenoxy group. The radical NR.sub.1 R.sub.2 is substituted in the meta or para position on the phenoxy radical. The polymers are elastomers, have desirable tensile strengths and may be used to form flexible or semi-rigid films, sheets, and foams. The polymers are extremely fire retardant and produce low smoke loads when heated in an open flame. They readily form salts with mineral acids that are water soluble.

    摘要翻译： 描述了具有二（C1-C10）烷基氨基苯氧基的聚（芳氧基磷腈）聚合物及其泡沫。 聚合物由以非规则形式出现并由下列通式表示的单元组成：其中R 1和R 2相同或不同，为C 1 -C 10直链或支链烷基。 公开的共聚二烷基氨基芳氧基 - 芳氧基磷腈由以下通式的单元表示：其中R 1和R 2如上定义，R代表氢，卤素，C 1 -C 10直链或支链烷基或C 1 -C 4直链 或在另一个苯氧基的任何空间允许位置上取代的支链烷氧基。 在苯氧基上的间位或对位取代基NR1R2。 聚合物是弹性体，具有所需的拉伸强度，并且可用于形成柔性或半刚性膜，片和泡沫。 当在明火中加热时，聚合物具有极强的阻燃性和低烟度。 它们容易与水溶性的无机酸形成盐。

    Catalytic process for the preparation of phosphazene polymers
    7.
    发明授权
    Catalytic process for the preparation of phosphazene polymers 失效
    用于制备磷腈聚合物的催化方法

    公开(公告)号：US4110421A

    公开(公告)日：1978-08-29

    申请号：US731745

    申请日：1976-10-12

    申请人： Ronald L. Dieck ,  Alan B. Magnusson

    发明人： Ronald L. Dieck ,  Alan B. Magnusson

    IPC分类号： C08F299/00 ,  C01B21/098 ,  C08F290/00 ,  C08G79/00 ,  C08G79/02 ,  C08J9/04 ,  C08J9/06 ,  C08L85/02 ,  C01B25/10

    CPC分类号： C08J9/06 ,  C08G79/025 ,  C08L85/02 ,  C08J2385/02 ,  Y10S260/24

    摘要： A process is disclosed for the catalytically-induced preparation of phosphazene polymers. Cyclic halophosphazenes are polymerized in the presence of a catalytically sufficient amount of a compound having the formula M(OR').sub.x where M is an alkali metal or alkaline earth metal, x is equal to the valence of the metal and R' is C.sub.1 to C.sub.10 linear or branched alkyl, C.sub.1 to C.sub.10 substituted linear or branched alkyl, the substituent selected from the group consisting of nitro, C.sub.1 to C.sub.10 alkyl, C.sub.1 to C.sub.10 alkoxy, C.sub.6 to C.sub.10 aryl and C.sub.6 to C.sub.10 aryloxy, or N.sub.3 P.sub.3 Cl.sub.z (OR').sub.6-z wherein R' is as defined above and z equals 0 to 5.BACKGROUND OF THE INVENTIONThe present invention relates to a process for the preparation of phosphazene polymers. More specifically, the present invention relates to a method for catalytically producing polyphosphazenes.DESCRIPTION OF THE PRIOR ARTPreparation of the polyphosphazenes has generally been recognized to be most readily accomplished by the technique of Allcock, et al as disclosed in U.S. Pat. No. 3,370,020. The preparation involves the use of the cyclic trimer, hexachlorocyclotriphosphazene as the sole starting material in what is essentially a melt polymerization technique. Purified trimer is thermally polymerized under sealed tube conditions at about 250.degree. C. for 20 to 48 hours to give substantially linear poly(dichlorophosphazene) and some unreacted trimer. The cyclic tetramer also is effective in this reaction. While the product of this reaction, poly(dichlorophosphazene), itself is a good elastomer of very high molecular weight, e.g. over one million, it suffers the severe disadvantage of undergoing relatively facile hydrolytic cleavage of the P-Cl bond followed by degradation of the polymer. The prior art has shown that attempts to increase the stability of the dichloropolymer by continued heating have proved ineffective since the highly crosslinked rubbery material produced by such heating is also hydrolytically unstable. Recent success for obtaining polyphosphazene polymers of good hydrolytic stability has been achieved by substituting all of the halogen on the linear polymer produced from the cyclic trimer by various organic species. The following scheme discloses the state of the prior art to date in which high molecular weight polyphosphazenes are produced by treating poly(dichlorophosphazene) I with a variety of organic nucleophiles, e.g. alcohols, phenols, and amines, to obtain the corresponding completely substituted polymers II, III and IV which are hydrolytically stable. ##STR1##The time period for accomplishing the ring opening polymerization reaction is economically disadvantageous, and considerable effort has been expended ascertaining what catalysts could be employed to successfully promote such ring opening polymerization. A variety of investigators have found that carboxylic acids, ethers, ketones, alcohols, nitromethane and metals such as zinc, tin or sodium, enhance the rate of polymerization of the cyclic trimer. The rate of enhancement is such that extensive polymerization is induced in 24 hours at 210.degree. C. compared to only 3% conversion to polymer in the same time in the absence of any catalyst. Comparable catalytic activity has also been shown by sulfur (at 215.degree.-254.degree. C.), by dialkyl paracresols and quinone or hydroquinone. See, for example, Allcock, "Phosphorus Nitrogen Compounds", Academic Press 1972, page 316 and following.The mechanism proposed for such catalytic enhancement in the conversion of the cyclic trimer to the linear polymer suggests that reagents that facilitate removal of chloride ion from phosphorus should be active catalysts. However, a variety of compounds, including those that should be good chloride acceptors, have been found to have no effect on the polymerization including carbon tetrachloride, chloroform, ligroin, benzene, biphenyl, cyclohexane, ethylbromide, phosphorus pentachloride, ammonia, water, mercuric chloride, aluminum chloride and stannic chloride.While the earlier discussed catalysts are effective for the purpose of catalyzing the ring-opening polymerization reaction, one of their major drawbacks is that the polymerization actually promotes the crosslinking reaction. Thus, while the disappearance of the cyclic trimer is enhanced, the resulting crosslinked polymer not only suffers the disadvantages of the prior art hydrolytically unstable crosslinked polychlorophosphazene V, but is additionally less reactive to the earlier mentioned nucleophiles due to its inherent insolubility. Further, there is no effective way to control molecular weight of the final product, such being so high as to make difficult any further manipulation such as melt or solution casting.There is, therefore, a need for effective catalysts to produce linear polyphosphazenes.SUMMARY OF THE INVENTIONIt is an object of the present invention to provide a novel process for the production of phosphazene polymers.It is a further object of the present invention to provide a novel process for the production of phosphazene polymeric foams.It is an additional object of the present invention to provide a novel process for the production of low molecular weight phosphazene polymers and foams from such low molecular weight polyphosphazenes.It is another object of the present invention to provide a novel process for the production of low molecular weight phosphazene polymers and foams from such low molecular weight polyphosphazenes which comprises thermally polymerizing a cyclic phosphazene with a catalytically sufficient amount of an alkali or alkaline earth metal compound.It is a further object of the present invention to provide a novel process for the production of low molecular weight phosphazene polymers and foams therefrom which comprises thermally polymerizing a cyclic phosphazene with a catalytically sufficient amount of an alkoxy-substituted cyclotriphosphazene.

    摘要翻译： 公开了催化诱导的磷腈聚合物的制备方法。 在催化足够量的具有式M（OR'）x的化合物的存在下，环状卤代膦腈聚合，其中M是碱金属或碱土金属，x等于金属的化合价，R'为C1至 C10直链或支链烷基，C1至C10取代的直链或支链烷基，选自硝基，C1至C10烷基，C1至C10烷氧基，C6

    Chain extending polyurethanes with a large excess of water
    10.
    发明授权
    Chain extending polyurethanes with a large excess of water 失效
    链延长聚氨酯与大量过量的水

    公开(公告)号：US4049632A

    公开(公告)日：1977-09-20

    申请号：US705117

    申请日：1976-07-14

    申请人： Alan B. Magnusson ,  Howard S. White

    发明人： Alan B. Magnusson ,  Howard S. White

    IPC分类号： C08G18/10 ,  C08G18/42 ,  C08G18/30 ,  C08G18/82

    CPC分类号： C08G18/42 ,  C08G18/10 ,  Y10S528/902

    摘要： A polyurethane-urea composition is described that is highly resistant to textile fiber-dressings. The composition is a product from the reaction of an ester urethane prepolymer formed from the reaction of a diisocyanate and a hydroxy-terminated polyester of equivalent weight 400-1,000 in which the ratio of isocyanate functionality:hydroxy functionality is from 2.0:1 to 4.0:1; and an excess of water.

    摘要翻译： 描述了高度耐纺织纤维敷料的聚氨酯 - 尿素组合物。 该组合物是由二异氰酸酯和当量重量为400-1,000的羟基封端的聚酯反应形成的酯氨基甲酸酯预聚物的反应产物，其中异氰酸酯官能度：羟基官能度的比例为2.0:1至4.0:1， 1; 和过量的水。