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公开(公告)号：ZA764225B
公开(公告)日：1977-07-27
申请号：ZA764225
申请日：1976-07-16
Applicant: HOECHST AG
Inventor： GEHRMANN K , OHORODNIK A , LOHMAR E , RIECHMANN W
IPC: C07F9/32 , C07F9/34 , C07F9/6571 , C07F9/6574 , C07F
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the column; those impurities having a boiling point lower than that of the respective 2,5-dioxo-1-oxa-2-phospholane are withdrawn overhead together with the inert gas; the 2,5-dioxo-1-oxa-2-phospholane thus freed from low-boiling impurities is withdrawn from the base of the distilling column and passed to a film evaporator; and the 2,5-dioxo-1-oxa-2-phospholane is distilled off from higher-boiling impurities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.
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公开(公告)号：ZA7603944B
公开(公告)日：1977-06-29
申请号：ZA7603944
申请日：1976-07-02
Applicant: HOECHST AG
Inventor： LOHMAR E , GEHRMANN K , OHORODNIK A , STUTZKE P
CPC classification number: C07F9/34
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公开(公告)号：NO132588C
公开(公告)日：1975-12-03
申请号：NO114170
申请日：1970-03-25
Applicant: HOECHST AG
Inventor： SENNEWALD K , OHORODNIK A , MITTLER W , HUNDECK J , HARDEL H-J
Abstract: 1282682 Dehalogenation of haloacids KNAPSACK AG 16 March 1970 [25 March 1969] 12540/70 Heading C2C Monohalocarboxylic acids are prepared from dihalocarboxylic acids, optionally in admixture with trihalocarboxylic acids, by hydrogenation at 60 to 170 C. using a stationary or suspended catalyst comprising a Group VIII metal with an inert carrier, the catalyst being activated by one or more of (a) a non-poisonous metal salt, oxide or hydroxide, and/or (b) an inorganic or organic proton donor. Examples relate to the purification of crude monochloroacetic acid obtained by the chlorination of glacial acetic acid in the presence of acetic anhydride and acetyl chloride, the product containing dichloroacetic acid, trichloroacetic acid and acetic acid. Metal and ammonium activators specified are metals, alkaline earth metals, rare earth metals or metals of Groups 4 or 5, e.g. lithium chloride, sodium acetate, sodium chloride, sodium chloroacetate, sodium carbonate, potassium acetate, potassium chloride, ammonium acetate, ammonium chloride, calcium chloride, aluminium chloride, cerium dioxide, titanium dioxide and vanadium pentoxide. Organic proton-donor activators specified are triethylamine, pyridine, 4-amino-pyridine, piperidine, glycine, urea or triphenyl-phosphine, salts thereof, trichlorosilane, glycocoll, butyraldehyde, di-isobutyl ketone, butyl acetate and cyanoacetic acid. Granular inert carriers of small grain size are advantageous. Specified catalyst-carrier systems are palladium-silica or silicic acid. The process is preferably operated continuously, with recycling of the hydrogenated products and separation of the catalyst therefrom.
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Patent Agency Ranking
公开(公告)号：DE1915037C3
公开(公告)日：1975-10-30
申请号：DE1915037
申请日：1969-03-25
Applicant: HOECHST AG, 6000 FRANKFURT
Inventor： SENNEWALD K , OHORODNIK A , MITTLER W , HUNDECK J , HARDEL H-J
Abstract: 1282682 Dehalogenation of haloacids KNAPSACK AG 16 March 1970 [25 March 1969] 12540/70 Heading C2C Monohalocarboxylic acids are prepared from dihalocarboxylic acids, optionally in admixture with trihalocarboxylic acids, by hydrogenation at 60 to 170 C. using a stationary or suspended catalyst comprising a Group VIII metal with an inert carrier, the catalyst being activated by one or more of (a) a non-poisonous metal salt, oxide or hydroxide, and/or (b) an inorganic or organic proton donor. Examples relate to the purification of crude monochloroacetic acid obtained by the chlorination of glacial acetic acid in the presence of acetic anhydride and acetyl chloride, the product containing dichloroacetic acid, trichloroacetic acid and acetic acid. Metal and ammonium activators specified are metals, alkaline earth metals, rare earth metals or metals of Groups 4 or 5, e.g. lithium chloride, sodium acetate, sodium chloride, sodium chloroacetate, sodium carbonate, potassium acetate, potassium chloride, ammonium acetate, ammonium chloride, calcium chloride, aluminium chloride, cerium dioxide, titanium dioxide and vanadium pentoxide. Organic proton-donor activators specified are triethylamine, pyridine, 4-amino-pyridine, piperidine, glycine, urea or triphenyl-phosphine, salts thereof, trichlorosilane, glycocoll, butyraldehyde, di-isobutyl ketone, butyl acetate and cyanoacetic acid. Granular inert carriers of small grain size are advantageous. Specified catalyst-carrier systems are palladium-silica or silicic acid. The process is preferably operated continuously, with recycling of the hydrogenated products and separation of the catalyst therefrom.
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公开(公告)号：NO132588B
公开(公告)日：1975-08-25
申请号：NO114170
申请日：1970-03-25
Applicant: HOECHST AG
Inventor： SENNEWALD K , OHORODNIK A , MITTLER W , HUNDECK J , HARDEL H-J
Abstract: 1282682 Dehalogenation of haloacids KNAPSACK AG 16 March 1970 [25 March 1969] 12540/70 Heading C2C Monohalocarboxylic acids are prepared from dihalocarboxylic acids, optionally in admixture with trihalocarboxylic acids, by hydrogenation at 60 to 170 C. using a stationary or suspended catalyst comprising a Group VIII metal with an inert carrier, the catalyst being activated by one or more of (a) a non-poisonous metal salt, oxide or hydroxide, and/or (b) an inorganic or organic proton donor. Examples relate to the purification of crude monochloroacetic acid obtained by the chlorination of glacial acetic acid in the presence of acetic anhydride and acetyl chloride, the product containing dichloroacetic acid, trichloroacetic acid and acetic acid. Metal and ammonium activators specified are metals, alkaline earth metals, rare earth metals or metals of Groups 4 or 5, e.g. lithium chloride, sodium acetate, sodium chloride, sodium chloroacetate, sodium carbonate, potassium acetate, potassium chloride, ammonium acetate, ammonium chloride, calcium chloride, aluminium chloride, cerium dioxide, titanium dioxide and vanadium pentoxide. Organic proton-donor activators specified are triethylamine, pyridine, 4-amino-pyridine, piperidine, glycine, urea or triphenyl-phosphine, salts thereof, trichlorosilane, glycocoll, butyraldehyde, di-isobutyl ketone, butyl acetate and cyanoacetic acid. Granular inert carriers of small grain size are advantageous. Specified catalyst-carrier systems are palladium-silica or silicic acid. The process is preferably operated continuously, with recycling of the hydrogenated products and separation of the catalyst therefrom.
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公开(公告)号：CH563186A5
公开(公告)日：1975-06-30
申请号：CH1583071
申请日：1971-10-29
Applicant: HOECHST AG
Inventor： OHORODNIK A , SENNEWALD K , HUNDECK J , STUTZKE P
IPC: B01J8/00 , B01J8/18 , B01J8/22 , C07C51/377 , B01J8/08
Abstract: 1363245 Liquid phase catalytic process, separating solids from liquid KNAPSACK AG 4 Oct 1971 [29 Oct 1970] 46060/71 Headings B1D and B1F In catalyst/liquid separator 7, liquid product is drawn off through valve 11 at a rate such that the upward rate of flow of liquid in separator 7 is less than the rate of sedimentation of catalyst in the separator. Circulation of reaction mixture is effected by the gas-lift effect of gas from line 9 and pump 3. The hydrogenative dehalogenation of dichloracetic acid to produce monochloracetic acid is described using a palladium catalyst on a silica carrier.
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公开(公告)号：DE1915037B2
公开(公告)日：1975-03-13
申请号：DE1915037
申请日：1969-03-25
Applicant: HOECHST AG, 6000 FRANKFURT
Inventor： SENNEWALD K , OHORODNIK A , MITTLER W , HUNDECK J , HARDEL H-J
Abstract: 1282682 Dehalogenation of haloacids KNAPSACK AG 16 March 1970 [25 March 1969] 12540/70 Heading C2C Monohalocarboxylic acids are prepared from dihalocarboxylic acids, optionally in admixture with trihalocarboxylic acids, by hydrogenation at 60 to 170 C. using a stationary or suspended catalyst comprising a Group VIII metal with an inert carrier, the catalyst being activated by one or more of (a) a non-poisonous metal salt, oxide or hydroxide, and/or (b) an inorganic or organic proton donor. Examples relate to the purification of crude monochloroacetic acid obtained by the chlorination of glacial acetic acid in the presence of acetic anhydride and acetyl chloride, the product containing dichloroacetic acid, trichloroacetic acid and acetic acid. Metal and ammonium activators specified are metals, alkaline earth metals, rare earth metals or metals of Groups 4 or 5, e.g. lithium chloride, sodium acetate, sodium chloride, sodium chloroacetate, sodium carbonate, potassium acetate, potassium chloride, ammonium acetate, ammonium chloride, calcium chloride, aluminium chloride, cerium dioxide, titanium dioxide and vanadium pentoxide. Organic proton-donor activators specified are triethylamine, pyridine, 4-amino-pyridine, piperidine, glycine, urea or triphenyl-phosphine, salts thereof, trichlorosilane, glycocoll, butyraldehyde, di-isobutyl ketone, butyl acetate and cyanoacetic acid. Granular inert carriers of small grain size are advantageous. Specified catalyst-carrier systems are palladium-silica or silicic acid. The process is preferably operated continuously, with recycling of the hydrogenated products and separation of the catalyst therefrom.
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公开(公告)号：SE371431B
公开(公告)日：1974-11-18
申请号：SE1789769
申请日：1969-12-23
Applicant: HOECHST AG
Inventor： SENNEWALD K , OHORODNIK A , MITTLER W , HUNDECK J
IPC: C07C53/16 , B01J23/00 , C07C51/00 , C07C51/377 , C07C51/487 , C07C67/00 , C07C51/42
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