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1.发明授权Process for the conversion of boron trifluoride dimethyl ether complex to the boron trifluoride dialkyl ether complex 失效三氟化硼二甲醚络合物转化为三氟化硼二烷基醚络合物的方法
公开(公告)号：US4371707A
公开(公告)日：1983-02-01
申请号：US216045
申请日：1980-12-15
IPC分类号： C07F5/02
CPC分类号： C07F5/02
摘要： A process for the conversion of boron trifluoride dimethyl ether complex to boron trifluoride dialkyl ether complex substantially free of dimethyl ether impurities, which comprises reacting the boron trifluoride-dimethyl ether complex, in the liquid phase, in the presence of dialkyl ether wherein at least one of the alkyl groups contains at least two carbon atoms, in a restricted vapor equilibration region, while simultaneously sweeping the said vapor equilibration region with a substantially inert gas, and heating to distill off the dimethyl ether. High purity of the boron trifluoride dialkyl ether complex is attained with this method, with only minimal traces of the boron trifluoride dimethyl ether complex, dimethyl ether remaining. The preferred product is boron trifluoride diethyl ether.
摘要翻译： 一种将三氟化硼二甲醚络合物转化为基本上不含二甲醚杂质的三氟化硼二烷基醚络合物的方法，其包括使三氟化硼 - 二甲醚络合物在液相中在二烷基醚存在下反应，其中至少一种 的烷基在受限的蒸气平衡区域中含有至少两个碳原子，同时用基本上惰性的气体同时吹扫所述蒸气平衡区域，并加热以蒸馏除去二甲醚。 通过该方法可以获得三氟化硼二烷基醚络合物的高纯度，只剩下少量的三氟化硼二甲醚络合物，二甲醚。 优选的产物是三氟化硼二乙醚。
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公开(公告)号：US4227027A
公开(公告)日：1980-10-07
申请号：US96955
申请日：1979-11-23
CPC分类号： C07C2/20 , C07C2/68 , C07C2527/1213 , C07C2531/02 , Y02P20/584
摘要： When saturated with boron trifluoride, certain polyhydric alcohols form adducts which catalyze hydrocarbon alkyl transfer reactions for which boron trifluoride is catalytic. The adduct is recovered from the reaction mixture and recycled, greatly reducing boron and fluoride values in the product and in any effluent. Examples include propylation of toluene in the presence of a recycled adduct of boron trifluoride with mannitol or sorbitol, and the oligomerization of decene by a recycled adduct of boron trifluoride with mannitol or butanediol. Some of the catalysts become viscous on cooling and are thus more easily separated from the reaction products which remain in a separate liquid phase.
摘要翻译： 当三氟化硼饱和时，某些多元醇形成催化三氟化硼催化的烃烷基转移反应的加合物。 加合物从反应混合物中回收并循环使用，大大降低了产品和任何流出物中的硼和氟化物值。 实例包括在三氟化硼与甘露糖醇或山梨糖醇的再循环加合物存在下甲苯的丙基化，以及通过三氟化硼与甘露糖醇或丁二醇的再循环加合物使癸烯低聚。 一些催化剂在冷却时变得粘稠，因此更容易与保留在单独的液相中的反应产物分离。
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公开(公告)号：US4265871A
公开(公告)日：1981-05-05
申请号：US36464
申请日：1979-05-07
CPC分类号： C01B17/90
摘要： Sulfuric acid contaminated with boron and fluoride values such as the waste acid of a boron trifluoride process is purified by contacting the contaminated acid with an inert gas to desorb boron trifluoride, and the inert gas is stripped by contacting with an absorbing liquid including concentrated sulfuric acid. Fluosulfonic acid is added to contaminated sulfuric acid at levels approximately three times the molar values of boric acid contaminant as an agent to spring non-volatile boron values. The absorption of boron trifluoride into the absorbing sulfuric acid is improved when it contains boric acid. Preferably the contaminated sulfuric acid to be purified is one portion of the waste liquid and the absorbing liquid is another portion of the waste liquid of a boron trifluoride manufacturing process. Boric acid is added to the absorbing liquid, then boron trifluoride is stripped from the inert gas and absorbed into the absorbing liquid. The absorbing liquid along with stripped boron trifluoride is recycled to a boron trifluoride manufacturing process. The inert gas can be recycled to the desorbing step.
摘要翻译： 用硼污染的硫酸和三氟化硼处理的废酸等氟化物值通过使被污染的酸与惰性气体接触以解吸三氟化硼来净化，并且通过与包含浓硫酸的吸收液体接触来汽提惰性气体 。 将氟磺酸加入到污染硫酸中，其水平为硼酸污染物的摩尔值的三倍，作为弹性非挥发性硼值的试剂。 当含有硼酸时，三氟化硼在吸收硫酸中的吸收得到改善。 优选地，被净化的污染硫酸是废液的一部分，吸收液是三氟化硼制造方法的废液的另一部分。 将硼酸加入到吸收液中，然后从惰性气体中汽提三氟化硼并吸收到吸收液中。 将吸收液与汽提的三氟化硼一起再循环至三氟化硼制造方法。 惰性气体可以再循环到解吸步骤。
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公开(公告)号：US4209654A
公开(公告)日：1980-06-24
申请号：US951911
申请日：1978-10-16
IPC分类号： C07C2/32 , B01J27/12 , B01J31/22 , B01J31/26 , C07B61/00 , C07C1/00 , C07C2/20 , C07C2/22 , C07C2/68 , C07C11/02 , C07C67/00 , C07C3/56 , C07C3/18
CPC分类号： B01J31/2226 , B01J27/12 , C07C2/20 , C07C2/68 , B01J2231/4205 , B01J2531/30 , B01J31/0201 , B01J31/26 , C07C2527/1213 , C07C2531/02 , Y02P20/584
摘要： When saturated with boron trifluoride, certain polyhydric alcohols form adducts which catalyze reactions for which boron trifluoride is catalytic. The adduct is recovered from the reaction mixture and recycled, greatly reducing boron and fluoride values in the product and in any effluent. Examples include propylation of toluene in the presence of a recycled adduct of boron trifluoride with mannitol or sorbitol.
摘要翻译： 当三氟化硼饱和时，某些多元醇形成催化三氟化硼催化反应的加合物。 加合物从反应混合物中回收并循环使用，大大降低了产品和任何流出物中的硼和氟化物值。 实例包括在三氟化硼与甘露糖醇或山梨糖醇的再循环加合物存在下丙烯化甲苯。
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公开(公告)号：US4157377A
公开(公告)日：1979-06-05
申请号：US939576
申请日：1978-09-05
CPC分类号： C01B35/063
摘要： Dry calcium fluoborate suitable for use in the manufacture of boron trifluoride is produced by reacting, in an aqueous medium, calcium fluoride, hydrofluoric acid and boric acid followed by removing water from the calcium fluoborate reaction product by purging the reaction product with a dry inert gas such as nitrogen, at a temperature between about 140.degree. to 160.degree. C.
摘要翻译： {PG，1，适用于制造三氟化硼的干燥的氟硼酸钙是通过在水性介质中使氟化钙，氢氟酸和硼酸反应，然后通过用氟化氢反应产物除去水， 干燥的惰性气体如氮气，在约140（20 {0至160 {20 {℃）
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公开(公告)号：US4174349A
公开(公告)日：1979-11-13
申请号：US955679
申请日：1978-10-30
IPC分类号： C07B39/00 , C07B31/00 , C07C17/20 , C07C45/63 , C07C51/58 , C07C67/00 , C07C17/10 , C07C17/12 , C07C17/14
CPC分类号： C07C45/63 , C07C17/208 , C07C51/58
摘要： Fluoroorganic compounds are prepared by reacting a haloorganic starting material in which at least one halo atom is replaceable with a fluorine atom by metathetical exchange, with calcium fluoride in the presence of a crown ether and an anhydrous, polar, basic organic solvent which complexes with the calcium ion and contains no --OH groups, at a temperature and for a period of time adequate to effect fluorination.
摘要翻译： 通过在冠醚和无水极性的碱性有机溶剂的存在下，通过使其中至少一个卤原子可与氟原子进行元间交换的氟代氟化物与氟化钙反应来制备氟有机化合物，该有机溶剂与 钙离子，并且在温度和时间足以实现氟化时不含-OH基团。
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公开(公告)号：US4072027A
公开(公告)日：1978-02-07
申请号：US760489
申请日：1977-01-19
摘要： A stabilized heat exchange medium is disclosed including a fluorocarbon, an absorbant and a tribasic phosphite stabilizer. The preferred absorbants are assymetrical furan derivatives containing at least 1 oxygen with a single bond to an adjacent carbon, and is most preferably an alkyl tetrahydrofurfuryl ether. The fluorocarbon contains 1 or 2 carbons, 1 or 2 hydrogens and the remainder chlorine and fluorine. The tribasic phosphites are of the formula (R.sub.1 'O)(R.sub.2 'O)(R.sub.3 'O)P, wherein R.sub.1 ', R.sub.2 ' and R.sub.3 ' are each independently alkyl, alkenyl, phenyl, alkylene phenyl, alkylene alkylphenyl or alkylphenyl.
摘要翻译： 公开了一种稳定的热交换介质，包括碳氟化合物，吸收剂和亚磷酸三酯稳定剂。 优选的吸收剂是含有至少1个氧，与相邻碳具有单键的对称呋喃衍生物，最优选烷基四氢糠基醚。 氟碳含有1或2个碳，1或2个氢，其余为氯和氟。 亚磷酸三亚酯具有式（R1'O）（R2'O）（R3'O）P，其中R1'，R2'和R3'各自独立地为烷基，烯基，苯基，亚烷基苯基，亚烷基烷基苯基或烷基苯基。
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公开(公告)号：US4375453A
公开(公告)日：1983-03-01
申请号：US334719
申请日：1981-12-28
CPC分类号： C01F17/0081 , C01F17/0012 , C01F17/0043 , C01G15/00 , C01P2004/61 , C01P2006/80
摘要： Gd.sub.2 O.sub.3 and Ga.sub.2 O.sub.3 are currently used for the fabrication of Gd.sub.3 Ga.sub.5 O.sub.12 (GGG) wafers which are employed as substrates for bubble domain memory devices. In the processing, in the order of 25% of the starting material ends up as process "saw kerf" contaminated with variable amounts of iron, nickel, magnesium, aluminum, zirconium, iridium and silicon. A process is described whereby the "saw kerf" can be reprocessed in sufficient purity to be re-used in the process, thereby improving the economics of production of GGG wafers significantly. Gadolinium and gallium oxides are recovered and separated from transition metal impurities introduced during fabrication of GGG wafers. The process "saw kerf" produced from slicing the crystal boule is dissolved in HCl, treated with H.sub.2 SO.sub.4, and the resulting sulfates separated. Metathesis with (NH.sub.4).sub.2 C.sub.2 O.sub.4 results in conversion of the sulfates to the ammonium oxalates which were calcined at 850.degree. C. to form Ga.sub.2 O.sub.3 and Gd.sub.2 O.sub.3 of purity >99.99%. The process can be extended to include purification and re-use of by-products generated in other grinding and polishing operations which may result in the recycling of the order of 80% of the generated by-products.
摘要翻译： Gd2O3和Ga2O3目前用于制造用作气泡域记忆装置底物的Gd 3 Ga 5 O 12（GGG）晶片。 在加工过程中，以可变量的铁，镍，镁，铝，锆，铱和硅污染的工艺“锯切”为起始原料的25％。 描述了一种方法，其中“锯切”可以以足够的纯度重新加工以在该过程中重新使用，从而显着提高了GGG晶片的生产经济性。 钆和镓氧化物被回收并与制造GGG晶片期间引入的过渡金属杂质分离。 将从晶体棒上切下的方法“锯切”溶解在HCl中，用H 2 SO 4处理，所得到的硫酸盐分离。 （NH 4）2 C 2 O 4的复分解导致硫酸盐转化成草酸铵，其在850℃下煅烧以形成纯度> 99.99％的Ga 2 O 3和Gd 2 O 3。 该方法可以扩展到包括在其它研磨和抛光操作中产生的副产物的纯化和再利用，这可能导致生成的副产物的80％的量级的再循环。
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公开(公告)号：US4337361A
公开(公告)日：1982-06-29
申请号：US238920
申请日：1981-02-27
IPC分类号： C07C49/167 , B01J27/00 , B01J27/12 , C07B61/00 , C07C45/00 , C07C45/27 , C07C45/32 , C07C45/56 , C07C67/00
CPC分类号： C07C45/567
摘要： A process for the preparation of hexafluoroacetone which comprises contacting, in the liquid phase, hexafluorothioacetone dimer in the presence of an aprotic solvent containing a catalytic amount of an alkali metal fluoride with a gaseous oxidant selected from the group consisting of air, O.sub.2, O.sub.3, NO.sub.2 and NO is disclosed. The preferred aprotic solvent is dimethylformamide, and the preferred gaseous oxidant is O.sub.2.
摘要翻译： 一种制备六氟丙酮的方法，该方法包括在含有催化量的碱金属氟化物的非质子溶剂存在下，在液相中与六氟硫代丙酮二聚物与选自空气，O 2，O 3， 公开了NO2和NO。 优选的非质子溶剂是二甲基甲酰胺，优选的气态氧化剂是O 2。
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10.发明授权
公开(公告)号：US4411843A
公开(公告)日：1983-10-25
申请号：US372576
申请日：1982-04-29
IPC分类号： C07C17/278 , C07C51/58
CPC分类号： C07C17/278 , C07C51/58
摘要： A process for the preparation of perhaloalkanoyl chloride is disclosed which comprises reacting 1,1,1-trichloroperfluoroalkane, with a sulfur trioxide-containing compound selected from the group consisting of oleum sulfur trioxide and stabilized sulfur trioxide in the presence of catalytic amounts of a halogen catalyst selected from the group consisting of iodine, bromine, iodine monobromide and iodine monochloride and bromine monochloride wherein the 1,1,1-trichloroperhaloalkane is a straight or branched chain acyclic organic compound having 2 to 8 carbon atoms and having at least one trihalomethyl group wherein at least one halo atom is fluorine and having the remaining carbon atoms substituted by F, Cl, Br or I atoms.
摘要翻译： 公开了一种制备全卤烷酰氯的方法，其包括在催化量的卤素存在下使1,1,1-三氯全氟烷烃与选自三氧化硫烟和硫酸三氧化硫的三氧化硫的化合物反应 选自碘，溴，一碘化碘和一氯化碘和一氯化氯的催化剂，其中1,1,1-三氯环烷烃是具有2-8个碳原子并具有至少一个三卤代甲基的直链或支链无环有机化合物 其中至少一个卤原子是氟并且其余的碳原子被F，Cl，Br或I原子取代。
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