![]() Method of separating hydrogen fluoride and trifluoride of boron from their complex and orthobenzoylb
专利摘要:
The invention relates to chemical chemistry, namely to the method of hydrogen fluoride and three-. boron fluoride from their complex with orthobenzoylbenzoic acid. In order to increase the yield of the products, the orthobenzoylbenzoic acid complex with hydrogen fluoride and boron trifluoride boron is subjected to distillation at 40-85 ° C in the presence of methylene chloride or 1,2-dichloroethane. 00 with so youh vj 公开号:SU1333227A3 申请号:SU833638955 申请日:1983-08-30 公开日:1987-08-23 发明作者:Девик Мишель 申请人:Продюи Шимик Южин Кюльман (Фирма); IPC主号:
专利说明:
one This invention relates to chemical technology, in particular to the selection of hydrogen fluoride and boron trifluoride from complexes with orthobenzoyl benzoic acid (OBB-acid). The purpose of the invention is to increase the yield of hydrogen fluoride and boron trifluoride. Note 1. 1 mol of phthalic anhydride to L mol of benzene is mixed with 10 mol of hydrogen fluoride and 10 mol of boron trifluoride. After partial degassing of boron trifluoride at 40 C, a solution of the complex OBV-acid is obtained, containing 203.3 g of OBB-acid, 306.7 BF, 200 g of HF and 22.7 g of impurities. Distillation is carried out in a stainless steel column with an internal diameter of 38 nm containing a packing. The temperature in the column is 41 C, the pressure is atmospheric. First, within 28 minutes, 110 g of a solution of the complex of O.BB-acid are supplied, then reflux of methylene chloride is supplied for 20 minutes. Gaseous HF and BF are collected in the annual part of the column. 0.5 g of sediment containing 0.24 g of BF hydrate and 0.2 g of N are collected in a decanter installed in the head of the column. Editor V.Danko Order 3853/58 Compiled by V. Grodzovska Tehred L. Serdyukova Proofreader I. Musk Circulation 455 Subscription VNIIPI USSR State Committee for Inventions and Discoveries 4/5, Moscow, Zh-35, Raushsk nab. 113035 Production and printing company, Uzhgorod, Project St., 4,. BF, 33.3 g of OBB-acid containing 28.6 g of the basic substance, 0.43 g of BF, and 0.1 g of HF are obtained by distillation. . Yield,%: acid 93,8j HF-99,6; 99.0. Example 2. The process is carried out at 8 Jt ° C according to Example 1, however, 1,2-dichloroethane is used as the halogen-containing aliphatic hydrocarbon. The evaporation rate of 1,2-dichloroethane is 4.22 kg / h. 110 g of the solution of the OBB-acid complex and then the phlegm G, 2-dichloroethane are introduced over 22 mi. The evaporation rate of 1,2-dichloroethane is 4.22 kg / h. Obtain 32 g of OBB-acid containing 28.0 g of the basic substance, 0.33 T BF and 0.1 g of HF. Yield,%: OBB-acid 92-, BF - 99.3; HF - 99.6. Formula of invention The method of separation of hydrogen fluoride and boron trifluoride from their complex with orthobenzoylbenzoic acid by distillation at 40-85 ° C, characterized in that, in order to increase the yield of products, the distillation is carried out in the presence of methylene chloride or 1,2-dichloroethane.
权利要求:
Claims (1) [1] Claim The method of separation of hydrogen fluoride and boron trifluoride from their complex with orthobenzoylbenzoic acid by distillation at 40-85 ° C, characterized in that, in order to increase the yield of products, distillation is carried out in the presence of methylene chloride or 1,2-dichloroethane.
类似技术:
公开号 | 公开日 | 专利标题 US2739174A|1956-03-20|Nitrating aromatic hydrocarbons with only nitric acid Portis et al.1970|Electrochemical dealkylation of aliphatic tertiary and secondary amines SU1333227A3|1987-08-23|Method of separating hydrogen fluoride and trifluoride of boron from their complex and orthobenzoylbenzoic acid US10214485B2|2019-02-26|Method of reprocessing alkanesulfonic acid US3510527A|1970-05-05|Preparation of p-nitrophenols US5387713A|1995-02-07|Process for purification of carboxylic acids Lepori et al.1983|Discriminating interactions between chiral molecules in the liquid phase: effect on volumetric properties US3637832A|1972-01-25|Preparation of straight chain dicarboxylic acids US2915558A|1959-12-01|Process for the separation of diisopropylbenzene dihydroperoxides EP0002598B1|1981-07-22|Process for the purification of alkane dicarboxylic acids having at least 4 carbon atoms US3376203A|1968-04-02|Purification of dialkyl sulfoxides by treatment with adsorptive carbon US3996029A|1976-12-07|Purification of gases containing hydrogen fluoride impurity US3284494A|1966-11-08|Process for producing alpha hydroxyisobutyric acid US2590096A|1952-03-25|Purification of phenanthrene by azeotropic distillation US2349518A|1944-05-23|Purification of phthalic anhydride US2204476A|1940-06-11|Production of hyposulphites US4743707A|1988-05-10|Process for purifying allyl alcohol US3329598A|1967-07-04|Photochemical methods for making sulfopivalic acid anhydride Erickson et al.1958|Chloroacetyl chloride from ketene and chlorine SU1298188A1|1987-03-23|Method for producing nitrogen oxide US2889365A|1959-06-02|Process for producing monochloroacetyl chloride by chlorinating ketene in sulfur dioxide US3347918A|1967-10-17|Production of cyclododecylamine SU1310395A1|1987-05-15|Method for isolating and purifying raw quinoline bases from sulfates of bases of naphthalene and absorption fractions of coal tar RU2041188C1|1995-08-09|Liquid-phase method of methyl chloride synthesis US2316737A|1943-04-13|Process for production of carbon tetrachloride
同族专利:
公开号 | 公开日 JPS5964503A|1984-04-12| EP0102297A3|1984-04-11| PL243563A1|1984-07-30| DE3361073D1|1985-11-28| DE102297T1|1985-02-28| FI77016B|1988-09-30| CS236891B2|1985-05-15| FI77016C|1989-01-10| EP0102297B1|1985-10-23| CA1198736A|1985-12-31| ES525273A0|1984-05-16| FR2532303B1|1985-01-25| US4496760A|1985-01-29| ES8404970A1|1984-05-16| FI833098A|1984-03-02| FR2532303A1|1984-03-02| KR840006006A|1984-11-21| JPS6313977B2|1988-03-29| KR860002163B1|1986-12-22| FI833098A0|1983-08-31| EP0102297A2|1984-03-07| IN158050B|1986-08-23|
引用文献:
公开号 | 申请日 | 公开日 | 申请人 | 专利标题 CA526912A|1956-06-26|Graff-Baker Carey|Recovery of fluorides from tolualdehyde-fluorides compositions| GB486886A|1935-12-13|1938-06-13|Du Pont|Improvements in or relating to the separation of the constituents of organic-inorganic addition compounds| FR814838A|1935-12-13|1937-06-30|Du Pont|Distillation process under different pressures| US2174118A|1936-09-30|1939-09-26|Du Pont|Ring closure of aromatic compounds with the aid of hydrofluoric acid| GB501670A|1936-11-21|1939-03-03|Standard Oil Dev Co|Improvements relating to the recovery of condensing agents| US2386798A|1942-10-31|1945-10-16|Standard Oil Co|Recovery of catalysts| GB605472A|1945-10-02|1948-07-23|Standard Oil Co|Improvements relating to the recovery of fluorides| US2468681A|1948-03-09|1949-04-26|Robert H Mcbride|Purification of hydrogen fluoride| US2534017A|1948-04-23|1950-12-12|Du Pont|Catalyst recovery process| US3108131A|1959-10-16|1963-10-22|Du Pont|Polyfluoroalkyl esters of certain ortho-substituted benzoic acids| US3110724A|1961-04-12|1963-11-12|Atlantic Refining Co|Polyoxyesters of benzoylbenzoic acid| US3745093A|1970-07-17|1973-07-10|Du Pont|Process for separating hexafluoroacetone from hydrogen fluoride| JPS533376B2|1974-12-27|1978-02-06| US4318854A|1979-02-07|1982-03-09|Hoffmann-La Roche Inc.|Intermediates in the production of 2-benzazepines| FR2496097B1|1980-12-16|1982-12-17|Ugine Kuhlmann|FR2543544B1|1983-03-30|1986-01-17|Ugine Kuhlmann|PROCESS FOR DECOMPOSING AN ORTHOBENZOYL-BENZOIC ACID COMPLEX, HYDROGEN FLUORIDE AND BORON TRIFLUORIDE| US4886581A|1986-07-03|1989-12-12|Daikin Industries Ltd.|Removal of hydrogen fluoride from 2,2,3,3-tetra-fluorooxetane| JP2569760B2|1988-09-30|1997-01-08|三菱瓦斯化学株式会社|Method for decomposing aromatic acylated product / HF-BF3 complex| US5041571A|1990-03-29|1991-08-20|Hoechst Celanese Corporation|Process of producing anthraquinones in one step| FR2731705B1|1995-03-15|1997-04-30|Atochem Elf Sa|2-ETHYL-ANTHRAQUINONE SYNTHESIS PROCESS| KR100476116B1|1997-06-13|2005-07-07|주식회사 삼양사|Ultra high purity benzoic acid recovery method using halogen-based organic solvent| CN103524323B|2013-10-17|2015-04-22|扬州大学|Method for catalytically synthesizing o-benzoylbenzoic acid by virtue of metal oxide supported solid superacid|
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申请号 | 申请日 | 专利标题 FR8214920A|FR2532303B1|1982-09-01|1982-09-01| 相关专利
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