Method of purifying dinitroanilines

专利摘要:
The present invention is directed to a process for the removal of nitrosamines from dinitroanilines.
公开号:SU747418A3
申请号:SU782647710
申请日:1978-08-16
公开日:1980-07-23
发明作者:Фрэнк Эйзембер Ричард
申请人:Эли Лилли Энд Компани (Фирма)；
IPC主号:

专利说明:

the presence of 10 g of the mixture.
PRI me R 3. Removal of nitroz. Min from 4-fluoromethyl - 2, 6-dinitro-g; d-n-propylaniline.
30 g of the mixture containing 4-fluoroethyl-2, b-dinitro-N, M-di PropyleneLIN and nitrosamine (14 h, nitroammon per 10 g of the mixture) are heated to EO-S, the start is 0.1 g of bromine and the reaction 1: They are mixed with stirring for 30 μC. After the reaction with an E-iyio mixture, the mixture is washed with 5 ml of a 10% sodium hydroxide thief. The organic layer is isolated and analyzed to determine the nitrosamine content. The analysis shows the presence of 1.4 g of nitrozamine iO mixture, the aqueous layer is extracted with 5 ml of methylene chloride; A sample of the extract is analyzed to determine the nitrosamine content. Bottom line indicates the presence of O, .15 μg / l nitrosamine
Example 4. 27 g of a mixture of 4 fluoromethyl-2, b-divi-cis-b, M-di-b: -propylene aniline with nitroamine (1750 g of the latter on the mixture) are heated at and added 0.2 g of bromine. Reaction mixture bind at 70 ° C with a 55 m / n EEA-RI stirring, VoRem Pos; the last 10 microns above the surface-with purge air. After this, the sample and analyzer are collected to determine the content of n; -: g of roses at / and -; The assay shows the presence of 12 grams of cytosamine on the mixture.
Example 5, 100 g of civiecH C-fluoromethyl-2, b-dinitro - g -; - din-propanolaniline with nitrosine amine (68 HMTposaivD-iHa per 10 g) are picked up at about 70 ° C and then O., 2 g of erms. The reaction is maintained at 70 ° C with stirring for 2 Periodically samples are taken, which are analyzed to determine:
Get the following; whose results;
Time Concentration
nctrosamine,
5 min3, 2
15 to
30 min
1h14
2h27
; Another test J selected-1 on the march 2 H; e. analyzed for; Cr: dividing 4-fluoromethyl-2, 6-, and; in1ch; grs dIH - propylanilic method, lo: ha. by bone chromatography, Established that its degree of purity is 97.2% of cocTaBJw.
PRI me R 6 „30: g of a mixture of 4 fsrmethyl - 2, b-dinitro-N, if-di-and-propylaniline with ointments (keeping the last 68; g pa
rpejsaiOT jvc 7 О С
add 5th 3-1; I. bromo, the reaction mixture is crystallized at 7 ° C at + 11 ° C in:: AP IV, HH,, reaction Icb temcate. was observed Obrazovanie a certain amount of CLEAR polymeric material. Tests of vaccine on soy, gerzh: -she nitrosis: and degree. H - Punctures 4 - fluoromethyl-, - 6 - dinitro-N; -; 1i-n-propylaniline and 1 trose L | -5n was not detected. Degree {stoti 82,5% ,,
with the exception
that for one is; ., use1; O, 5 ып} ОН1; -entered
and a dl of another is hydrochloric acid .. 0.5 ml of HOURNESS; In Kp aoya service
4-fluoromethyl-- 2
V (68 g
per 10 g) add 3 i-liter of water and COOT hydrofluoric acid, bold with; keep the mixture under stirring for 2 ° C min. After that, Pa 3 fj, e; i and t are layers. Acidic; The lamination layer is not traced and extracted with a diluted volume of methylene chloride; a, Samples of the product and the extract in methylene chloride, are used to determine the content of the cytoreamine, Obtaining. Here are the results listed in the table.
PRI me R 8. 30 g of a mixture of 4 fluoride; 5L-2, b-dinitro-N, N-di-n-propylaniline with nitrosamino: -; (63 g 1o ;; le,: -, it is heated by 10 g); io. Gaseous x, ENT bubbled 3 4-fluoromethyl-2, b-dinitro-N, N-di-n-iropylaniline at a rate of about 35 ml / min; 30 hectares, after icrobot; air for the next 5 min. B for the whole ii; oro time 4 - fluoromethyl - 2, b-di-P1Tro - K, M di-n-propylaniline you, lehr 1 Screw at 70 ° С, Sample is analyzed and analysis shows the presence of 16 g of iprosa and tla on 10g of the mixture.
Example 9. 1 ml WATER and 30 g of a mixture of 4-fluoromethyl-2,6-dinitro H, N-di-n-propylaniline with nitrosamine (68 g of the last on) are mixed and heated to. Chlorine gas is bubbled into the mixture at a rate of about. 35 ml / min for 30 min, after which air is bubbled for 10 min. The reaction mixture was kept at 90 ° C. The sample is analyzed and the analysis shows the filling of 13 g of nitrosamine on the mixture.
Example 10. 30 g of a mixture of 4-fluoromethyl-2, b-dinitro-N, N-di-n-propylaniline with nitrosamine (68 g of the latter on) are heated and kept at. Then 2 MP of 10% sodium carbonate solution are added and chlorine is bubbled at a rate of 15 ml / min. Samples are taken periodically, layers are separated in each sample and the product layer is analyzed for nitrosamine content. Get the following results:
Concentration
Time
nitrosamine,
30 min15
1h28
2 p1,2
Example 11. 30 g of a mixture of 4-fluoromethyl-2, b-dinitro-N, N-di-n-propylaniline with nitrosamine (68 g of the latter on) are heated to 70 ° C and then 0.5 g of N-bromosuccinimide is added. The reaction mixture was kept at 70 ° C for 30 minutes. The sample analyzed: the content of nitrosamine is 1.7 g per mixture.
Example 12. 30 g of a mixture of 4-fluoromethyl-2, b-dinitro-N, N-di-n-propylaniline with nitrosamine (68 g of the latter per) are melted and washing with 15 ml of 5% sodium carbonate solution. The layers are separated, to
0.1 g of bromine is added to the organic layer at 7 ° C and the mixture is blended at this temperature for 30 ms. The sample is analyzed for nitrosamine content. This connection was not detected.

权利要求:
Claims (1)
[1]
1. Vorozhtsov N.N. Basics of synthesis of intermediate products and dyes. M.-L., I960 ,, p. 521.

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同族专利:

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引用文献:

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DE377859C|1923-06-28|Anton Neidl|Scythe ring|

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US3317606A|1963-05-21|1967-05-02|Lummus Co|Process for separating vicinal and nonvicinal toluene diamines|IL67948A|1983-02-18|1988-05-31|Agan Chemical Manufacturers|Method for removal of nitrosoamine impurities from herbicides|

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DE3345157A1|1983-12-14|1985-06-27|Hoechst Ag, 6230 Frankfurt|METHOD FOR PRODUCING NITROSAMINE-FREE N, N-DISUBSTITUTED NITROAROMATIC AMINES AND THEIR STABILIZATION AGAINST NITROSAMINE FORMATION|

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IT1190440B|1985-12-18|1988-02-16|Finchimica Spa|IMPROVED PROCEDURE FOR PURIFYING TRIFLURALINE|

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IL79248A|1986-06-26|1990-07-12|Agan Chemical Manufacturers|Process for purifying dinitroaniline herbicides|

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US4876388A|1986-07-31|1989-10-24|IΠCI. S.p.A.|Method for the purification of trifuraline|

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US5510534A|1995-01-04|1996-04-23|Atanor S.A.|Process for reducing the nitrosamine content of herbicides|

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US5728881A|1997-03-05|1998-03-17|Srm Chemical, Ltd. Co.|Process for preparing trifluralin|

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US5922915A|1998-05-11|1999-07-13|Srm Chemical, Ltd., Co.|Process for removing N-nitroso compounds from organo-amine compositions including dinitroaniline herbicides|

法律状态:

优先权:

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申请号 | 申请日 | 专利标题

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US82534577A| true| 1977-08-17|1977-08-17|

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