公开(公告)号：CA1055877A

公开(公告)日：1979-06-05

申请号：CA256929

申请日：1976-07-14

Applicant: HOECHST AG

Inventor： GEHRMANN KLAUS ,  OHORODNIK ALEXANDER ,  LOHMAR ELMAR ,  RIECHMANN WERNFRIED

IPC: C07F9/32 ,  C07F9/34 ,  C07F9/6571 ,  C07F9/6574 ,  B01D3/10

Abstract: 2,5 dioxo-1-oxa-2-phospholanes of the general formula: in which R1 stands for a n alkyl radical having form 1 to 4 carbon atoms, or a phenyl radical, and R2 and R3 each stand for hydrogen or CH3, are distillativelypurified. To this end the respective crude compound is preheated to 120 to 160.degree.C and fed to the head of a distilling column provided with a plurality of individually heatable trays maintained at temperatures increasing from the upper-most tray to the lowermost, the uppermost tray in the column being maintained at 160 to 200.degree.C, the pressure at the head of the column being 20 to 200 mm Hg, preferably 50 to 120 mm Hg; an inert gas preheated at 160 to 200.degree.C is introduced countercurrently at the base of the column; those impurities having a boiling point lower than that of the respective 2,5-dioxo-1-oxa-2-phospholane are withdrawn overhead together with the inert gas; the 2,5-dioxo-1-oxa-2-phospholane thus freed from low-boiling impurities is withdrawn from the base of the distilling column and passed to a film evaporator; and the 2,5-dioxo-1-oxa-2-phospholane is distilled off from higher-boiling impurities in the film evaporator under a pressure of 0.1 to 5 mm Hg.

公开(公告)号：CH630093A5

公开(公告)日：1982-05-28

申请号：CH860177

申请日：1977-07-12

Applicant: HOECHST AG

Inventor： SCHAEFER STEFAN ,  GEHRMANN KLAUS DR ,  OHORODNIK ALEXANDER DR ,  STEIL KARL-HEINZ ,  RIECHMANN WERNFRIED ,  BYLSMA FRIEDHELM

IPC: C07F9/42 ,  C07F9/48 ,  C07F9/52

公开(公告)号：CH604800A5

公开(公告)日：1978-09-15

申请号：CH513776

申请日：1976-04-23

Applicant: HOECHST AG

Inventor： KUXDORF BERNHARD ,  PUESCHE HERBERT ,  ERPENBACH HEINZ DR ,  RIECHMANN WERNFRIED

IPC: B01D3/16 ,  B01D3/20 ,  B01D3/32

公开(公告)号：CA1087206A

公开(公告)日：1980-10-07

申请号：CA282646

申请日：1977-07-13

Applicant: HOECHST AG

Inventor： SCHAEFER STEFAN ,  GEHRMANN KLAUS ,  OHORODNIK ALEXANDER ,  STEIL KARL-HEINZ ,  RIECHMANN WERNFRIED ,  BYLSMA FRIEDHELM

IPC: C07F9/42 ,  C07F9/48 ,  C07F9/52 ,  C07F9/28

Abstract: PRODUCTION OF METHYLDICHLOROPHOSPHANE Production of methyldichlorophosphane. The compound is made by reacting methane and phosphorus trichloride in a reaction zone in which a temperature higher than 500.degree.C is maintained. More specifically, hot reaction gas coming from the reaction zone is mechanically freed from solid matter, and the reaction gas freed from solid matter is passed to a quenching zone in which it is quenched with liquefied reaction mixture having 0.3 to 5 weight% of an organic barium compound or a non-ionic surfactant dissolved therein.

公开(公告)号：DE2631608B1

公开(公告)日：1978-01-26

申请号：DE2631608

申请日：1976-07-14

Applicant: HOECHST AG

Inventor： SCHAEFER STEFAN ,  GEHRMANN KLAUS DIPL-CHEM DR ,  OHORODNIK ALEXANDER DIPL-CHEM ,  STEIL KARL-HEINZ ,  RIECHMANN WERNFRIED ,  BYLSMA FRIEDHELM

IPC: C07F9/52

Abstract: Pren. of methyldichlorophosphine by reaction of CH4 and PCl3 at >500 degrees C with mechanical sepn. of solid material from the hot reaction gas issuing from the reaction zone and rapidly cooling by means of liq. reaction mixt. contg. in the dissolved state, 0.3-5 wt.% of an organic Ba cpd., or a non-ionic surfactant. Pref. the appts. used comprises a preheating zone, a solid sepn. zone, a main heating zone, a second solid sepn. zone and a rapid cooling zone, the two sepn. zones being outside the electrically heated reaction zones. CH3PCl2 is useful in flame-proofing fibres and plastics materials. The present process seeks to prevent deposition of solid decompsn. prods. from CH3PCl2 in the reactors and allow economic recycling of unreacted starting materials which may form 80% of the amts. used.

公开(公告)号：DE2531920B1

公开(公告)日：1976-10-21

申请号：DE2531920

申请日：1975-07-17

Applicant: HOECHST AG

Inventor： GEHRMANN KLAUS DIPL-CHEM DR ,  OHORODNIK ALEXANDER DIPL-CHEM ,  LOHMAR ELMAR DIPL-CHEM DR ,  RIECHMANN WERNFRIED

IPC: C07F9/32 ,  C07F9/34 ,  C07F9/6571 ,  C07F9/6574 ,  C07F9/30

Abstract: 2,5 DIOXO-1-OXA-2-PHOSPHOLANES OF THE GENERAL FORMULA: in which R1 stands for an alkyl radical having from 1 to 4 carbon atoms, or a phenyl radical, and R2 and R3 each stand for hydrogen or CH3, are distillatively purified. To this end the respective crude compound is preheated to 120 DEG to 160 DEG C and fed to the head of a distilling column provided with a plurality of individually heatable trays maintained at temperatures increasing from the upper-most tray to the lowermost, the uppermost tray in the column being maintained at 120 DEG to 160 DEG C and the lowermost tray being maintained at 160 DEG to 200 DEG C, the pressure at the head of the column being 20 to 200 mm Hg, preferably 50 to 120 mm Hg; an inert gas preheated to 160 DEG to 200 DEG C is introduced countercurrently at the base of the column; those impurities having a boiling point lower than that of the respective 2,5-dioxo-1-oxa-2-phospholane are withdrawn overhead together with the inert gas; the 2,5-dioxo-1-oxa-2-phospholane thus freed from low-boiling impurities is withdrawn from the base of the distilling column and passed to a film evaporator; and the 2,5-dioxo-1-oxa-2-phospholane is distilled off from higher-boiling impurities in the film evaporator under a pressure of 0.1 to 5 mm Hg.

公开(公告)号：DE2718391B1

公开(公告)日：1978-08-24

申请号：DE2718391

申请日：1977-04-26

Applicant: HOECHST AG

Inventor： OHORODNIK ALEXANDER DIPL-CHEM ,  GEHRMANN KLAUS DIPL-CHEM DR ,  SCHAEFER STEFAN ,  STEIL KARL-HEINZ ,  RIECHMANN WERNFRIED ,  BYLSMAN FRIEDHELM

IPC: C07F9/52

公开(公告)号：DD131026A5

公开(公告)日：1978-05-24

申请号：DD20000477

申请日：1977-07-12

Applicant: HOECHST AG

Inventor： SCHAEFER STEFAN ,  GEHRMANN KLAUS ,  OHORODNIK ALEXANDER ,  STEIL KARL-HEINZ ,  RIECHMANN WERNFRIED ,  BYLSMA FRIEDHELM

IPC: C07F9/42 ,  C07F9/48 ,  C07F9/52

Abstract: Production of methyldichlorophosphane. The compound is made by reacting methane and phosphorus trichloride in a reaction zone in which a temperature higher than 500 DEG C is maintained. More specifically, hot reaction gas coming from the reaction zone is mechanically freed from solid matter, and the reaction gas freed from solid matter is passed to a quenching zone in which it is quenched with liquefied reaction mixture having 0.3 to 5 weight % of an organic barium compound or a non-ionic surfactant dissolved therein.

公开(公告)号：CH598272A5

公开(公告)日：1978-04-28

申请号：CH689176

申请日：1976-06-01

Applicant: HOECHST AG

Inventor： GEHRMANN KLAUS DR ,  LOHMAR ELMAR DR ,  OHORODNIK ALEXANDER DR ,  RIECHMANN WERNFRIED

IPC: C07F9/32 ,  C07F9/34 ,  C07F9/6571 ,  C07F9/6574 ,  C07F9/30

Abstract: 2,5 DIOXO-1-OXA-2-PHOSPHOLANES OF THE GENERAL FORMULA: in which R1 stands for an alkyl radical having from 1 to 4 carbon atoms, or a phenyl radical, and R2 and R3 each stand for hydrogen or CH3, are distillatively purified. To this end the respective crude compound is preheated to 120 DEG to 160 DEG C and fed to the head of a distilling column provided with a plurality of individually heatable trays maintained at temperatures increasing from the upper-most tray to the lowermost, the uppermost tray in the column being maintained at 120 DEG to 160 DEG C and the lowermost tray being maintained at 160 DEG to 200 DEG C, the pressure at the head of the column being 20 to 200 mm Hg, preferably 50 to 120 mm Hg; an inert gas preheated to 160 DEG to 200 DEG C is introduced countercurrently at the base of the column; those impurities having a boiling point lower than that of the respective 2,5-dioxo-1-oxa-2-phospholane are withdrawn overhead together with the inert gas; the 2,5-dioxo-1-oxa-2-phospholane thus freed from low-boiling impurities is withdrawn from the base of the distilling column and passed to a film evaporator; and the 2,5-dioxo-1-oxa-2-phospholane is distilled off from higher-boiling impurities in the film evaporator under a pressure of 0.1 to 5 mm Hg.