• 专利附录
  • 专利说明
  • 权利要求
  • 类似技术
  • 同族专利
  • 引用文献
  • 法律状态
  • 优先权
    • 专利摘要:
    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.
    公开号:SU942600A3
    申请号:SU772503095
    申请日:1977-07-14
    公开日:1982-07-07
    发明作者:Шефер Штефан；Германн Клаус；Охородник Александер；Штайль Карл-Хайнц；Рихманн Вернфрид；Билсма Фридхельм
    申请人:Хехст Аг (Фирма)；
    IPC主号:
    专利说明:

    This invention relates to the chemistry of organophosphorus compounds, namely, a method for separating methylcyclochloride, which is of great importance not only as a semi-organic organophosphorus synthesis, but is also used as the INITIATIVE material for non-combustible finishing of fibers and materials. A known method for the separation of methyldichlorophosphine by distilling the reaction mixture obtained by reacting methane with phosphorus trichloride when heated to 35 ° -9OO C in the presence of a catalyst, phosgene tl. The closest to the proposed technical essence and the achieved result is a method for separating methyldi chlorophosphine from the reaction mixture obtained by reacting methane in the reaction zone with phosphorus trichloride in the presence of carbon tetrachloride at 4OO-70 ° C, consisting in the fact that the reaction mixture forms consisting mainly of phosphorus trichloride and methyldichlorophosphine, treated at 4O-5O With a passivating agent — phenol, orthocresol, n-butanorle, bisphenol, hisphenol, or .N-methylSHLINOM for binding trichloride phosphorus, followed by isolation of the target product by distillation 2}. The disadvantages of this method include the formation of solid solutions, which are deposited on the main surface of the heat exchangers, which prevents the normal functioning of the equipment and makes it necessary to clean the equipment at short intervals. The purpose of the invention is the prevention of the clogging of equipment by hard deposits. This goal is achieved by the fact that in the process of separation of methyldichlorophosphine from the reaction mixture, by semi-interaction by reacting methane with phosphorus trichloride in the reaction zone in the absence of carbon tetrachloride at 500–650 Cj, a hot reaction gas, coming out of the radioactivity zone, is cleaned from the radioactivity zone and cleaned from 500 ° Cj, cleaned from the radioactivity zone, cleaned from the radioactivity zone, cleaned from the radioactivity zone, cleaned from the radioactivity zone, cleaned from the radioactivity zone, cleaned from the radioactivity zone, cleaned from the radioactivity zone, cleaned from the radioactivity zone, cleaned from the radioactivity zone, cleaned from the radioactivity zone, cleaned from the radioactivity zone and cleaned from 500 ° Cj, cleaned from the radioactidate zone, cleaned from the radioactivity zone, cleaned from the radioactivity, cleaned from the radioactivity, cleaned from the radioactivity, cleaned from the radioactivity, cleaned from the radioactivity, and cleaned from 500 ° Cj. by and cooled in a Venturi tube with a liquefied reaction mixture containing soluble sol. 1.3-2% w / v of a mixture of phenol and barium sulfonate, or a non-ionic surfactant a-ethoxylated unbranched aliphatic alcohol with 16-1.8 carbon atoms, or ethylene oxide polymer, or ethylene oxide polymer and propylene oxide, to produce a gas phase containing methane and vozoroc chloride, which is subjected to two-stage cooling to minus 5 minus 5СгС, is subsequently washed with water and alkali, are compressed, followed by drying and recycling to the reaction zone, and the liquid reaction mixture which is circulated between the rapid cooling units and the cooling zone, part of the chi of the quenching reaction mixture and fed to a stripper to obtain a steam mixture containing methyldichlorophosphine and phosphorus trichloride, which condense, add the above additions of an organic barium compound or non-ionic surfactant to it and recirculate to the two-stage cooling stage, and get a bottom product withdrawn in an amount corresponding to the amount of methyl methyl chlorophosphine produced in the reaction, which is subjected to distillation in a thin-film evaporator with obtaining containing phosphorus trichloride and methyldichlorophosphine distillate, followed by feeding it to isolate the target product. The distinguishing features of the proposed methyldichlorophosphine isolation method include preliminary, prior to distillation, the mechanical purification of solid gas from the impurities, its rapid cooling in the Venguri tube and following processing in the writing. in a way. The proposed method for the separation of megyl dichlorophosphine prevents the clogging of equipment by hard deposits, since the introduction of organic barium compounds or non-ionic surfactants prevents the decomposition of methyldichlorophosphine, and therefore the formation of salt-like solids, which deposit and clog the equipment, especially in the form of salt-like solids, which deposit and clog the equipment, especially in the form of salt-like solids, which deposit and clog the equipment, especially in the form of salt, like salt-like solids, which deposit and clog equipment, especially In the proposed method, the reaction zone consists of a preheating zone, a main heating zone and is heated outside by electricity, with, on the one hand, the exit from the preheating zone is connected to the entrance to the main heating zone, and on the other, the exit from the main heating zone with an inlet located outside the electrically heated reaction zone — a cooling zone, each connection being made through a solid material separation zone. The drawing shows a process diagram. PCP is supplied,., and according to line I of SRI 2, CCS is supplied in such proportion that 2-7 mol.% of CER are contained in the mixture of liquids. Through line 3, methane is supplied to the plant, which through line 4 together with the RSED / SSb mixture enters the circulating evaporation 5, in which, at a given elevated temperature, methane is saturated with the RSbd / SSED mixture. Thus, the gas mixture with a given SND: PQ molar ratio: SSRd is continuously supplied through conduit 6 to the electrically heated tubular reactor 7. The reactor consists of a preheating zone 8 and another main heating 9. In the preheating zone, the initial mixture is heated to the reaction temperature (50 l-SSO C), while in the main heating zone 9 it is maintained at a constant reaction temperature. Such a division into two stages is advantageous to withstand an exact exposure time. Both parts of the tubular reactor are positioned in such a way that the exit of the preheating zone 8 through the first solid separation zone 1O outside the heating chamber of the reactor 7 is connected to the entrance to the main heating zone 9. The outlet of the main heating zone 9, again outside the heating chamber, is connected to the second zone 11 of the separation of solids. Due to such a device, the ingress of solids to the subsequent circulation system of the liquid is significantly reduced. The hot, gaseous reaction mixture from the second zone 11 of the separation of solid substances, via line 12, enters the rapid cooling system 13 designed as a Venturi tube. A flowing continuous reaction mixture is used as the cooling liquid.
    59426006
    权利要求:
    Claims (2)
    [1]
    1.Patent of the USSR N "341238, cl. C 07 F 9/52, published 1972.
    [2]
    2. The US patent fo 3519685, kl.62O543, published. 1964 (prototype). 012 mixture and potsayug on ogparku with ggolucheniem vapor mixture soserisaschey metipdihlorfosfin and phosphorus trichloride, which is condensed is introduced into it supplements the organic compound of barium or neishogennogo surface active aforementioned substances and ratsirkuliruyut on statsto two-stage cooling and receive the bottom product withdrawn in kolichestvo corresponding the amount of methyldichlorophosphine formed in the reaction zone, which is subjected to distillation in a thin-film evaporator to obtain phosphorus trichloride containing op and metildihlorfosfin distillate with posledukshey feed it to the selection ueneBoro product. Priority by featured. 14,07,76 - by all indications for the introduction of an additive of a non-ionic surfactant of ethoxylated unbranched aliphatic alcohol with 16-18 carbon atoms, or a polymer of ethylene oxide, or a polymer of ethylene oxide and propyl oxide. 26.O4.77 - the introduction of the additive - non-isogenic surfactant - ethoxylated unrefined aliphatic alcohol with 16-18 atoms
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    类似技术:
    公开号 | 公开日 | 专利标题
    Atherton et al.1945|174. Studies on phosphorylation. Part II. The reaction of dialkyl phosphites with polyhalogen compounds in presence of bases. A new method for the phosphorylation of amines
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    SU1480758A3|1989-05-15|Method of producing 1,2-dicholroethane
    US3013093A|1961-12-12|Alkylation process
    US3483279A|1969-12-09|Michaelis-arbuzov reaction
    US3201435A|1965-08-17|Process for the production of trimethyl phosphite
    US3823207A|1974-07-09|Process for the preparation of triarylphosphites
    US4764607A|1988-08-16|Method for recovering caprolactam
    CA1084864A|1980-09-02|Production of pure methyldichlorophosphane
    Harger et al.1989|Evidence for cyclic azaphosphiridine oxide intermediates in the methoxide-induced rearrangements of N-alkyl α-chlorophosphonamidates: formation of phosphoramidates as well as α-aminophosphonates
    SU383304A1|METHOD OF OBTAINING 0, O-DIALKYLCHLORTHIOPHOSPHATE
    US3347937A|1967-10-17|Continuous process for manufacture of trihalophenols
    US4305789A|1981-12-15|Energy efficient process of preparing triaryl phosphates
    GB2104542A|1983-03-09|Continuous saponification method and related system
    US2125490A|1938-08-02|Manufacture of aromatic alcohol
    同族专利:
    公开号 | 公开日
    FR2358416A1|1978-02-10|
    JPS5629879B2|1981-07-10|
    FR2358416B1|1983-10-07|
    CA1087206A|1980-10-07|
    AT352753B|1979-10-10|
    CH630093A5|1982-05-28|
    IT1079286B|1985-05-08|
    JPS5318517A|1978-02-20|
    DD131026A5|1978-05-24|
    US4104304A|1978-08-01|
    NL7707763A|1978-01-17|
    GB1562008A|1980-03-05|
    ATA499877A|1979-03-15|
    引用文献:
    公开号 | 申请日 | 公开日 | 申请人 | 专利标题
    US3210418A|1953-10-19|1965-10-05|Fmc Corp|Preparation of aliphatic dihalophosphines|DE2901298A1|1979-01-13|1980-07-24|Hoechst Ag|PREVENTION OF SOLID DEPOSITS IN MIXTURES CONTAINING METHYLDICHLORPHOSPHANE|
    DE2936609A1|1979-09-11|1981-04-02|Hoechst Ag, 6000 Frankfurt|METHOD FOR PRODUCING 2-CHLORFORMYLETHYL-METHYL-PHOSPHINO ACID CHLORIDES|
    CN102357353A|2011-09-20|2012-02-22|韩扶军|fixed bed reactor used for producing methyl phosphoric dichloride|
    CN108659042B|2018-06-22|2020-08-04|河北威远生物化工有限公司|Extraction separation method and extraction rectification equipment of alkyl phosphine dichloride|
    CN109134536A|2018-08-20|2019-01-04|南京红太阳股份有限公司|A kind of method of fluidized bed synthesizing methyl dichloride phosphine|
    CN109111477A|2018-08-20|2019-01-01|南京红太阳股份有限公司|A kind of Industrialized synthesis method of dichloromethylphosphine|
    CN110563761B|2019-09-11|2022-03-01|利尔化学股份有限公司|Method for cleaning coking substance of methyl phosphine dichloride synthesis trapping system|
    法律状态:
    优先权:
    申请号 | 申请日 | 专利标题
    DE2631608A|DE2631608C2|1976-07-14|1976-07-14|Process for the production of methyldichlorophosphine|
    DE19772718391|DE2718391C2|1977-04-26|1977-04-26|Process for the production of methyldichlorophosphine|
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