• 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:
    Verfahren zur Herstellung von nitrosaminfreien N, N-disubstituierten nitroaromatischen Aminen durch Abbau ihrer herstellungsbedingten Nitrosaminbestandteile und Stabilisierung der Produkte gegen erneute Nitrosaminbildung, indem man die Amine in flüssiger bzw. geschmolzener Form mit einer Sulfonsäure behandelt, ggfs. in Gegenwart von inerten organischen Lösungsoder Verdünnungsmitteln.
    公开号:SU1373315A3
    申请号:SU843822554
    申请日:1984-12-12
    公开日:1988-02-07
    发明作者:Хайнрих Рудольф；Альбрехт Конрад
    申请人:Хехст Аг (Фирма)；
    IPC主号:
    专利说明:

    00
    -h
    with
    with
    ate

    CN
    The invention of tnosigs to nitroaromatic amnion, ti to the diligent purification of nitroaromatic general formula
    , N09
    f VN (l
    (I)
    where R is CF, or ,,
    which isiol uthol r acupion i ep-bicide,
    The aim of the invention is to increase h 1 st 1 th 1 and stub. Tests of target liquidity by means of a technical target product with UL1) f 1kistot, for example aliphatic h1-sco1 1, arsenic, 1ralife gly, chlorine or amiph1su: be 0.05 - 0.3% by weight at 50-90 ° С.
    Determination of the number of Pbrozamip L-STVs is carried out by a gas ..) bromactus (1 |; - by the analytical method from chups nitela1ostyo to approximately OO, 1 pptii (0.1 mg / / kg),
    and R and; e r. M) i i {Hr.fi.nyp; - JiHf :. -. with the content - di-n - ;; rop 1.n}: and,) oaamana 58 ppm heated P c; h-i .; . from meiajiKoi i to BCi li, after which 0.1 g of p-toluenesulfok. –110 g; and stirred for 5 hours at the same time; -.-- hierature. Then the product og: -aup is cooled without stirring1) s, the p-toluene-sulfonic acid precipitating -5-t-s at the bottom of the reaction vessel, and triflural so cleaned in this way. investigate with the help of an indication--: -. method of gas chromatography of tea; maintenance of di-n-gropylnitrg. zpmin.- ;,. Laligz gives content lp1tro amine. 0,
    EXAMPLE 2. 50 g of i-guralin reef with di-n-propyl-grominamine content 58 ppm is heated before and after that 0.3 g of dsdeptitbenzene phosphate-acid is added. The mixture is further stirred for about 5 minutes and then refined for another 2 hours during the task :; This temperature is used for cooling and a sample is taken for analytical analysis; a combination of: nitrose min. A; talysis yields -71% {di-n-- -propapnitrosamine; 0.1 ppm;
    PRIMEME 3. 50 g of trifluralin containing di-n-pro 1I1 Chigroamip
    20
    25
    35
    4U
    four
    50
    55
    30 is treated with pgmo1 0.5 g butane; 1-hydrochloric acid according to the lazine method in example 1; Carcass 6 hr) a sample, for analytical (rtr-L penitenes of nitrosamine., - gives the content of di-n-propyl - nitrosamine, 3 ppm.
    ; i R and e R 4. 50 g -1 riflu1.alina with gshi holding di-n-propylnitrosamine 3L) -ipn; treated at 90 ° C with an additional 1- (1 0.3 g amidosulfung acid as indicated in the method described in Example 1. After 8 hours, npo6v is taken for anadical 1 P o determination; 1G:) MiiH, i. The analysis gives a content of 0.3 ppm di-n-ggro pilsam trozamine.
    11, and m e P J. 50 g of triflur- .lin g with a content of di-n-propylnitrosamine 53 pd- are treated at 70 ° C at: -11L; T; 0.2 g of chlorosulfonic acid IK is indicated and example I mets-do. After 3 h of the test, ana ;;; 13 ko-t:) rsch bark content l, and -n-propylnit-rgzl, miaa 0.1 ppm.
    I R ime R 6. 50 g of trifluralin with C () reagent, cation of di-n-propi-chnitrosamine ZE ppc is treated at 90 ° C. . After 6 h, a sample of r; l apality, ie, determination, is taken. The analysis gives the di-n-propylnite roamine - (1,2 rrp.
    Example. 50 g of isopropaline with g: (- | hold 1-1 lin n-prgiitlnitrosamine 15 ppm is treated at 70 ° C with Oj2 rn-oluol acid acids, similarly to Example 1. 3 h after treatment, the content of di-n- pyopylnitro; amine is -0,2 ppm. I
    EXAMPLE 8, 50 gt rifluralin containing di-n-propylnitrosamine 30) n processing - 1 wipe at 70 ° C with | LMO 1; and 0.2 p-toluenesul (L-acid but with the specified method 1 After 5 hours after treatment, the product is smolded with 50 v distillate and blended, stirred for 30 minutes at 50 ° C and added (1HL-t by means of) iiaTri J10 and 1HPI 8. Then set; th temperature eiue about vj min lpoi: s1 od. t mixing and incubated until ve. tichin), p1 8. After e. the aqueous phase and c) H work1-ann thrilluralin followed by i-a content and they J RM ichmina:, 1 ppm dn-pro 1, | 1nitrosamine in the base phase:
    i: 0.2 ppm di-n-propyl nitrosamine in treated trifluralin.
    EXAMPLE 9: Nitrosamine Cleavage and Stabilization Against Repeated Increase of Nitrosamine Thanks to Proposed Additives
    100 gtrifluralin containing 0.6 ppm of di-n-propyl nitrosamine is melted and the initial amount is divided in half. 0.3% by weight dodecylbenzenesulfonic acid was added to one half and then both samples were stored for 1 week at 70 ° C. Determination of a sample of di-n-propyl nitrosamine mixed with dodecyl benzene sulfoxy acid gives a content of 0.2 ppm di-n-propyl nitrosamine, while its content in the unstabilized sample is increased to 2.5 ppm.
    Thus, the proposed purification method for N, H-disubstituted nitroaromatic amines makes it possible to increase the purity and stabilize the target product against the formation of nitrosamines.
    权利要求:
    Claims (2)
    [1]
    1. Method of purification of N, N-nH3aMeD; eH-nitroaromatic amines of the general formula
    N02) g
    N0
    where R is CF, or CXCH,), by splitting the nitrosamine components due to their preparation by treating the product with an acid at about a temperature, characterized in that, in order to increase purity and stabilize the target product against nitrosamine re-formation, sulfonic acid the amount of 0.05-0.5% by weight of the amine and the process is carried out at 50-90 ° C,
    [2]
    2. A method according to claim 1, characterized in that aliphatic, aromatic, araliphatic chloro or amidosulfonic acid is used as sulphonic acid.
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    同族专利:
    公开号 | 公开日
    DE3345157A1|1985-06-27|
    DD231565A5|1986-01-02|
    BR8406389A|1985-10-08|
    EP0151725A3|1986-05-28|
    ZA849703B|1985-07-31|
    JPH0729996B2|1995-04-05|
    EP0151725B1|1988-03-02|
    AT32710T|1988-03-15|
    AU584316B2|1989-05-25|
    US4638090A|1987-01-20|
    IL73808D0|1985-03-31|
    EP0151725A2|1985-08-21|
    HU193723B|1987-11-30|
    IL73808A|1988-03-31|
    JPS60146851A|1985-08-02|
    HUT37115A|1985-11-28|
    KR920005378B1|1992-07-02|
    CA1256902A|1989-07-04|
    AU3665384A|1985-06-20|
    DE3469519D1|1988-04-07|
    KR850004577A|1985-07-25|
    引用文献:
    公开号 | 申请日 | 公开日 | 申请人 | 专利标题
    US4136117A|1973-06-25|1979-01-23|American Cyanamid Company|Preparation of 2,6-dinitroanilines|
    US4226789A|1977-07-18|1980-10-07|Eli Lilly And Company|Removal of nitrosamines from denitroanilines by treatment with HCl|
    RO75656A|1977-07-18|1981-04-20|Eli Lilly And Co,Us|PROCEDURE FOR THE PURIFICATION OF DYNITROANILINS|
    US4127610A|1977-08-17|1978-11-28|Eli Lilly And Company|Dinitroaniline purification with bromine and chlorine|
    US4185035A|1977-09-02|1980-01-22|Eli Lilly And Company|Dinitroaniline purification with inorganic acid halides|
    US4120905A|1977-09-21|1978-10-17|Eli Lilly And Company|Removal of nitrosating agents|
    JPH0113460B2|1980-08-25|1989-03-06|Nippon Kayaku Kk|IL78948A|1985-06-06|1991-03-10|Finchimica Srl|Process for purifying crude trifluralin|
    DE3785356T2|1987-12-29|1993-10-28|Finchimica Srl|Method of treating dinitroanilines to reduce their nitrosamine content and / or to stabilize them against the formation of nitrosamines.|
    AU594850B2|1987-12-29|1990-03-15|Finchimica S.P.A.|A method for the treatment of dinitroanilines to reduce their nitrosamine content and/or to stabilise them against the formation of nitrosamines|
    US5160530A|1989-01-24|1992-11-03|Griffin Corporation|Microencapsulated polymorphic agriculturally active material|
    US5196585A|1990-10-02|1993-03-23|Dowelanco|Process for treating dinitroanilines with sulfite to reduce impurities and to reduce the ability to produce nitrosamines|
    IT1261259B|1993-09-13|1996-05-09|Finchimica Srl|PROCEDURE FOR THE PREPARATION OF ETHALFLURALIN|
    US5728881A|1997-03-05|1998-03-17|Srm Chemical, Ltd. Co.|Process for preparing trifluralin|
    法律状态:
    优先权:
    申请号 | 申请日 | 专利标题
    DE19833345157|DE3345157A1|1983-12-14|1983-12-14|METHOD FOR PRODUCING NITROSAMINE-FREE N, N-DISUBSTITUTED NITROAROMATIC AMINES AND THEIR STABILIZATION AGAINST NITROSAMINE FORMATION|
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