• 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:
    METHOD OF CONTINUOUS OBTAINING OF DIISOCYANATES OF GENERAL FORMULA i, - OCN-R-NCO where R is the group (S) (n) -,. .j (CH) -, by reacting a solution of a primary diamine of the general formula NHg-R-NHj; where R has the indicated values., with a solution of excess phosgene in an inert solvent at elevated pressures and temperatures, and the reagents are mixed by injecting solutions of diamine and phosgene under pressure using a nozzle, so as to increase the yield of the target product first, a solution of phosgene is fed, and then a solution of diamine with a temperature of 20-180 ° C, is fed into a solution of phosgene at a temperature using a jet nozzle with an internal diameter of 0.3-5.5 mm with a pressure drop of 1-80 atm.
    公开号:SU1192613A3
    申请号:SU823441302
    申请日:1982-05-21
    公开日:1985-11-15
    发明作者:Генниг Ганс-Иоахим；Ларс Юрген；Либш Дитер
    申请人:Байер А.Г.(Фирма)；
    IPC主号:
    专利说明:

    The invention relates to a continuous process for the preparation of a diisocyanato with the general formula OCN-R-NCO, (I) {de R - groups - (CH,) g -, -CgH-CHg-C H -, -Sbi, (CH) -. The purpose of the invention is to increase the yield of the target product. FIG. 1 shows a jet nozzle provided with a washing chamber; in fig. 2 technological scheme of the proposed method. The device contains a lead jc mixing chamber pipeline 1 for supplying the amine solution, jet nozzle 2 leading to the mixing chamber pipeline 3 for feeding the phosgene solution, mixing chamber 4 pump 5 for feeding the amine solution, pump 6 for feeding the phosgene solution suitable for heating the amine solution heat exchanger 7, suitable for heating the phosgene solution, heat exchanger 8 connected to the mixing chamber heated tubular reactor 9 (n is necessary for carrying out the proposed method), reducing valve 10, pipes wire P d retraction isocyanate solution Tel'nykh expand vessel 12, a cooler 13 and .truboprovod 14 for discharging the resulting gas phase. Example 1. In an installation containing a tubular reactor and a mixing chamber with an internal diameter of 25 mm with a total volume of the mixing chamber and a tubular reactor of 7.3 liters, the reaction was continuously subjected to 36.6 kg / h of a 15% solution of 1.6 α-diaminohexane in o-dichlorobenzene and 120 kg / h of a 44.6% phosgene solution in o-dichlorobenzene. The phosgene solution heated to 180 ° C is mixed with the amine solution heated to 130 ° C by feeding the amine solution by means of a jet nozzle having an internal diameter (clear) of 0.5 mm and a length of 4 mm into a mixing chamber filled without bubbles continuously supplied phosgene solution. The distance of the nozzle from the opposite outlet of the mixing chamber connected to the tubular reactor is 30 cm. The distance of the jet from the side wall of the mixing chamber is 12.25 mm. The mixing chamber, the tubular reactor and the phosgene solution are under pressure at 60 atm, the amine solution at the nozzle inlet at a pressure of 81 atm. The reaction mixture is continuously withdrawn from the tubular reactor through an exhaust valve and separated into gas and liquid phases in a separator. Liquid components are removed from the gas phase in a cooler by fractional condensation and recycled to the liquid phase. During the processing by distillation of the combined liquid phases, 7.83 kg / h of 1,6-diisocyanate hexane (98.5% by weight of the diamine) are obtained. PRI me R. 2. The process is carried out analogously to example 1, however, the pressure in the mixing and reaction chambers is 30 atm, and the solution of amine in front of the jet nozzle is under pressure of 58 atm. The yield of 1,6-diisocyanate hexane7, 7 kg / h (97% of theoretical). Example 3. A device similar to the device of Example 1 is used, however, a tubular reactor volume is chosen such that the total volume of the mixing chamber and the tubular reactor is 0.9 liters, the nozzle diameter is 0.5 mm. Analogously to the example of the reaction, 40 kg / h of a solution of 1,6 diiminohexane in o-dichlorobenzene heated to 17.8% and a 61.7% solution of phosgene in o-dichlorobenzene heated to 210 C and heated to 210 C and heated to 210 ° C atm In this case, the amine solution before entering the nozzle is under a pressure of 80 atm. The reaction temperature in the mixing chamber and the connected reaction zone is maintained at 220 ° C. The result is 9.91 g / h of 1,6-diisocyanatohexane (96% of theoretical, calculated on the diamine used). Example 4. Analogously to Example 3, the reaction is subjected to a 54 kg / h of a 16.8% aqueous solution of 1,6-diaminohexane in o-dichlorobenzene heated to 100 C and 108 kg / h to a 43.9% aqueous solution heated to 200 ° C phosgene. The diameter of the nozzle is 0.5 mm. The pressure of the reactor is 60 atm, and the pressure of the amine solution before entering the nozzle is 88 atm. The temperature in the mixing and reaction zones 221 C, Get 12.3 kg / h of 1,6-diisocyanatohexane (93.8% of theoretical). Example 5. The total volume of the mixture of the 1-cell chamber and the tubular reaction
    the torus in the device is 1.55 liters nozzle diameter 0.4 mm,
    33 kg / h of heated to 22% solution of 1.6 diaminohexane in O dichlorobenzene are reacted with 123 kg / h of heated to 62.2% solution of phosgene in o-dichlorobenzene. The pressure in the mixing and reaction zone 50 atm. The amine solution before entering the nozzle is under a pressure of 75 atm. The temperature in the mixing and reaction zones 200c.
    Get 9.89 kg / h of 1,6-diisocyanatohexane (94.9% of theoretical)
    Example 6. The diameter of the nozzle in the device of Example 1 is 0.55 mm.
    53.6 kg / h of a 18% aqueous solution of 4,4-diaminodiphenylmethane in chlorobenzene heated to 160 ° C undergo a reaction from 96.4 kg / h of a solution of phosgene in chlorobenzene heated to I90 C. The pressure in the mixing and reaction zones 65 atm. Solutions before entering the nozzle are under a pressure of 95 atm.
    This gives 11.7 kg / h of 4.4-diisocyanatodiphenylmethane (96% of theoretical).
    Example 7 The total volume of the mixing chamber and the connected reaction zone in the device is 3.7 liters, the nozzle diameter is 0.4 mm.
    42.2 kg / h of a 46.7% solution of a mixture of 2,4-di-aminotoluene and 2,6-diaminotoluene heated to 172 C in a weight ratio of 1.86: 1 in o-dichlorobenzene is reacted with 123.6 kg / h heated to 21bc 80% solution of phosgene in o-dichlorobenzene. The pressure in the mixing and reaction zone 60 atm. The pressure of the amine solution before entering the nozzle. 110 atm The temperature in the mixing and reaction zones,
    Get 16.8 kg / h diisocyanatotoluene (97% of theoretical.
    Example 8. The process is carried out in the apparatus of Example 5 using a nozzle having a clear diameter of 0.4 mm.
    33 kg / h of a 22% solution of 1,6-diaminohexane in o-dichlorobenzene heated to 135 C are reacted with 123 kg / h of a 62.2% solution of phosgene in o-dichlorobenzene heated to 190c. Under this pressure
    in the mixing and reaction zones 60 bar, and the pressure of the amine solution before entering the nozzle is 61 atm, i.e. pressure drop is 1 atm. The temperature in the mixing and reaction zones 200 C.
    9.7 kg / h of 1,6-diisocyanatohexane are obtained (92.4% of the theoretical, calculated on the starting di-
    10 amine).
    Example 9. The process is carried out in the apparatus of Example 3 using a nozzle having a clear diameter of 0.3 mm.
    15 32.7 kg / h heated to 100 С
    A 25.1% solution of a mixture of 2,4-diaminotoluene in a weight ratio of 1.54: 1 in o-dichlorobenzene is reacted with 127.3 kg / h
    20 to 100 to 62.2% phosgene solution in o-dichlorobenzene. In this case, the temperature and pressure in the mixing and reaction zones are 135c and 40 atm, and the pressure of the amine solution
    25 before entering the nozzle 120 atm, i.e. the pressure drop is 80 atm. 11.3 kg / h of diisocyanato-toluene are obtained (96.3% of the theoretical, calculated on the starting diamine).
    30 Example 10. The process is carried out in a device comprising a nozzle with a diameter of 5.5 mm, a tubular reactor and having an internal diameter of 200 mm.
     the total volume of the reactor and the mixer is 31.4 liters,
    7273 kg / h of a solution of 1,6-diaminohexane in α-chlorobenzene heated to 15% is reacted with 25180 kg / h of a solution of phosgene in chlorobenzene heated to 44.2%. At the same time, the pressure in the mixing and reaction zones is 60 atm, and the amine solution at the entrance to the nozzle is under a pressure of 110 atm, t, e, the pressure drop is 50 atm.
    1503 kg / h of 1,6-diisocyanatohexane are obtained (95% of the theoretical, in terms of initial diamine j).
    0 Example 11, the process is carried out analogously to example 7, however, the solution of the mixture of diamines and solution of diocreHa supplied to the reaction has a temperature of 20 and 150 ° C, respectively
    5 wherein the pressure in the mixing and reaction zones is 40 atm, and the pressure of the diamine mixture solution before entering the nozzle is 60 atm.
    Get 1,6,7 kg / h 1, b-diisocyanotoluene (96.4% of theoretical.
    Example 2. The process is carried out analogously to example 1, however, 40 kg / h of an 18% aqueous solution of 1,6-diaminohexane 8 o-dichlorobenzene. with a temperature of 180 C is subjected zai 1rdays: tviyu with
    120 kg / h of a 60% phosgene solution in o-dichlorobenzene with a temperature of 225 ° C. The pressure in the mixing and reacting zones is 100 atm. The pressure of the diamine solution before entering the nozzle is 120 atm.
    The yield of 1,6-diisocyanatohexane 97% of theoretical.

    / 3.
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    //
    权利要求:
    Claims (1)
    [1]
    METHOD FOR CONTINUOUS PRODUCTION OF DIISOCIANATES OF THE GENERAL FORMULA 'у ·· - -
    OCN-R-NCO where R are the groups 'g (CHj) 6 -, C € H 4 -CH -CgH-CfrH ^ CH ^) -,' by reacting a solution of primary diamine of the general formula
    NH 2 -R-NH f where R has the indicated meanings ^ with a solution of excess phosgene in an inert solvent at elevated pressures and temperatures, the reagents being mixed by feeding pressure solutions of diamine and phosgene using a nozzle, which means that, in order to increase the yield of the target product, first a phosgene solution is fed, and then a diamine solution with a temperature of 20-180 ° C is fed into the phosgene solution at a temperature of 100-225 ° C by means of a jet nozzle with an inner diameter of 0.3-5.5 mm at pressure drop 1–80 atm.
    , SU „„ 1192613 i JI
    类似技术:
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    同族专利:
    公开号 | 公开日
    EP0065727A1|1982-12-01|
    JPS57200346A|1982-12-08|
    DE3121036A1|1982-12-16|
    ES8304071A1|1983-02-16|
    EP0065727B1|1984-07-25|
    US4419295A|1983-12-06|
    UA7217A1|1995-06-30|
    JPH0153664B2|1989-11-15|
    DD206782A5|1984-02-08|
    CA1183145A|1985-02-26|
    MX159880A|1989-09-25|
    ES512549A0|1983-02-16|
    BR8203067A|1983-05-10|
    DE3260452D1|1984-08-30|
    引用文献:
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    DE3717058C2|1987-05-21|1992-12-17|Bayer Ag, 5090 Leverkusen, De|
    DE3717057C2|1987-05-21|1989-11-02|Bayer Ag, 5090 Leverkusen, De|
    CA2010224A1|1989-02-23|1990-08-23|Teruyuki Nagata|Preparation process of xylylene diisocyanate|
    DE4217019A1|1992-05-22|1993-11-25|Bayer Ag|Process for the preparation of aromatic diisocyanates|
    DE4412327A1|1994-04-11|1995-10-12|Bayer Ag|Process for the preparation of diisocyanates|
    DE4443642A1|1994-12-08|1996-06-13|Bayer Ag|Continuous process for the production of organic isocyanates|
    DE19817691A1|1998-04-21|1999-10-28|Basf Ag|Production of diphenylmethanediisocyanate and polyphenylene-polymethylene-polyisocynate mixtures|
    ITMI20010860A1|2001-04-24|2002-10-24|Enichem Spa|PROCEDURE FOR THE CONTINUOUS PRODUCTION OF POLYISOCYANATES|
    DE10222968A1|2002-05-23|2003-12-04|Basf Ag|Process for the preparation of isocyanates|
    US20040008572A1|2002-07-09|2004-01-15|Stuart Joseph Y.|Coaxial jet mixer nozzle with protruding centerbody and method for mixing two or more fluid components|
    DE10260082A1|2002-12-19|2004-07-01|Basf Ag|Process for the continuous production of isocyanates|
    DE10260094A1|2002-12-19|2004-07-01|Basf Ag|Process for the preparation ofaliphatic isocyanates|
    DE10310888A1|2003-03-11|2004-09-23|Basf Ag|Production of polyisocyanates useful for polyurethane production comprises reacting an amine with phosgene in a tubular reactor and passing the reactor effluent to a distillation column|
    DE10349504A1|2003-10-23|2005-05-25|Bayer Technology Services Gmbh|Process for the preparation of isocyanates in the gas phase|
    CN1964776A|2004-06-09|2007-05-16|亨茨曼国际有限公司|Mixer nozzle and method for mixing two or more fluids and process for manufacturing isocyanates|
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    WO2018114846A1|2016-12-21|2018-06-28|Covestro Deutschland Ag|Process for preparing an isocyanate|
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    法律状态:
    优先权:
    申请号 | 申请日 | 专利标题
    DE19813121036|DE3121036A1|1981-05-27|1981-05-27|METHOD FOR THE CONTINUOUS PRODUCTION OF ORGANIC MONO- OR POLYISOCYANATES|
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