A method for producing high purity 2,4-dinitro
Synthesis of the method according to claim I, further
chlorobenzene, wherein: achieved by the following process
steps:. A mixed sulfuric nitric acid into the nitration reactor,
followed by dropwise addition of p-nitrochlorobenzene,
uniform stirring, the reaction temperature was controlled at
65~ 70. . . B. After the addition was complete
nitrochlorobenzene, the nitration reactor temperature was
raised to 105 ° C to maintain 2~2. 5 hours, stirring was
stopped, the stationary delamination. c. Place the spent acid
fraction was extracted into the pot, and extracted After
completion of the addition of organic matter on the spent acid
nitrochlorobenzene reacted with the remaining nitric acid
extraction to extraction pot. The extraction temperature is
controlled at 70~75 ° C, d. After completion of the static
extraction layered, the input waste acid concentration
section, after applying concentrated, recovered
nitrochlorobenzene as a batch nitration the feed after
extraction. e. Insert the nitrification reactor into nitrate
solution passing separated and washed with water pan, into
the third volume of the nitrate solution and a temperature of
70~ 75 ° C hot water, adding the washing to neutral Na2C03
· 10H20. f. Stop stirring, static hierarchical give 2,4-
nitrochlorobenzene qualified to enter the tank, storage.
Synthesis of dinitrochlorobenzene.
1. A method of synthesis of dinitro chlorobenzene, reaction was
carried out in a micro reactor with two inlets and one outlet,
characterized in that: 1) In a mixed acid of nitric acid and
sulfuric acid nitrating agent, nitration agent mass ratio of
sulfuric acid and nitric acid, i.e., η / s is O. I~O 5, containing
less than nitrating agent IOwt%;. 2) mixing the acid and
reaction mass the material flowing through the bifurcated
chlorophenyl synchronization delivered by metering pump to
the micro two inlet channels of the reactor, controlling the
molar ratio of nitric acid to 1.6~2.4 and chlorobenzene; 3) two
feeds liquid contact in a microchannel reactor, the reaction
and after mixing, flows from the outlet of the reactor into
separator; liquid hourly space velocity LHSV of microchannel
reactor is 500~SOOOtr1; 4) the reaction product was
separated out in the separator, the aqueous phase and the
organic phase was separated, the aqueous phase and
recovering the nitrated products, the organic product was
washed , dried, purified by crystallization to give
dinitrochlorobenzene; the microchannel reactor comprises
two closure plates and a microchannel plate; microchannel
plate positioned at least three microchannels, i.e., at least two
inlet passages, respectively, and at least one inlet connected
to the reaction channel through ; Two inlet channels
respectively connected to the inlet, and an outlet connected to
the reaction channel; and at least one inlet passage and at a
side of the reaction gang microchannel plate.
2. The synthesis method according to claim I, wherein: the
mass ratio of the nitrating agent is nitric acid and sulfuric O.
I~O 3, a water content less than or equal 5wt%; molar nitric
acid and chlorobenzene ratio of 2. O~2 4;. The reaction
temperature is room temperature to 130. . .
3. The method of synthesis according to claim I, wherein:
corresponds to the reaction pressure of the reactor liquid
hourly space velocity range is O. I~O 2MPa..
4.
comprising: a high purity process dinitrochlorobenzene
aqueous phase from the product recovery of dissolved, the
organic phase mass of the product was recovered organic
product ratio is generally I: 10~20; reusable product after
separation and purification of water by means of a
conventional method and apparatus for phase was
concentrated, purified and concentrated spent acid.
The synthesis method according to claim I, wherein: when the
product allowing nitrochlorobenzene containing a mass
concentration of 20% or less and the ratio of raw material
may be, I) mixed acid n / s is O .. I~O 3, a water content IOwt%
or less, the molar ratio of nitric acid and chlorobenzene I. 6~2
O;.. or 2) mixed acid n / s is O. 3~O 5, IOwt% or less water
content, molar ratio of nitric acid and chlorobenzene 2. O~2.
4.
Preparation of 1-
chloro-2,4-
dinitrobenzene
100 g of chlorobenzene are added drop by
drop to a mixture of 160 g of nitric
acid (d=1.50 g/ml) and 340 g of sulfuric
acid (d=1.84 g/ml) while the mixture is
stirred mechanically. The temperature rises
because of the heat of the reaction, but is not
allowed to go above 50-55° C. After all
the chlorobenzene has been added, the
temperature is raised slowly to 95° C and is
kept there for 2 hours longer while the
stirring is continued. The upper layer of
light yellow liquid solidifies when cold. It is
removed, broken up under water, and
rinsed. The spent acid, on dilution with
water, precipitates an additional quantity of
1-chloro-2,4-dinitrobenzene. All the product
is brought together, washed with cold water,
then several times with hot water while it is
melted, and finally once more with cold
water under which it is crushed. Then it is
drained and allowed to dry at ordinary
temperature. The product, melting at about
50° C, consists largely of 1-chloro-2,4-
dinitrobenzene, m.p. 53.4° C, along with a
small quantity of the 2,6-dinitro compound,
m.p. 87-88° C.
Chemistry of Powder and Explosives, by T.
L. Davis, 135, 1941