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91. 发明授权

US3379670A Process for preparation of spinnable solutions of acrylonitrile polymers or copolymers having a high-acrylonitrile content 失效
标题翻译：制备具有高丙烯腈含量的丙烯腈聚合物或共聚物的可纺丝溶液的方法
公开(公告)号：US3379670A
公开(公告)日：1968-04-23
申请号：US65933067
申请日：1967-08-09
申请人： SNIA VISCOSA
发明人： DEMETRIO CORRADI , ALBERTO PASIN
IPC分类号： C08F20/42 , C08F20/44 , C08G18/10 , C08J9/24 , C09D175/04
CPC分类号： C08G18/10 , C08F2/36 , C08F20/42 , C08F20/44 , C08J9/24 , C09D175/04 , C08G18/8061 , C08L27/04
摘要： Spinnable solutions of polyacrylonitrile, or of copolymers containing over 85% by weight of acrylonitrile, are produced by polymerization of the monomer(s) in dimethyl formamide in at least two sequential stages, in the first of which the polymerization is carried out at 60 DEG to 65 DEG C. until reaching not less than 30% and not more than 40% conversion of the monomer(s), while in the second stage or the following stages the polymerization is carried on under controlled temperature conditions until reaching a higher conversion, the amount of dimethyl formamide and catalyst required to attain said higher conversion being divided into as many fractions as there are stages and one of said fractions being individually added at the beginning of each stage. The final conversion attained is desirably in the range 70 to 80%. The temperature conditions may be controlled by carrying out the process under sub-atmospheric pressure, in which case the polymerization is terminated by increasing the pressure and distilling off unreacted monomer(s). In the examples, the polymerization is carried out in two stages. In Examples 1 and 3 copolymers of acrylonitrile, sodium allyl sulphonate and methyl methacrylate are prepared and in Example 2 a copolymer of acrylonitrile, sodium allyl sulphonate and ethyl acrylate. Lauroyl peroxide is used as catalyst and thiourea dioxide is present in the reaction solutions of Examples 1 and 2.
摘要翻译：聚丙烯腈或含有超过85重量％丙烯腈的共聚物的可纺溶液是通过在至少两个连续阶段中将二甲基甲酰胺中的单体聚合制备的，其中第一个聚合反应在60℃进行至65℃，直到达到不少于30％且不超过40％的单体转化率，而在第二阶段或后续阶段，聚合在受控温度条件下进行直至达到更高的转化率，达到所述较高转化率所需的二甲基甲酰胺和催化剂的量被分成与阶段相同的分数，并且在每个阶段开始时分别加入一个所述级分。所得到的最终转化率优选为70〜80％。可以通过在亚大气压下进行该方法来控制温度条件，在这种情况下，通过增加压力并蒸发未反应的单体终止聚合。在实施例中，聚合分两个阶段进行。在实施例1和3中，制备丙烯腈，烯丙基磺酸钠和甲基丙烯酸甲酯的共聚物，在实施例2中是丙烯腈，烯丙基磺酸钠和丙烯酸乙酯的共聚物。月桂酰过氧化物用作催化剂，二氧化硫脲存在于实施例1和2的反应溶液中。

92. 发明授权

US3328332A Process for solution polymerization of acrylonitrile 失效
公开(公告)号：US3328332A
公开(公告)日：1967-06-27
申请号：US50417165
申请日：1965-10-23
申请人： EASTMAN KODAK CO
发明人： DANNELLY CLARENCE C , CALDWELL JOHN R
IPC分类号： C08F20/44
CPC分类号： C08F20/44 , C08F2/36

93. 发明授权

US3297670A Process for removal of silver nitrate from silver nitrate containing acrylonitrile polymers 失效
标题翻译：从含硝酸银的丙烯腈聚合物中除去硝酸银的方法
公开(公告)号：US3297670A
公开(公告)日：1967-01-10
申请号：US38325364
申请日：1964-07-16
申请人： GRACE W R & CO
发明人： EHRIG RAYMOND J
IPC分类号： C08F6/02 , C08F20/44
CPC分类号： C08F6/02 , C08F2/16 , C08F20/44 , C08L33/20

94. 发明授权

US3285894A Polymerization initiators comprising alkali metal alcoholates 失效
标题翻译：包含碱金属醇化物的聚合引发剂
公开(公告)号：US3285894A
公开(公告)日：1966-11-15
申请号：US31567963
申请日：1963-10-11
申请人： CESKOSLOVENSKA AKADEMIE VED
发明人： DRAHOSLAV LIM , JIRI TREKOVAL
IPC分类号： C08F4/08 , C08F4/46 , C08F20/44
CPC分类号： C08F4/08 , C08F2/36 , C08F20/44

95. 发明授权

US3274140A Production of polymer solutions 失效
标题翻译：生产聚合物溶液
公开(公告)号：US3274140A
公开(公告)日：1966-09-20
申请号：US23877062
申请日：1962-11-19
申请人： COURTAULDS LTD
发明人： JOHN BREALEY GRAHAM
IPC分类号： C08F20/44
CPC分类号： C08F20/44 , C08F2/16
摘要： Solutions of acrylonitrile polymers containing at least 80% by weight of acrylonitrile units are prepared by dissolving in an aqueous inorganic thiocyanate solution a polymerizable material containing acrylonitrile in the proportion necessary to give the desired polymer and polymerizing the material in the presence of a free radical forming initiator and a secondary alcohol containing 3 to 5 carbon atoms. The initiator may be an azo compound, e.g. azo-bis-isobutyronitrile. Examples describe the polymerization of solutions of mixtures of acrylonitrile, methyl acrylate and itaconic acid in aqueous sodium thiocyanate solution in the presence of azo-bis-isobutyronitrile and (1 to 3 and 5) isopropyl alcohol and (4) secondary butyl alcohol and secondary amyl alcohol. The solutions may be spun to form fibres.

96. 发明授权

US3208962A Process for the manufacture of acrylonitrile polymer solution 失效
标题翻译：制备丙烯腈聚合物溶液的方法
公开(公告)号：US3208962A
公开(公告)日：1965-09-28
申请号：US7894560
申请日：1960-12-28
申请人： TOHO RAYON KK
发明人： MASAKAZU TANIYAMA , MICHIAKI NAKAJIMA
IPC分类号： C08F20/44
CPC分类号： C08F20/44 , C08F2/16
摘要： Acrylonitrile is polymerized in aqueous solution containing zinc chloride, hydrogen peroxide and from 0,1 to 10 moles of an oxygen acid of chlorine or metal salt thereof per mole of hydrogen peroxide, the total weight of hydrogen peroxide and acid being from 0,1 to 10% by weight of the monomer. The acrylonitrile may be polymerized alone or in admixture with other monomers such as methacrylic acid, amide, nitrile and esters, acrylic acid, amide and esters, e.g. methyl and butyl acrylates, allyl alcohol, vinyl acetate, itaconic acid, vinyl pyridines, N-vinyl-4-beta-hydroxyethyl-imidazole and ethylene and allyl sulphonic acids and salts thereof. Oxygen acids of chlorine specified are hypochlorous, chlorous, chloric and perchloric. In addition to zinc chloride the aqueous solution may contain other salts, e.g. sodium, ammonium, calcium and magnesium chlorides, or organic compounds, e.g. alcohols, ketones or nitriles. The process is preferably carried out by the continuous addition of the reactants to a vessel in such a way that it is occupied only by the reactants.

97. 发明授权

US3193537A Process for the production of acrylonitrile polymers in the presence of a dicarboxylic acid and a metallic ion 失效
标题翻译：在二羧酸和金属离子存在下制备丙烯腈聚合物的方法
公开(公告)号：US3193537A
公开(公告)日：1965-07-06
申请号：US15579961
申请日：1961-11-29
申请人： BAYER AG
发明人： KARL DINGES , HERBERT MARZOLPH
IPC分类号： C08F2/00 , C08F20/44
CPC分类号： C08F20/44 , C08F2/16
摘要： Acrylonitrile is polymerized alone, or together with a copolymerizable monomer in an aqueous medium at pH values of from 2 to 6 with the aid of per-compounds and sulphur compounds of lower oxidation stage, in the presence of (a) 0.1 to 10 millimol of oxalic and/or malonic acid per mol of monomer(s), and (b) 0.5 to 20 p.p.m. of Cu11 ions, and/or 0.1 to 40 p.p.m. of Su11 ions and or 0.2 to 80 p.p.m. of Hg11 ions (based on the quantity of monomer in each case). Comonomers specified for use with acrylonitrile are acrylic and methacrylc esters, e.g. methyl acrylate, vinyl and vinylidene chlorides, vinyl acetate, acrylic and methacrylic acids and amides, styrene, vinyl sulphonic acid and styrene sulphonic acid. Also present during the polymerization may be thioglycol or an aliphatic mercaptan. Monomer and catalyst may be added to the reaction vessel as polymerisation proceeds. The acrylonitrile polymers produced are stated to have good thermostability.

98. 发明授权

US3168546A Organic ammonium sulfite ester compounds and method of preparation 失效
标题翻译：有机亚硫酸铵酯化合物及其制备方法
公开(公告)号：US3168546A
公开(公告)日：1965-02-02
申请号：US7913960
申请日：1960-12-29
申请人： BAYER AG
发明人： ALBERT BALLAUF , WERNER BLANK , DIETRICH GLABISCH , MARTIN WANDEL
IPC分类号： B01F17/00 , C07C301/00 , C08F4/00 , C08F20/44 , C08F36/04 , C08K5/19 , C08K5/41 , C08K5/42 , C09K3/16 , D06M13/248 , D06M13/438
CPC分类号： D06M13/438 , B01F17/0057 , C07C301/00 , C08F2/16 , C08F4/00 , C08F20/44 , C08F36/04 , C08K5/19 , C08K5/41 , C08K5/42 , C09K3/16 , D06M7/00 , D06M13/248 , D06M2200/40 , Y10S260/20 , C08L21/00 , C08F4/28
摘要： The invention comprises organic ammonium compounds of formula: where R1 is a hydrocarbon radical, optionally substituted, R2 and R3 are hydrogen or hydrocarbon radicals, optionally substituted, and R4 is an alkylene radical, optionally substituted, and two of the radicals R1, R2 and R3 may be linked to form a heterocyclic ring. R1, R2 and R3 may be substituted with free, esterified or etherified hydroxyl groups or carbocyclic or heterocyclic radicals, and R4 may be substituted with alkyl, hydroxyalkyl or aryl radicals. The compounds may be prepared by reacting an amine with an epoxide and sulphur dioxide, or with an addition product of ethylene oxide and sulphur dioxide, or by reacting a tertiary amine with a glycol sulphite. The reaction may be carried out with or without an inert solvent, e.g. water, dioxane or methylene chloride. In examples compounds are prepared by reacting ethylene oxide and sulphur dioxide with dodecyldimethylamine, dodecylamine and (HO.CH2.CH2.O.CH2.CH2)3N; by reacting the addition product of ethylene oxide and sulphur dioxide with dodecyldimethylamine, cyclohexyldimethylamine, stearylmethylamine, oleyldiethanolamine, triethylamine and products obtained by reacting ethylene oxide with triethanolamine, dimethylethanolamine and stearylmethylamine; by reacting propylene oxide and sulphur dioxide with stearylmethylamine; and by reacting glycol sulphite with dodecyldimethylamine and triethanolamine. A list of amines suitable for preparing the compounds is given including amines, alkanolamines, ethers of alkanolamines, esters of alkanolamines, 2-(dimethylaminomethylene)-tetrahydrofuran, piperidine, N-methylpiperidine and N-methylmorpholine. Other epoxides mentioned are glycide and styrene oxide.ALSO:Organic ammonium compounds which may be used as the reducing component in the redox system in the polymerization of unsaturated compounds, have the formula: where R1 is a hydrocarbon radical, optionally substituted, R2 and R3 are hydrogen or hydrocarbon radicals, optionally substituted, and R4 is an alkylene radical, optionally substituted, and two of the radicals R1, R2 and R3 may be linked to form a heterocyclic ring. R1, R2 and R3 may be substituted with free, esterified or etherified hydroxyl groups or carbocyclic or heterocyclic radicals, and R4 may be substituted with alkyl, hydroxyalkyl or aryl radicals. In the polymerization of acrylonitrile an aqueous solution of a compound of the above formula is added to a mixture of acrylonitrile, acrylic acid methyl ester, water, sulphuric acid and potassium peroxide disulphate, under nitrogen, and the polymerization carried out at 50 DEG C. with shaking.ALSO:The formation of electrostatic charges on synthetic fibres is prevented by contacting with organic ammonium compounds of formula where R1 is a hydrocarbon radical, optionally substituted, R2 and R3 are hydrogen or hydrocarbon radicals, optionally substituted, and R4 is an alkylene radical, optionally substituted, and two of the radicals R1, R2 and R3 may be linked to form a heterocyclic ring. R1, R2 and R3 may be substituted with free, esterified or etherified hydroxyl groups or carbocyclic or heretocyclic radicals, and R4 may be substituted with alkyl, hydroxyalkyl or aryl radicals. Compounds of the above formula are used to spray and impregnate polyamide fibres, based on e -caprolactam, polyacrylonitrile fibres, polyester fibres and polyvinylchloride fibres.

99. 发明授权

US3154499A Radioactive source comprising a polyamidoxime or a polyhydroxamic acid complexed with a radioactive metal 失效
标题翻译：放射源包括与放射性金属络合的聚偕胺肟或多羟肟酸
公开(公告)号：US3154499A
公开(公告)日：1964-10-27
申请号：US8391161
申请日：1961-01-23
申请人： NOPCO CHEM CO
发明人： FETSCHER CHARLES A
IPC分类号： C08F8/00 , D06M10/00 , G21C3/58 , G21G4/04
CPC分类号： G21G4/04 , C08F8/32 , C08F8/42 , D06M10/008 , G21C3/58 , Y02E30/38 , C08F20/44 , C08F212/08 , C08F265/04

100. 发明授权

US3141869A Process for the production of acrylonitrile polymers 失效
标题翻译：生产丙烯腈聚合物的方法
公开(公告)号：US3141869A
公开(公告)日：1964-07-21
申请号：US5667560
申请日：1960-09-19
申请人： BAYER AG
发明人： INGOFROH DENNSTEDT
IPC分类号： C08F2/22 , C08F4/00 , C08F20/44
CPC分类号： C08F4/00 , C08F2/16 , C08F20/44
摘要： Acrylonitrile is polymerized, alone or together with another copolymerizable monomer, in an aqueous medium at pH values below 7 with the aid of a free-radical forming substance or a redox system in the presence of a colourless or substantially colourless watersoluble aluminium salt and, if necessary, with the addition of heavy metal ions, e.g. those of divalent iron and copper. Also present may be complex formers for heavy metal ions, e.g. ethylene diamine tetraacetic acid, imidotriglycolic acid and alkal metal and ammonium fluorides, pyrophosphates and hexametaphosphates. Comonomers specified are methyl methacrylate, acrylate esters, acrylic acid, styrene, styrene sulphonic acid, vinyl acetate and vinyl and vinylidene chlorides. Catalysts specified are dialkyl and diacyl peroxides, hydrogen peroxide, azodiisobutyronitrile and redox systems based on a persulphate and sulphur compounds of low oxidation stages. Aluminium salts specified are the chloride, sulphate and nitrate and potash alum. The various components of the polymerization system may be added during the course of the reaction. Specification 902,704 is referred to.

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