CN105859561A - Crystallization process of needle-like 2,4-dinitrotoluene crystals - Google Patents
Crystallization process of needle-like 2,4-dinitrotoluene crystals Download PDFInfo
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- CN105859561A CN105859561A CN201610278578.2A CN201610278578A CN105859561A CN 105859561 A CN105859561 A CN 105859561A CN 201610278578 A CN201610278578 A CN 201610278578A CN 105859561 A CN105859561 A CN 105859561A
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- RMBFBMJGBANMMK-UHFFFAOYSA-N 2,4-dinitrotoluene Chemical compound CC1=CC=C([N+]([O-])=O)C=C1[N+]([O-])=O RMBFBMJGBANMMK-UHFFFAOYSA-N 0.000 title claims abstract description 66
- 239000013078 crystal Substances 0.000 title claims abstract description 59
- 238000002425 crystallisation Methods 0.000 title claims abstract description 40
- 230000008025 crystallization Effects 0.000 title claims abstract description 40
- 238000000034 method Methods 0.000 title claims abstract description 31
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 33
- 238000003756 stirring Methods 0.000 claims abstract description 14
- 239000000839 emulsion Substances 0.000 claims abstract description 11
- 239000007788 liquid Substances 0.000 claims abstract description 10
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 9
- 239000007864 aqueous solution Substances 0.000 claims description 8
- 238000003828 vacuum filtration Methods 0.000 claims description 2
- 238000001035 drying Methods 0.000 abstract description 5
- 238000001816 cooling Methods 0.000 abstract description 3
- 238000000926 separation method Methods 0.000 abstract description 2
- 239000000047 product Substances 0.000 description 37
- 230000000052 comparative effect Effects 0.000 description 8
- 238000004519 manufacturing process Methods 0.000 description 6
- 239000000243 solution Substances 0.000 description 5
- 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
- 230000015572 biosynthetic process Effects 0.000 description 3
- 238000005516 engineering process 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
- 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
- 238000004458 analytical method 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
- 238000001914 filtration Methods 0.000 description 2
- 210000003739 neck Anatomy 0.000 description 2
- 239000000575 pesticide Substances 0.000 description 2
- 229920002635 polyurethane Polymers 0.000 description 2
- 239000004814 polyurethane Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000000634 powder X-ray diffraction Methods 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
- 229910052717 sulfur Inorganic materials 0.000 description 2
- 239000011593 sulfur Substances 0.000 description 2
- 238000009423 ventilation Methods 0.000 description 2
- BBUPBICWUURTNP-UHFFFAOYSA-N 2,4-dimethyl-1-nitrobenzene Chemical compound CC1=CC=C([N+]([O-])=O)C(C)=C1 BBUPBICWUURTNP-UHFFFAOYSA-N 0.000 description 1
- 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
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 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
- 230000007613 environmental effect Effects 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
- 238000007873 sieving Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 235000011149 sulphuric acid Nutrition 0.000 description 1
- 239000001117 sulphuric acid Substances 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 crystallization process of needle-like 2,4-dinitrotoluene crystals. The crystallization process comprises the following steps of A, dissolving, wherein molten 2,4-dinitrotoluene and hot water at the temperature of 70 DEG C to 95 DEG C are mixed, and natural cooling is carried out after even stirring; B, crystallization, wherein when the 2,4-dinitrotoluene water solution is in an emulsion shape, cold water is added, needle-like crystals are separated out fast, solid-liquid separation is carried out after stirring, and wet 2,4-dinitrotoluene is obtained; C, drying, wherein wet 2,4-dinitrotoluene is dried to constant weight at the temperature below 60 DEG C and passes through a sieve with the aperture of 1 mm, and the finished needle-like 2,4-dinitrotoluene crystals are obtained. The products are long and even needle-like 2,4-dinitrotoluene crystals, the crystal length reaches 3 mm to 5 mm, and the color is uniform faint yellow. The product is high in purity, low in moisture and good in quality, and the crystal form completely meets the application requirement of 2,4-dinitrotoluene in the new field.
Description
Technical field
The present invention relates to a kind of needle-like 2, the crystallization processes of 4-dinitrotoluene (DNT) crystal, belong to Chemical Engineering crystallization technique neck
Territory.
Background technology
2,4-dinitrotoluene (DNT)s (2,4-DNT) are a kind of important organic chemical intermediates, are widely used in pesticide, dye
Material, medicine and other chemical industries.2,4-DNT can derive prepared a series of intermediate, are used 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..Along with developing rapidly of fine chemistry industry, with dyestuff, medicine, pesticide, polyurethane material
The chemical products that material etc. is main are continuously developed the purposes so that 2,4-DNT and are further developed and develop.
Traditional 2,4-DNT production method is to prepare through nitration mixture (concentrated sulphuric acid and concentrated nitric acid) nitrification with toluene for raw material, institute
Obtain and product includes 2,4-DNT and 2,6-DNT, after needing crystallization further, purification, isolate 2,4-DNT；The method prepares
2,4-DNT purity is relatively low, only about 96%, although product price is cheap, but market application is few.Select to improve nitrification
Property, it is that raw material carries out nitrification under mixed acid system with para-nitrotoluene (p-MNT), it is possible to obtain the purest 2,4-dinitro
Toluene, product purity reaches 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 higher market competitiveness.No matter using which kind of preparation method, 2,4-DNT is mostly after washing is refined, by molten condition
Directly cooling obtains, and product appearance is faint yellow lamellar or needle-like solid, and crystallization situation is unstable, and crystal formation is the most uneven.Such as,
2, in the method for 4-dinitrotoluene (DNT), its step are prepared at a kind of mixed acid nitrifying disclosed in Chinese patent CN104529785A
3 separating, washing processes, cooling is through the liquid 2 of washing, and 4-DNT crude product, to room temperature, makes 2,4-DNT solidify out into faint yellow lamellar
Or the solid-state 2,4-DNT of needle-like, and separate with cleaning mixture.2 be prepared out, 4-DNT product, its crystallization process is entirely not
Controlled, multiple crystal formation mixes.
Along with the development of science and technology, 2,4-DNT have had ample scope for abilities in new field, such as safe automobile air bag
Gas generator, it is used for preparing Boeing air bag slide and is used as army's high-explosive bomb additive.At these new necks
When territory uses, in order to obtain the highest more controlled stability and safety, it is desirable to 2,4-DNT is uniform acicular crystal, and
The longer the better for crystallization length.In order to reach this purpose, many companies all carry out Improvement in trial.At present, only U.S.
IPI S. R. L. has gone out 2 with methanol for solvent crystallization, 4-DNT acicular crystal, but, length of its crystallization is only about 0.5mm, and
And length is uneven, it is impossible to meet the use requirement of frontier.
Up to now, there is no open method both at home and abroad and prepare needle-like 2,4-DNT crystallizes, and is that a technology urgently to be resolved hurrily is difficult
Topic.
Summary of the invention
The technical issues that need to address of the present invention are to provide the crystallization processes 2 of a kind of needle-like 2,4-DNT crystal,
4-dinitrotoluene (DNT) crystallizes, and facilitates implementation industrial-scale production.
For solving above-mentioned technical problem, the technical solution used in the present invention is:
A kind of needle-like 2, the crystallization processes of 4-dinitrotoluene (DNT) crystal, comprise the following steps:
A, dissolving
Molten state 2,4-dinitrotoluene (DNT) and 70 DEG C～95 DEG C of hot water are mixed, Temperature fall after stirring；
B, crystallize
When 2, when 4-dinitrotoluene (DNT) aqueous solution is emulsion form, adds cold water, separate out rapidly acicular crystal；Carry out after stirring
Solid-liquid separation, it is thus achieved that 2,4-dinitrotoluene (DNT) wet products；
C, be dried
By 2,4-dinitrotoluene (DNT) wet product is dried to constant weight below 60 DEG C, after 1mm aperture sieve, obtains needle-like 2,4-bis-
Methylnitrobenzene crystal finished product.
Described molten state 2, the volume of 4-dinitrotoluene (DNT) is 400 parts, and the volume of dissolving hot water is 500～800 parts,
The volume of crystallize cold water is 100～200 parts；The temperature of dissolving hot water is 75～85 DEG C, and crystallize cold water is normal-temperature water,
It is preferably 10～30 DEG C.
In described step A, rotating speed during dissolving controls at 60r/min～80r/min.The concrete control method of rotating speed is:
When 2, when 4-dinitrotoluene (DNT) aqueous temperature is down to 69 DEG C～70 DEG C, adjustment of rotational speed to 85r/min～110r/
min；When 2,4-dinitrotoluene (DNT) aqueous temperature is down to 67 DEG C～68 DEG C, in emulsion form time, faster rotational speed to 120r/min with
On.
Be preferably, when 2, when 4-dinitrotoluene (DNT) aqueous temperature is down to 69 DEG C～70 DEG C, adjustment of rotational speed to 90r/min～
100r/min；When 2,4-dinitrotoluene (DNT) aqueous temperature is down to 67 DEG C～68 DEG C, in emulsion form time, faster rotational speed to 120r/
Min～150r/min.
In described step B, cold water feed postition is for adding by several times or disposably adding, and solid-liquid separating method is vacuum filtration
Or centrifuge dripping.
In described step B, when cold water disposably adds fashionable, to 2, incline at the mixing center of 4-dinitrotoluene (DNT) aqueous solution
Enter.
In described step C, needle-like 2,4-dinitrotoluene (DNT) crystal uses standing mode to be dried, and dry run forbids rocking.
Described needle-like 2, a length of 3mm～5mm of 4-dinitrotoluene (DNT) crystallization, 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 sieve.
Owing to have employed technique scheme, the technological progress acquired by the present invention is:
(1) crystallization processes of the present invention is with water as recrystallisation solvent, controls crystallization by the addition of appropriate cold water, it is thus achieved that long
And uniform needle-like 2,4-dinitrotoluene (DNT) crystallizes, and crystallization length all reaches 3mm～5mm, and 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 the 2,4-DNT application requirement in frontier.
(2) present invention process is simple to operation, and controllability is strong, and use equipment mostly is conventional equipment, it is not necessary to put into too much money
Gold, production cost is low, yield is high, product purity is high, is especially suitable for industrial-scale production.
(3) present invention is using water as recrystallisation solvent, and whole crystallization process does not the most use organic solvent, very environmental protection；And
And crystallization temperature controls below 100 DEG C, potential safety hazard is the least.
Accompanying drawing explanation
Fig. 1 is the X-ray powder diffraction spectrum of the crystal that the inventive method prepares；
Fig. 2 and Fig. 3 is the electron micrograph that the crystal that the inventive method prepares amplifies 100 times；
IPI S. R. L. of Fig. 4 and Tu5Shi u s company crystal amplifies the electron micrograph of 100 times.
Detailed description of the invention
Below in conjunction with embodiment and accompanying drawing, the present invention is described in further details:
Embodiment 1
A kind of needle-like 2, the crystallization of 4-dinitrotoluene (DNT) crystal, use following steps to prepare:
A, dissolving
400ml molten state 2,4-dinitrotoluene (DNT) and 80 DEG C of hot water 600ml are mixed, naturally drops after stirring
Temperature；Dissolve rotating speed to control at 80r/min.When 2, when 4-dinitrotoluene (DNT) aqueous temperature is down to 69 DEG C～70 DEG C, rotating speed is carried
High to 90r/min.
B, crystallize
When 2,4-dinitrotoluene (DNT) aqueous solutions continue to be cooled to 67 DEG C～68 DEG C, now solution becomes emulsion form, rapidly will
The cold water that 150ml temperature is 25 DEG C, to 120r/min, is poured at Solutions Center by faster rotational speed simultaneously；Acicular crystal is had rapidly to analyse
Going out, liquid becomes limpid at once.Stirring carries out sucking filtration in a moment, obtains 2,4-dinitrotoluene (DNT) wet product.
C, be dried
By 2,4-dinitrotoluene (DNT) wet product rests on dry platform, is dried to constant weight at 50 DEG C～60 DEG C, protects when being dried
Holding ventilation, dry platform is avoided overheated in order to avoid melting.Gained 2,4-DNT dry product passes through along crystal longitudinal direction
1mm aperture standard screen, obtains flaxen needle-like 2,4-dinitrotoluene (DNT) crystal finished product.
Embodiment 2
A kind of needle-like 2, the crystallization of 4-dinitrotoluene (DNT) crystal, use following steps to prepare:
A, dissolving
400ml molten state 2,4-dinitrotoluene (DNT) and 75 DEG C of hot water 800ml are mixed, naturally drops after stirring
Temperature；Dissolve rotating speed to control at 70r/min.When 2, when 4-dinitrotoluene (DNT) aqueous temperature is down to 69 DEG C～70 DEG C, rotating speed is carried
High to 95r/min.
B, crystallize
When 2,4-dinitrotoluene (DNT) aqueous solutions continue to be cooled to 67 DEG C～68 DEG C, now solution is the thickest, become emulsion form, fast
The cold water that 200ml temperature is 20 DEG C, by faster rotational speed to 130r/min, is poured at Solutions Center by speed simultaneously；Needle-like is had rapidly to tie
Partial crystallization goes out, and liquid becomes limpid at once.Stirring carries out sucking filtration in a moment, obtains 2,4-dinitrotoluene (DNT) wet product.
C, be dried
By 2,4-dinitrotoluene (DNT) wet product rests on dry platform, is dried to constant weight, opens time dry at 50 DEG C～60 DEG C
Open air exhauster, and dry platform is avoided overheated in order to avoid melting.Gained 2,4-DNT dry product leads to along crystal longitudinal direction
Cross 1mm aperture standard screen, obtain flaxen needle-like 2,4-dinitrotoluene (DNT) crystal finished product.
Embodiment 3
A kind of needle-like 2, the crystallization of 4-dinitrotoluene (DNT) crystal, use following steps to prepare:
A, dissolving
400ml molten state 2,4-dinitrotoluene (DNT) and 85 DEG C of hot water 500ml are mixed, naturally drops after stirring
Temperature；Dissolve rotating speed to control at 60r/min.When 2, when 4-dinitrotoluene (DNT) aqueous temperature is down to 69 DEG C～70 DEG C, rotating speed is carried
High to 90r/min.
B, crystallize
When 2,4-dinitrotoluene (DNT) aqueous solutions continue to be cooled to 67 DEG C～68 DEG C, now solution becomes emulsion form, rapidly will
The cold water that 100ml temperature is 30 DEG C, to 125r/min, is poured at Solutions Center by faster rotational speed simultaneously；Acicular crystal is had rapidly to analyse
Going out, liquid becomes limpid at once.Stirring is centrifuged drying in a moment, obtains 2,4-dinitrotoluene (DNT) wet product.
Centrifuge dripping process control rotating speed and the time of drying, to avoid damage to crystal.
C, be dried
By 2,4-dinitrotoluene (DNT) wet product rests on dry platform, is dried to constant weight at 50 DEG C～60 DEG C, protects when being dried
Holding ventilation, dry platform is avoided overheated in order to avoid melting.Gained 2,4-DNT dry product passes through along crystal longitudinal direction
1mm aperture standard screen, obtains flaxen needle-like 2,4-dinitrotoluene (DNT) crystal finished product.
Embodiment 4
A kind of needle-like 2, the crystallization of 4-dinitrotoluene (DNT) crystal, use following steps to prepare:
A, dissolving
400ml molten state 2,4-dinitrotoluene (DNT) and 80 DEG C of hot water 700ml are mixed, naturally drops after stirring
Temperature；Dissolve rotating speed to control at 75r/min.When 2, when 4-dinitrotoluene (DNT) aqueous temperature is down to 69 DEG C～70 DEG C, rotating speed is carried
High to 100r/min.
B, crystallize
When 2,4-dinitrotoluene (DNT) aqueous solutions continue to be cooled to 67 DEG C～68 DEG C, now solution becomes emulsion form, rapidly will
The cold water that 150ml temperature is 20 DEG C, to 140r/min, is gradually dropped by faster rotational speed simultaneously；Along with the instillation of cold water, have rapidly
Acicular crystal separates out, and liquid becomes limpid at once.Stirring is centrifuged drying in a moment, obtains 2,4-dinitrotoluene (DNT) wet product.
Centrifuge dripping process control rotating speed and the time of drying, to avoid damage to crystal.
C, be dried
By 2,4-dinitrotoluene (DNT) wet product rests on dry platform, is dried to constant weight, opens time dry at 50 DEG C～60 DEG C
Opening air exhauster, take steam away at any time, dry platform is avoided overheated in order to avoid melting.Gained 2,4-DNT dry product is along crystallization
Thing longitudinal direction passes through Unite States Standard 1mm aperture sieve, obtains flaxen needle-like 2,4-dinitrotoluene (DNT) crystal finished product.
Comparative example 1
The method disclosed in embodiment 1 is used in Chinese patent CN104529785A to prepare 2,4-dinitrotoluene (DNT), as
Comparative example 1.This product is faint yellow, is the mixture of flaky crystal and acicular crystal.
Comparative example 2
Use the 2,4-DNT crystal as a comparison case 2 that American I PI Corp. produces.Comparative example 2 product is yellowish
Color acicular crystal, crystallization length is appreciably shorter.
Example 1～embodiment 4, comparative example 1～the 2,4-DNT product obtained by comparative example 2 carry out performance
Test.Test result is shown in Table 1.
Table 1 2,4-DNT properties of product test tables of data
During sieving, the acicular crystal part of comparative example 1 product can pass through sieve aperture, but flaky crystal particle diameter is relatively
Greatly, it is impossible to pass through sieve aperture；The crystal of comparative example 2 product is short and small, in powder, is all flowed out by sieve aperture.And product of the present invention
Degree of crystallinity is high, crystal formation is good, crystallization is long, crystal length between 3.5mm～5mm, uniformity, the percent of pass that sieves reach 95% with
On, comply fully with 2, the requirement that 4-dinitrotoluene (DNT) is applied in frontier.
Product of the present invention carries out X-ray powder diffraction detection, and detection parameter is as follows:
Instrument: the X-ray powder diffractometer that Brooker AXS company of Germany produces, INSTRUMENT MODEL D8ADVANCE；
Running voltage: 40kV, operating current: 40mA；
Scanning speed: 0.02 °/0.3s；Sweep limits: 5～50 °.
X-ray diffraction data see table, and X-ray diffraction spectrogram is shown in Fig. 1.
Claims (9)
1. a needle-like 2, the crystallization processes of 4-dinitrotoluene (DNT) crystal, it is characterised in that comprise the following steps:
A, dissolving
By molten state 2, the hot water of 4-dinitrotoluene (DNT) and 70 DEG C～95 DEG C mixes, Temperature fall after stirring；
B, crystallize
When 2, when 4-dinitrotoluene (DNT) aqueous solution is emulsion form, adds cold water, separate out rapidly acicular crystal；Solid-liquid is carried out after stirring
Separate, it is thus achieved that 2,4-dinitrotoluene (DNT) wet products；
C, be dried
By 2,4-dinitrotoluene (DNT) wet product is dried to constant weight below 60 DEG C, after 1mm aperture sieve, obtains needle-like 2,4-dinitro
Toluene crystal finished product.
A kind of needle-like 2 the most according to claim 1, the crystallization processes of 4-dinitrotoluene (DNT) crystal, it is characterised in that: described
Molten state 2, the volume of 4-dinitrotoluene (DNT) is 400 parts, and the volume of dissolving hot water is 500～800 parts, crystallize cold water
Volume is 100～200 parts；The temperature of dissolving hot water is 75～85 DEG C, and crystallize cold water is normal-temperature water.
A kind of needle-like 2 the most according to claim 2, the crystallization processes of 4-dinitrotoluene (DNT) crystal, it is characterised in that: described
In step A, rotating speed during dissolving controls at 60r/min～80r/min.
A kind of needle-like 2 the most according to claim 3, the crystallization processes of 4-dinitrotoluene (DNT) crystal, it is characterised in that: when 2,
When 4-dinitrotoluene (DNT) aqueous temperature is down to 69 DEG C～70 DEG C, adjustment of rotational speed to 85r/min～110r/min；When 2,4-dinitro
Base toluene aqueous temperature is down to 67 DEG C～68 DEG C, in emulsion form time, faster rotational speed to more than 120r/min.
A kind of needle-like 2 the most according to claim 4, the crystallization processes of 4-dinitrotoluene (DNT) crystal, it is characterised in that: when 2,
When 4-dinitrotoluene (DNT) aqueous temperature is down to 69 DEG C～70 DEG C, adjustment of rotational speed to 90r/min～100r/min；When 2,4-dinitro
Base toluene aqueous temperature is down to 67 DEG C～68 DEG C, in emulsion form time, faster rotational speed to 120r/min～150r/min.
A kind of needle-like 2 the most according to claim 2, the crystallization processes of 4-dinitrotoluene (DNT) crystal, it is characterised in that: described
In step B, cold water feed postition is for adding by several times or disposably adding, and solid-liquid separating method is vacuum filtration or centrifuge dripping.
A kind of needle-like 2 the most according to claim 6, the crystallization processes of 4-dinitrotoluene (DNT) crystal, it is characterised in that: described
In step B, when cold water disposably adds fashionable, to 2, it is poured at the mixing center of 4-dinitrotoluene (DNT) aqueous solution.
A kind of needle-like 2 the most according to claim 2, the crystallization processes of 4-dinitrotoluene (DNT) crystal, it is characterised in that: described
In step C, needle-like 2,4-dinitrotoluene (DNT) crystal uses standing mode to be dried, and dry run forbids rocking.
A kind of needle-like 2 the most according to claim 2, the crystallization processes of 4-dinitrotoluene (DNT) crystal, it is characterised in that: described
Needle-like 2, a length of 3mm～5mm of 4-dinitrotoluene (DNT) crystallization, fusing point is 67.5～70.5 DEG C；Lead to along crystal longitudinal direction
The percent of pass crossing 1mm aperture sieve is not less than 95%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| 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 |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| 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 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105859561A true CN105859561A (en) | 2016-08-17 |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100999472A (en) * | 2006-12-31 | 2007-07-18 | 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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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100999472A (en) * | 2006-12-31 | 2007-07-18 | 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 |
Non-Patent Citations (1)
| Title |
|---|
| JAGARLAPUDI A. R. P. SARMA ET AL.: "Solid state nuclear bromination with N-bromosuccinimide. Part 1. Experimental and theoretical studies on some substituted aniline, phenol and nitro aromatic compounds", 《J. CHEM. SOC., PERKIN TRANS.》 * |
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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 |