CN105859561B - A kind of crystallization processes of the dinitrotoluene (DNT) crystal of needle-like 2,4 - Google Patents
A kind of crystallization processes of the dinitrotoluene (DNT) crystal of needle-like 2,4 Download PDFInfo
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- CN105859561B CN105859561B CN201610278578.2A CN201610278578A CN105859561B CN 105859561 B CN105859561 B CN 105859561B CN 201610278578 A CN201610278578 A CN 201610278578A CN 105859561 B CN105859561 B CN 105859561B
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- DYSXLQBUUOPLBB-UHFFFAOYSA-N 2,3-dinitrotoluene Chemical compound CC1=CC=CC([N+]([O-])=O)=C1[N+]([O-])=O DYSXLQBUUOPLBB-UHFFFAOYSA-N 0.000 title claims abstract description 79
- 239000013078 crystal Substances 0.000 title claims abstract description 54
- 238000002425 crystallisation Methods 0.000 title claims abstract description 47
- 230000008025 crystallization Effects 0.000 title claims abstract description 47
- 238000000034 method Methods 0.000 title claims abstract description 26
- RMBFBMJGBANMMK-UHFFFAOYSA-N 2,4-dinitrotoluene Chemical compound CC1=CC=C([N+]([O-])=O)C=C1[N+]([O-])=O RMBFBMJGBANMMK-UHFFFAOYSA-N 0.000 claims abstract description 64
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 31
- 238000003756 stirring Methods 0.000 claims abstract description 14
- 239000000839 emulsion Substances 0.000 claims abstract description 10
- 239000007788 liquid Substances 0.000 claims abstract description 10
- 239000007864 aqueous solution Substances 0.000 claims abstract description 8
- 239000007787 solid Substances 0.000 claims abstract description 4
- 238000000926 separation method Methods 0.000 claims abstract description 3
- 238000001035 drying Methods 0.000 claims description 14
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 12
- 238000003828 vacuum filtration Methods 0.000 claims description 2
- 230000015572 biosynthetic process Effects 0.000 abstract description 4
- 239000000047 product Substances 0.000 description 37
- 230000000052 comparative effect Effects 0.000 description 8
- 238000004519 manufacturing process Methods 0.000 description 8
- 239000000243 solution Substances 0.000 description 7
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 4
- 238000002844 melting Methods 0.000 description 4
- 230000008018 melting Effects 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000005755 formation reaction Methods 0.000 description 3
- 239000000543 intermediate Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000000634 powder X-ray diffraction Methods 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- 239000005864 Sulphur Substances 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 239000003905 agrochemical Substances 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 239000000975 dye Substances 0.000 description 2
- 238000000635 electron micrograph Methods 0.000 description 2
- 239000002360 explosive Substances 0.000 description 2
- 210000003739 neck Anatomy 0.000 description 2
- 229920002635 polyurethane Polymers 0.000 description 2
- 239000004814 polyurethane Substances 0.000 description 2
- 238000004886 process control Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000001953 recrystallisation Methods 0.000 description 2
- 238000007873 sieving Methods 0.000 description 2
- 229910052717 sulfur Inorganic materials 0.000 description 2
- 239000011593 sulfur Substances 0.000 description 2
- 238000009423 ventilation Methods 0.000 description 2
- XTRDKALNCIHHNI-UHFFFAOYSA-N 2,6-dinitrotoluene Chemical compound CC1=C([N+]([O-])=O)C=CC=C1[N+]([O-])=O XTRDKALNCIHHNI-UHFFFAOYSA-N 0.000 description 1
- ZPTVNYMJQHSSEA-UHFFFAOYSA-N 4-nitrotoluene Chemical compound CC1=CC=C([N+]([O-])=O)C=C1 ZPTVNYMJQHSSEA-UHFFFAOYSA-N 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 229920005830 Polyurethane Foam Polymers 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 238000003889 chemical engineering Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000012043 crude product Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 238000006396 nitration reaction Methods 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 230000001546 nitrifying effect Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000011496 polyurethane foam Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 1
- DVKJHBMWWAPEIU-UHFFFAOYSA-N toluene 2,4-diisocyanate Chemical compound CC1=CC=C(N=C=O)C=C1N=C=O DVKJHBMWWAPEIU-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C201/00—Preparation of esters of nitric or nitrous acid or of compounds containing nitro or nitroso groups bound to a carbon skeleton
- C07C201/06—Preparation of nitro compounds
- C07C201/16—Separation; Purification; Stabilisation; Use of additives
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07B—GENERAL METHODS OF ORGANIC CHEMISTRY; APPARATUS THEREFOR
- C07B2200/00—Indexing scheme relating to specific properties of organic compounds
- C07B2200/13—Crystalline forms, e.g. polymorphs
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a kind of crystallization processes of the dinitrotoluene (DNT) crystal of needle-like 2,4, comprise the following steps：A dissolves, and the dinitrotoluene (DNT) of molten state 2,4 is mixed with 70 DEG C~95 DEG C hot water, Temperature fall after stirring；B crystallizations, when 2, the 4 dinitrotoluene (DNT) aqueous solution are in emulsion form, cold water is added, separates out acicular crystal rapidly；Separation of solid and liquid is carried out after stirring, obtains 2,4 dinitrotoluene (DNT) wet products；C is dried, and 2,4 dinitrotoluene (DNT) wet products are dried to constant weight below 60 DEG C, after 1mm aperture sieves, produce the dinitrotoluene (DNT) crystal finished product of needle-like 2,4.Product of the present invention is the long and uniform dinitrotoluene (DNT) of needle-like 2,4 crystallization, and crystallization length reaches 3mm~5mm, and color is homogeneous faint yellow；Product purity is high, moisture is low, quality is good, and its crystal formation complies fully with application requirement of 2,4 dinitrotoluene (DNT)s in frontier.
Description
Technical field
The present invention relates to a kind of needle-like 2, the crystallization processes of 4- dinitrotoluene (DNT) crystal, belongs to Chemical Engineering crystallization technique neck
Domain.
Background technology
2,4- dinitrotoluene (DNT)s (2,4-DNT) are a kind of important organic chemical intermediates, are widely used in agricultural chemicals, dye
Material, medicine and other chemical industries.2,4-DNT can derive a series of obtained intermediates, for manufacturing Sulphur Yellow GC, sulphur yellow brown
The dyestuffs such as 5G, sulfur yellow brown 6g, sulfur red brown b3r, produce explosive TNT, prepared by production polyurethane foam plastics, polyurethane products
With intermediate 2,4 toluene diisocyanate etc..With the rapid development of fine chemistry industry, with dyestuff, medicine, agricultural chemicals, polyurethane material
Chemical products based on material etc. are continuously developed so that the purposes of 2,4-DNT is further developed and developed.
Traditional 2,4-DNT production methods are to nitrify to be made through nitration mixture (concentrated sulfuric acid and concentrated nitric acid) as raw material using toluene, institute
Obtain in product and include 2,4-DNT and 2,6-DNT is, it is necessary to further crystallize, isolate 2,4-DNT after purification；This method is made
2,4-DNT purity it is relatively low, only 96% or so, although product price is cheap, market application is few.In order to improve nitrification selection
Property, it is that raw material is nitrified under mixed acid system with para-nitrotoluene (p-MNT), more pure 2,4- dinitros can be obtained
Toluene, product purity reach more than 99%, and moisture is less than 0.25%, and fusing point is 68 DEG C~70 DEG C；Product purity high-quality is good, tool
There is the stronger market competitiveness.No matter using which kind of preparation method, 2,4-DNT be after washing is refined, by molten condition mostly
Directly cooling obtains, and product appearance is faint yellow sheet or needle-like solid, and crystallization situation is unstable, and crystal formation is also uneven.For example,
In the method that a kind of mixed acid nitrifying disclosed in Chinese patent CN104529785A prepares 2,4- dinitrotoluene (DNT)s, its step
3 separating, washing processes, liquid 2 of the cooling by washing, 4-DNT crude products to room temperature, make 2,4-DNT solidify out into faint yellow sheet
Or the solid-state 2,4-DNT of needle-like, and separated with cleaning solution.2, the 4-DNT products being prepared out, its crystallization process are entirely not
Controllable, a variety of crystal formations mix.
With the development of science and technology, 2,4-DNT have ample scope for abilities in new field, such as safe automobile air bag
Gas generator, for preparing Boeing air bag slide and as army's high-explosive bomb additive.In these new necks
Domain is in use, in order to obtain higher more controllable stability and security, it is desirable to and 2,4-DNT be uniform acicular crystal, and
Crystallizing length, the longer the better.In order to reach this purpose, many companies all are attempting to carry out Improvement.At present, only U.S.
IPI S. R. L. has gone out 2,4-DNT acicular crystals by solvent crystallization of methanol, and still, its length crystallized is only 0.5mm or so, and
And length is uneven, the requirement of frontier can not be met.
So far, it there is no open method to prepare needle-like 2 both at home and abroad, 4-DNT crystallizations, be that a technology urgently to be resolved hurrily is difficult
Topic.
The content of the invention
The technical problem to be solved in the invention is to provide a kind of crystallization processes 2 of needle-like 2,4-DNT crystal,
4- dinitrotoluene (DNT)s crystallize, and are easy to implement industrial-scale production.
In order to solve the above technical problems, the technical solution used in the present invention is：
A kind of needle-like 2, the crystallization processes of 4- dinitrotoluene (DNT) crystal, comprises the following steps：
A, dissolve
By molten state 2,4- dinitrotoluene (DNT)s are mixed with 70 DEG C~95 DEG C hot water, Temperature fall after stirring；
B, crystallization
When 2, the 4- dinitrotoluene (DNT)s aqueous solution is in emulsion form, cold water is added, separates out acicular crystal rapidly；Carried out after stirring
Separation of solid and liquid, obtain 2,4- dinitrotoluene (DNT) wet products；
C, drying
2,4- dinitrotoluene (DNT)s wet product is dried to constant weight below 60 DEG C, after 1mm aperture sieves, produces needle-like 2,4- bis-
Nitrotoleune crystal finished product.
The molten state 2, the volume of 4- dinitrotoluene (DNT)s is 400 parts, and the volume of dissolving hot water is 500~800 parts,
The volume of crystallization cold water is 100~200 parts；The temperature of dissolving hot water is 75~85 DEG C, and crystallization is normal-temperature water with cold water,
Preferably 10~30 DEG C.
In the step A, rotating speed during dissolving is controlled in 60r/min~80r/min.The specific control method of rotating speed is：
When 2,4- dinitrotoluene (DNT) aqueous temperatures are down to 69 DEG C~70 DEG C, adjustment of rotational speed to 85r/min~110r/
min；When 2,4- dinitrotoluene (DNT) aqueous temperatures are down to 67 DEG C~68 DEG C, in emulsion form when, faster rotational speed to 120r/min with
On.
Preferably, when 2,4- dinitrotoluene (DNT) aqueous temperatures are down to 69 DEG C~70 DEG C, adjustment of rotational speed to 90r/min~
100r/min；When 2,4- dinitrotoluene (DNT) aqueous temperatures are down to 67 DEG C~68 DEG C, in emulsion form when, faster rotational speed to 120r/
Min~150r/min.
In the step B, for cold water feed postition to add or disposably adding by several times, solid-liquid separating method is vacuum filtration
Or centrifuge dripping.
In the step B, when cold water disposably adds, to the mixing center of 2, the 4- dinitrotoluene (DNT) aqueous solution at incline
Enter.
In the step C, needle-like 2,4- dinitrotoluene (DNT)s crystal is dried using standing mode, and drying process forbids rocking.
The needle-like 2, the length of 4- dinitrotoluene (DNT)s crystallization is 3mm~5mm, and fusing point is 67.5~70.5 DEG C；Along crystallization
Thing longitudinal direction is not less than 95% by the percent of pass of 1mm aperture sieves.
By adopting the above-described technical solution, the technological progress acquired by the present invention is：
(1) crystallization processes of the present invention control crystallization by the addition of appropriate cold water, obtain length using water as recrystallisation solvent
And uniform needle-like 2, the crystallization of 4- dinitrotoluene (DNT)s, crystallization length reach 3mm~5mm, color is homogeneous faint yellow；Product
Purity is not less than 99%, and moisture and volatile matter content are less than 0.25%, and fusing point is 68 DEG C~70 DEG C, and purity is high, quality is good, and it is brilliant
Type complies fully with application requirement of the 2,4-DNT in frontier.
(2) present invention process is simple to operation, and controllability is strong, the use of equipment is mostly conventional equipment, without putting into excessive money
Gold, production cost is low, high income, product purity are high, is especially suitable for industrial-scale production.
(3) for the present invention using water as recrystallisation solvent, whole crystallization process is very environmentally friendly completely without using organic solvent；And
And crystallization temperature is controlled below 100 DEG C, potential safety hazard very little.
Brief description of the drawings
Fig. 1 is the X-ray powder diffraction collection of crystal made from the inventive method；
Fig. 2 and Fig. 3 is the electron micrograph that crystal made from the inventive method amplifies 100 times；
Fig. 4 and Fig. 5 is the electron micrograph that IPI S. R. L. of u s company crystal amplifies 100 times.
Embodiment
The present invention is described in further details with reference to embodiment and accompanying drawing：
Embodiment 1
A kind of needle-like 2, the crystallization of 4- dinitrotoluene (DNT) crystal, is prepared using following steps：
A, dissolve
By 400ml molten states 2,4- dinitrotoluene (DNT)s are mixed with 80 DEG C of hot water 600ml, dropped naturally after stirring
Temperature；Rotating speed control is dissolved in 80r/min.When 2,4- dinitrotoluene (DNT) aqueous temperatures are down to 69 DEG C~70 DEG C, rotating speed is carried
Height arrives 90r/min.
B, crystallization
When 2, the 4- dinitrotoluene (DNT) aqueous solution continue to be cooled to 67 DEG C~68 DEG C, now solution becomes emulsion form, rapidly will
Faster rotational speed is poured at Solutions Center to 120r/min, while by the cold water that 150ml temperature is 25 DEG C；There is acicular crystal analysis rapidly
Go out, liquid becomes limpid at once.Filtered after stirring a moment, obtain 2,4- dinitrotoluene (DNT) wet products.
C, drying
2,4- dinitrotoluene (DNT) wet products are rested on dry platform, dries at 50 DEG C~60 DEG C to constant weight, is protected when drying
Hold ventilation, dry platform and avoid overheat, in order to avoid melting.Gained 2,4-DNT dry product passes through along crystal longitudinal direction
1mm apertures standard screen, produce flaxen needle-like 2,4- dinitrotoluene (DNT) crystal finished products.
Embodiment 2
A kind of needle-like 2, the crystallization of 4- dinitrotoluene (DNT) crystal, is prepared using following steps：
A, dissolve
By 400ml molten states 2,4- dinitrotoluene (DNT)s are mixed with 75 DEG C of hot water 800ml, dropped naturally after stirring
Temperature；Rotating speed control is dissolved in 70r/min.When 2,4- dinitrotoluene (DNT) aqueous temperatures are down to 69 DEG C~70 DEG C, rotating speed is carried
Height arrives 95r/min.
B, crystallization
When 2, the 4- dinitrotoluene (DNT) aqueous solution continue to be cooled to 67 DEG C~68 DEG C, now solution is slightly thick, becomes emulsion form, fast
Faster rotational speed is poured at Solutions Center by speed to 130r/min, while by the cold water that 200ml temperature is 20 DEG C；There is needle-like knot rapidly
Partial crystallization goes out, and liquid becomes limpid at once.Filtered after stirring a moment, obtain 2,4- dinitrotoluene (DNT) wet products.
C, drying
2,4- dinitrotoluene (DNT) wet products are rested on dry platform, dries at 50 DEG C~60 DEG C to constant weight, is opened when drying
Open air exhauster, and dry platform and avoid overheat, in order to avoid melting.Gained 2,4-DNT dry product leads to along crystal longitudinal direction
1mm apertures standard screen is crossed, produces flaxen needle-like 2,4- dinitrotoluene (DNT) crystal finished products.
Embodiment 3
A kind of needle-like 2, the crystallization of 4- dinitrotoluene (DNT) crystal, is prepared using following steps：
A, dissolve
By 400ml molten states 2,4- dinitrotoluene (DNT)s are mixed with 85 DEG C of hot water 500ml, dropped naturally after stirring
Temperature；Rotating speed control is dissolved in 60r/min.When 2,4- dinitrotoluene (DNT) aqueous temperatures are down to 69 DEG C~70 DEG C, rotating speed is carried
Height arrives 90r/min.
B, crystallization
When 2, the 4- dinitrotoluene (DNT) aqueous solution continue to be cooled to 67 DEG C~68 DEG C, now solution becomes emulsion form, rapidly will
Faster rotational speed is poured at Solutions Center to 125r/min, while by the cold water that 100ml temperature is 30 DEG C；There is acicular crystal analysis rapidly
Go out, liquid becomes limpid at once.Centrifuge dripping is carried out after stirring a moment, obtains 2,4- dinitrotoluene (DNT) wet products.
Centrifuge dripping process control rotating speed and drying time, to avoid damage to crystal.
C, drying
2,4- dinitrotoluene (DNT) wet products are rested on dry platform, dries at 50 DEG C~60 DEG C to constant weight, is protected when drying
Hold ventilation, dry platform and avoid overheat, in order to avoid melting.Gained 2,4-DNT dry product passes through along crystal longitudinal direction
1mm apertures standard screen, produce flaxen needle-like 2,4- dinitrotoluene (DNT) crystal finished products.
Embodiment 4
A kind of needle-like 2, the crystallization of 4- dinitrotoluene (DNT) crystal, is prepared using following steps：
A, dissolve
By 400ml molten states 2,4- dinitrotoluene (DNT)s are mixed with 80 DEG C of hot water 700ml, dropped naturally after stirring
Temperature；Rotating speed control is dissolved in 75r/min.When 2,4- dinitrotoluene (DNT) aqueous temperatures are down to 69 DEG C~70 DEG C, rotating speed is carried
Height arrives 100r/min.
B, crystallization
When 2, the 4- dinitrotoluene (DNT) aqueous solution continue to be cooled to 67 DEG C~68 DEG C, now solution becomes emulsion form, rapidly will
Faster rotational speed is gradually dropped to 140r/min, while by the cold water that 150ml temperature is 20 DEG C；With the instillation of cold water, have rapidly
Acicular crystal separates out, and liquid becomes limpid at once.Centrifuge dripping is carried out after stirring a moment, obtains 2,4- dinitrotoluene (DNT) wet products.
Centrifuge dripping process control rotating speed and drying time, to avoid damage to crystal.
C, drying
2,4- dinitrotoluene (DNT) wet products are rested on dry platform, dries at 50 DEG C~60 DEG C to constant weight, is opened when drying
Open air exhauster, take steam away at any time, dry platform avoid overheat, so as not to melting.Gained 2,4-DNT dry product is along crystallization
Thing longitudinal direction produces flaxen needle-like 2,4- dinitrotoluene (DNT) crystal finished products by Unite States Standard 1mm aperture sieves.
Comparative example 1
2,4- dinitrotoluene (DNT)s are prepared using the method disclosed in embodiment 1 in Chinese patent CN104529785A, as
Comparative example 1.The product is faint yellow, is flaky crystal and the mixture of acicular crystal.
Comparative example 2
Using the 2,4-DNT crystal as a comparison case 2 of IPI S. R. L. of U.S. production.The product of comparative example 2 is yellowish
Color acicular crystal, crystallization length are appreciably shorter.
2,4-DNT product obtained by 1~embodiment of Example 4,1~comparative example of comparative example 2 carries out performance
Test.Test result is shown in Table 1.
The 2,4-DNT properties of product test data table of table 1
During sieving, the acicular crystal part of the product of comparative example 1 can by sieve aperture, but flaky crystal particle diameter compared with
Greatly, sieve aperture can not be passed through；The crystal of the product of comparative example 2 is short and small, in powdered, is all flowed out by sieve aperture.And product of the present invention
Crystallinity is high, crystal formation is good, crystallization length, and crystal length is between 3.5mm~5mm, uniformity, sieving percent of pass reach 95% with
On, comply fully with the requirement that 2,4- dinitrotoluene (DNT)s are applied in frontier.
Product of the present invention is subjected to X-ray powder diffraction detection, detection parameters are as follows：
Instrument：The X-ray powder diffraction instrument of German Brooker AXS companies production, INSTRUMENT MODEL D8ADVANCE；
Operating voltage：40kV, operating current：40mA；
Sweep speed：0.02°/0.3s；Scanning range：5~50 °.
X-ray diffraction data see the table below, and X-ray diffraction spectrogram is shown in Fig. 1.
Claims (6)
1. a kind of needle-like 2, the crystallization processes of 4- dinitrotoluene (DNT) crystal, it is characterised in that comprise the following steps：
A, dissolve
By molten state 2,4- dinitrotoluene (DNT)s are mixed with 70 DEG C ~ 95 DEG C of hot water, Temperature fall after stirring；
B, crystallization
When 2,4- dinitrotoluene (DNT) aqueous temperatures are down to 69 DEG C ~ 70 DEG C, adjustment of rotational speed to 85r/min ~ 110r/min；When
2,4- dinitrotoluene (DNT) aqueous temperatures are down to 67 DEG C ~ 68 DEG C, in emulsion form when, faster rotational speed to more than 120r/min, add
Cold water, acicular crystal is separated out rapidly；Separation of solid and liquid is carried out after stirring, obtains 2,4- dinitrotoluene (DNT) wet products；
C, drying
2,4- dinitrotoluene (DNT)s wet product is dried to constant weight below 60 DEG C, after 1mm aperture sieves, produces needle-like 2,4- dinitros
Toluene crystal finished product；
The molten state 2, the volume of 4- dinitrotoluene (DNT)s is 400 parts, and the volume of dissolving hot water is 500 ~ 800 parts, crystallization
It it is 100 ~ 200 parts with the volume of cold water；Crystallization is normal-temperature water with cold water；
The needle-like 2, the length of 4- dinitrotoluene (DNT)s crystallization is 3mm ~ 5mm, and fusing point is 67.5 ~ 70.5 DEG C；Along crystal longitudinal direction
Direction is not less than 95% by the percent of pass of 1mm aperture sieves.
2. a kind of needle-like 2 according to claim 1, the crystallization processes of 4- dinitrotoluene (DNT) crystal, it is characterised in that：It is described
In step A, rotating speed during dissolving is controlled in 60r/min ~ 80r/min.
3. a kind of needle-like 2 according to claim 1, the crystallization processes of 4- dinitrotoluene (DNT) crystal, it is characterised in that：When 2,
When 4- dinitrotoluene (DNT) aqueous temperatures are down to 69 DEG C ~ 70 DEG C, adjustment of rotational speed to 90r/min ~ 100r/min；When 2,4- dinitros
Toluene aqueous temperature is down to 67 DEG C ~ 68 DEG C, in emulsion form when, faster rotational speed to 120r/min ~ 150r/min.
4. a kind of needle-like 2 according to claim 1, the crystallization processes of 4- dinitrotoluene (DNT) crystal, it is characterised in that：It is described
In step B, for cold water feed postition to add or disposably adding by several times, solid-liquid separating method is vacuum filtration or centrifuge dripping.
5. a kind of needle-like 2 according to claim 4, the crystallization processes of 4- dinitrotoluene (DNT) crystal, it is characterised in that：It is described
In step B, when cold water disposably adds, to the mixing center of 2, the 4- dinitrotoluene (DNT) aqueous solution at be poured into.
6. a kind of needle-like 2 according to claim 1, the crystallization processes of 4- dinitrotoluene (DNT) crystal, it is characterised in that：It is described
In step C, needle-like 2,4- dinitrotoluene (DNT)s crystal is dried using standing mode, and drying process forbids rocking.
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| CN201610278578.2A CN105859561B (en) | 2016-04-28 | 2016-04-28 | A kind of crystallization processes of the dinitrotoluene (DNT) crystal of needle-like 2,4 |
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| CN100434414C (en) * | 2006-12-31 | 2008-11-19 | 河南大学 | Utilizing process of nitrobenzene distilation redsdue |
| CN105001093A (en) * | 2015-07-01 | 2015-10-28 | 南京理工大学 | Method for purifying hexanitrostibene |
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Effective date of registration: 20180712 Address after: 052260 eight Li Zhuang village, ten Zhuang Town, Jinzhou City, Shijiazhuang, Hebei Patentee after: Shijiazhuang Bao Yuan automobile material Co., Ltd. Address before: 052260 Chaoyang Garden C4, Chaoyang Road, Jinzhou, Shijiazhuang, Hebei. Patentee before: Liu Gengli |
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