• 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:
    The invention relates to substituted isotanes, in particular toluene diisocyanate (TDI1, which is used in the polymer industry. Upon production of Td, up to 10-15% of heavy liquid substances are formed, which concentrate the distillate to 30-40% of the TDI content. Distillation residue
    公开号:SU1264840A3
    申请号:SU782634047
    申请日:1978-07-12
    公开日:1986-10-15
    发明作者:Эйу Пьер；Дъосси Филипп
    申请人:Продюи Шимик Южин Кюльман (Фирма)；
    IPC主号:
    专利说明:

    1 The invention relates to the isolation of products from industrial wastes, in particular, to a method for separating tolu and diisocyanate (TDI) from industrial wastes. In the production of TDI, between 10 and 15% of heavy liquid compounds are formed. These heavy compounds are concentrated by distilling TDI to the usual concentration of TDI and heavy compounds. Due to the increase in viscosity of the mixture, it is difficult to continue further distillation in order to obtain high concentrations of heavy compounds and the desired product (TDI) remains in the waste. The aim of the invention is to reduce the content of toluene diisocyanate in solid residues by using certain cross-coupling conditions. The process is carried out as follows. The initial mixture is continuously heated on a wall with a maximum temperature of 250 ° C, evaporating TDI at a relatively low temperature (120 ° C at a pressure of 12 mm Hg) while stirring for a sufficient time; to ensure mass transfer. As it progresses along the apparatus, the mixture is gradually heated to a temperature of approximately 215 ° O, a transition from a viscous state to a pasty state, and then a solid one. Stirring should ensure heat transfer, product progression in the evaporator, scraping of solids, and grinding of the foam that may form. The volume of the apparatus must be such that the duration of the presence of products in it ensures the necessary mass transfer (15-36 min). The substances leaving the apparatus contain at least 3% TDI. After that, their temperature can be raised to 280 ° C without danger of foaming at the end of the apparatus in order to remove the last traces of TDI. Dry, porous and crushed waste can be easily removed either to a vacuum-collecting system, acting as a tambour, or even better, by continuous extrusion with a heated screw through a spinneret, which provides gas-tightness. Solid waste in the form of powder or dense granules is picked up by pneumatic conveying and sent 402 to an incinerator, and TDI is condensed. An apparatus with a surface of 20–25 m and a volume of 1600 l, coupled with an extruder, ensures continuous separation of heavy TDI compounds from a plant with a capacity of 30000 t / year TDI. Example. The mixture taken from one concentration column and consisting of 43% TDI and 57% heavy compounds will be loaded into the apparatus at the rate of 60 kt / h at 120 ° C. The apparatus, with a total volume of 20 liters, has a heated surface of 0.86 m and is equipped with two self-cleaning screw-type agitators, which rotate at different speeds. With a pressure of 12 mm Hg. the mixture is gradually heated to a temperature of 215 ° C and turns into a powder containing 2.8% TDI after holding for 15 minutes. TDIs are condensed and collected, and heavy waste is extruded under pressure through a die and granules with a diameter of 6 and a length of 15 mm are obtained in an amount of 30 kg / h. Examples 2-4. Analogously to Example 1, but with different loading and holding times, the results are shown in the table .. Example 3 shows that a minimum holding time of 15 minutes is required to produce wastes with a low content of TDI. Apply p 5. (C15avlenie). In the apparatus as in example 1 is served when the flow rate of 50 kg / h mixture containing 45% TDI and 55% of the residues. The temperature of this mixture is adjusted to 26 ° C under a vacuum of 15 mm Hg. After condensation, 19.2 kg / h of TDI and 30.8 kg / h of solid residues containing 0.17% of free TDI are collected. The residence time was 18 minutes. It is noted that under these conditions more than 14% of free TDI is polymerized in the apparatus. P m and m 6 (comparison). Analogously to Example 1, when the flow rate is 50 kg / h, a mixture containing 45% TDI and 55% of residues is supplied to the apparatus. The temperature of this mixture is adjusted to 15 mm Hg under vacuum. After condensation, 21.5 kg / h of TDI and 28.5 kg / h of residues containing 3.5% of free TCI are collected. Under these conditions, poor T-CI evaporation is observed, the loss is about 4.4% of the TDI contained in the residues. Thus, the method allows to reduce the content of TDI in solid residues to 0.05-3.4% versus 10- 20% in the known method. 40 Formula and breaches Method for separating toluene diisocyanate from production wastes containing 43-45% toluene diisocyanate and 55-57% t of solid residues by evaporation at elevated temperature and reduced pressure, also with the aim of reducing the content of toluene diisocyanate in solid residues, evaporation is carried out in an evaporator with stirring and scraping with an initial temperature of 120 ° C, which is increased to 215 ° C at a pressure of 12 mm Hg. and the residence time in the evaporator is 15-36 minutes with continuous removal of the solid residue.
    权利要求:
    Claims (1)
    [1]
    Claim
    Method for the extraction of toluene diisocyanate from industrial wastes containing 43-45% toluene diisocyanate and 55-57% heavy residues by evaporation at elevated temperature and reduced pressure, so that, in order to reduce the content toluene diisocyanate in solid residues, evaporation is carried out in an evaporator with stirring and scraping with an initial temperature of 120 ° C, which is increased to 215 ° C at a pressure of 12 mm Hg and residence time [in the evaporator 15-36 min with continuous removal of solid residue.
    - Compiled by I. Kulikova
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    同族专利:
    公开号 | 公开日
    IT1111627B|1986-01-13|
    AU522377B2|1982-06-03|
    DK154426B|1988-11-14|
    DD138314A5|1979-10-24|
    BR7804465A|1979-03-20|
    IN148484B|1981-03-07|
    JPS5419938A|1979-02-15|
    AU3790278A|1980-01-17|
    EP0000463A1|1979-01-24|
    IE781366L|1979-01-12|
    DK310578A|1979-01-13|
    DK154426C|1989-04-10|
    FR2397396A1|1979-02-09|
    IT7868483D0|1978-06-23|
    IE47024B1|1983-11-30|
    JPS612057B2|1986-01-22|
    US4216063A|1980-08-05|
    FR2397396B1|1980-01-18|
    DE2861504D1|1982-02-25|
    EP0000463B1|1982-01-06|
    ES471637A1|1979-02-01|
    AR214462A1|1979-06-15|
    PT68171A|1978-07-01|
    CA1094090A|1981-01-20|
    引用文献:
    公开号 | 申请日 | 公开日 | 申请人 | 专利标题
    US2706169A|1954-03-04|1955-04-12|Du Pont|Flash distillation of 2,4-tolylene diisocyanate|
    US2974725A|1954-05-04|1961-03-14|Bayer Ag|Process and apparatus for continuously obtaining dry materials|
    US3457291A|1965-04-01|1969-07-22|Union Carbide Corp|Production of isocyanates|
    US3405040A|1965-08-31|1968-10-08|Mobay Chemical Corp|Method for recovering tolylene diisocyanate|
    US3542112A|1968-06-05|1970-11-24|Artisan Ind|Thin-film evaporator having multi-zone temperature control jacket|
    CA998060A|1970-05-22|1976-10-05|Carl F. Irwin|Recovery of organic isocyanate|
    DD130143B1|1975-08-15|1979-12-27|Guenter Muecke|METHOD FOR CONTINUOUS THERMAL SEPARATION OF ORGANIC ISOCYANATES FROM LIQUID DISTILLATION RESIDUE|DE2915830A1|1979-04-19|1980-10-23|Basf Ag|PRODUCTION OF TOLUYLENE DIISOCYANATE AND / OR HIGH-BOILING SOLVENTS IN THE FLUID BED FROM DISTILLATION RESIDUES OF THE TOLUYLENE DIISOCANATE PRODUCTION|
    FR2625742B1|1988-01-13|1990-06-22|Rhone Poulenc Chimie|PROCESS FOR SEPARATION OF TOLUENE DIISOCYANATE CONTAINED IN THE RESIDUES OF ITS MANUFACTURE|
    JPH02138567U|1989-04-21|1990-11-19|
    US5051152A|1989-09-26|1991-09-24|Air Products And Chemicals, Inc.|Preparation of urethane prepolymers having low levels of residual toluene diisocyanate|
    JP2504851Y2|1990-02-07|1996-07-24|株式会社シマノ|Lead switch mounting structure for fishing reels|
    DE4317669A1|1993-05-27|1994-12-01|Bayer Ag|Process for the preparation of isocyanates and continuous work-up of the residue|
    DE4430951C1|1994-08-31|1996-05-23|Bayer Ag|Method and device for separating a solid residue from its solution in a stirred material bed|
    US5962728A|1997-10-31|1999-10-05|Arco Chemical Technology, L.P.|Isocyanate residue purification|
    DE10260092A1|2002-12-19|2004-07-01|Basf Ag|Process for the purification of isocyanates|
    WO2007036479A1|2005-09-29|2007-04-05|Basf Se|Method for purifying residues containing isocyanates|
    CN102408354A|2011-10-24|2012-04-11|天津大学|Method and device for recovering toluene diisocynate|
    EP2872481B1|2012-07-11|2016-08-24|Covestro Deutschland AG|Method for working up distillation residues from isocyanate production|
    法律状态:
    优先权:
    申请号 | 申请日 | 专利标题
    FR7721436A|FR2397396B1|1977-07-12|1977-07-12|
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