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    • 13. 发明授权
    • Method for producing silane
    • 硅烷的制造方法
    • US06852301B2
    • 2005-02-08
    • US10450207
    • 2001-11-21
    • Hans-Dieter BlockLeslaw MleczkoAndreas BulanRainer WeberSigurd BuchholzTorsten Sill
    • Hans-Dieter BlockLeslaw MleczkoAndreas BulanRainer WeberSigurd BuchholzTorsten Sill
    • C01B33/04C01B33/18
    • C01B33/046C01B33/043C01B33/18
    • The invention relates to a method for producing silane (SiH4) by a) reacting metallurgical silicon with silicon tetrachloride (SiCl4) and hydrogen (H2), to form a crude gas stream containing trichlorosilane (SiHCl3) and silicon tetrachloride (SiCl4), b) removing impurities from the resulting crude gas stream by washing with condensed chlorosilanes, c) condensing and subsequently, separating the purified crude gas stream by distillation, d) returning the partial stream consisting essentially of SiCl4 to the reaction of metallurgical silicon with SiCl4 and H2, e) disproportionating the partial stream containing SiHCl3, to form SiCl4 and SiH4 and f) returning the SiH4 formed by disproportionation to the reaction of metallurgical silicon with SiCl4 and H2, the crude gas stream containing trichlorosilane and silicon tetrachloride being liberated from solids as far as possible by gas filtration before being washed with the condensed chlorosilanes. The washing process with the condensed chlorosilanes is carried out at a pressure of 25 to 40 bar and at a temperature of at least 150° C. in a single-stage distillation column and is carried out in such a way that 0.1 to 3 wt. % of the crude gas stream containing trichlorosilane and silicon tetrachloride is recovered in the form of a condensed liquid phase consisting essentially of SiCl4, this liquid phase then being removed from the SiCl4 circuit and expanded to a pressure of 1 bar outside said SiCl4 circuit and cooled to a temperature of 10 to 40° C., whereby dissolved impurities separate out and are then removed by filtration.
    • 本发明涉及一种通过以下步骤制备硅烷(SiH 4)的方法:a)使冶金硅与四氯化硅(SiCl 4)和氢(H 2)反应,形成含有三氯硅烷(SiHCl 3)和四氯化硅(SiCl 4)的粗气流,b) 通过用冷凝的氯硅烷洗涤从所得粗气流中除去杂质,c)冷凝并随后通过蒸馏分离纯化的粗气流,d)将基本上由SiCl 4组成的部分流返回到冶金硅与SiCl 4和H 2的反应中, e)歧化含SiHCl3的部分流,以形成SiCl4和SiH4,以及f)将通过歧化形成的SiH 4返回至冶金硅与SiCl4和H2的反应,将含有三氯硅烷和四氯化硅的粗气流从固体释放至 在用冷凝的氯硅烷洗涤之前可能通过气体过滤。 冷凝氯硅烷的洗涤过程在单级蒸馏塔中在25至40巴的压力和至少150℃的温度下进行,并以0.1至3重量% 含有三氯硅烷和四氯化硅的粗气流的%以基本上由SiCl 4组成的冷凝液相的形式回收,然后将该液相从SiCl4回路除去并在SiCl 4回路外扩张至1巴的压力,并冷却 温度为10〜40℃,由此分离出溶解的杂质,然后通过过滤除去。
    • 16. 发明授权
    • Process for the preparation of chromic acid
    • 制备色素的方法
    • US5096548A
    • 1992-03-17
    • US626076
    • 1990-12-11
    • Norbert LonhoffLudwig SchmidtHans-Dieter BlockRainer Weber
    • Norbert LonhoffLudwig SchmidtHans-Dieter BlockRainer Weber
    • C25B1/00B01J47/12C01G37/033C25B1/22C25B15/08C25C1/10
    • C01G37/033C25B1/22C25C1/10
    • A process for the production of chromic acid, comprising(a) dissolving ferrochrome in sulphuric acid and mother liquor from the subsequent crystallization of ammonium chrome alum, optionally with the addition of at least one of catholyte and anolyte overflow from the subsequent electrolysis,(b) removing undissolved constituents by filtration,(c) removing dissolved iron by the addition of at least one of ammonia and ammonium sulphate to the filtrate obtained, crystallizing iron ammonium sulphate and filtering,(d) crystallizing and filtering ammonium chrome alum from the remaining solution and returning the filtrate for dissolving ferrochrome in step (a),(e) dissolving the ammonium chrome alum in water,(f) precipitating and separating chromium-(III) hydroxide from the resulting solution by adding a base, optionally under reducing conditions,(g) dissolving the separated chromium hydroxide in chromic acid and optionally sulphuric acid so that either a single solution in chromic acid is obtained or two solutions are obtained, one in chromic acid and another in sulphuric acid,(h) separating the solution(s) from undissolved constituents, and(i) utilizing the solution of chromium hydroxide in chromic acid as anolyte in the electrolytic production of chromic acid in an electrolytic cell divided by a membrane, and either utilizing the same solution as catholyte in the above mentioned electrolytic cell divided by a membrane or utilizing the solution of chromium hydroxide in sulphuric acid as catholyte in the above mentioned electrolytic cell divided by a membrane, hydrogen and metallic chromium being deposited electrolytically at the cathode and/or chromium (II) ions being produced electrolytically at the cathode.
    • 一种生产铬酸的方法,包括(a)将铬铁铬酸盐和母液从随后的铵铬明矾结晶中溶解,任选地从随后的电解中加入至少一种阴极电解液和阳极电解液溢出物(b )通过过滤除去未溶解的组分,(c)通过向所得滤液中加入至少一种氨和硫酸铵除去溶解的铁,结晶硫酸铁铵并过滤,(d)从剩余溶液中结晶并过滤铵铬明矾 并在步骤(a)中返回用于溶解铬铁的滤液,(e)将铵铬明矾溶解在水中,(f)通过加入碱(任选在还原条件下)将所得溶液中的铬 - (III) (g)将分离的氢氧化铬溶解在铬酸和任选的硫酸中,使得单一的铬酸溶液 得到两种溶液,一种在铬酸中,另一种在硫酸中,(h)将溶液与未溶解的组分分离,和(i)在电解生产中利用铬酸中的铬酸溶液作为阳极电解液 在由电解槽中分离的膜中的铬酸,或者利用与上述电解槽中的阴极电解液相同的溶液,或者利用氢氧化铬溶液作为阴极电解液,除去上述电解槽 在阴极处电解沉积的阴极和/或铬(II)离子沉积的膜,氢和金属铬。
    • 20. 发明授权
    • Preparation of alkane phosphonic and phosphinic acid aryl esters
    • 烷烃膦酸和次膦酸芳酯的制备
    • US4377537A
    • 1983-03-22
    • US222221
    • 1981-01-02
    • Hans-Dieter BlockHans-Gunther Frohlen
    • Hans-Dieter BlockHans-Gunther Frohlen
    • B01J21/00C07F9/32C07F9/38C07F9/40
    • C07F9/4084C07F9/3282
    • A process for the preparation of an alkane phosphonic acid diaryl ester or an alkane phosphinic acid aryl ester of the formula ##STR1## wherein R.sup.1 is C.sub.1 -C.sub.20 alkyl or alkenyl group,R.sup.2 is a C.sub.1 -C.sub.20 alkyl or alkenyl group or a C.sub.6 -C.sub.10 aryl or aryloxy group,R.sup.3 is C.sub.6 -C.sub.10 aryl group,k is 0 or 1,p is 1 or 2,k+p=2,plus an alkane phosphonic acid diaryl ester, alkane phosphinic acid aryl ester or phosphine oxide of the formula ##STR2## R.sup.4 and R.sup.5 each independently is C.sub.1 -C.sub.20 alkyl group, a C.sub.6 -C.sub.10 aryl group or a C.sub.6 -C.sub.10 aryloxy group,R.sup.6 is C.sub.1 -C.sub.20 alkyl or alkenyl group,n and m each is 0, 1 or 2, andn+m=2,comprising reacting an aryloxy compound of trivalent phosphorus of the formula ##STR3## (a) with an alkyl phosphite or alkyl phosphonite of the formula ##STR4## in the presence of an Arbusow catalyst, or (b) a rearrangement product formed in the presence of an Arbusow catalyst and of the formula ##STR5##
    • 制备下式的烷烃膦酸二芳基酯或烷烃次膦酸芳基酯的方法,其中R 1是C 1 -C 20烷基或烯基,R 2是C 1 -C 20烷基或链烯基或C 6 -C 20烷基, C10芳基或芳氧基,R3为C6-C10芳基,k为0或1,p为1或2,k + p = 2,加上烷烃膦酸二芳基酯,烷烃次膦酸芳酯或氧化膦 其中R4和R5各自独立地为C1-C20烷基,C6-C10芳基或C6-C10芳氧基,R6是C1-C20烷基或烯基,n和m各自为0 ,1或2和n + m = 2,包括在Arbusow催化剂的存在下使式(a)的三价磷的芳氧基化合物与式IMAMA的烷基亚磷酸酯或烷基亚膦酸酯反应, 或(b)在Arbusow催化剂存在下形成并具有式(IMAGE)的重排产物