CN110668954A - Preparation method of 2, 4-dinitroaniline - Google Patents
Preparation method of 2, 4-dinitroaniline Download PDFInfo
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- CN110668954A CN110668954A CN201910904206.XA CN201910904206A CN110668954A CN 110668954 A CN110668954 A CN 110668954A CN 201910904206 A CN201910904206 A CN 201910904206A CN 110668954 A CN110668954 A CN 110668954A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C209/00—Preparation of compounds containing amino groups bound to a carbon skeleton
- C07C209/04—Preparation of compounds containing amino groups bound to a carbon skeleton by substitution of functional groups by amino groups
- C07C209/06—Preparation of compounds containing amino groups bound to a carbon skeleton by substitution of functional groups by amino groups by substitution of halogen atoms
- C07C209/10—Preparation of compounds containing amino groups bound to a carbon skeleton by substitution of functional groups by amino groups by substitution of halogen atoms with formation of amino groups bound to carbon atoms of six-membered aromatic rings or from amines having nitrogen atoms bound to carbon atoms of six-membered aromatic rings
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B65—CONVEYING; PACKING; STORING; HANDLING THIN OR FILAMENTARY MATERIAL
- B65D—CONTAINERS FOR STORAGE OR TRANSPORT OF ARTICLES OR MATERIALS, e.g. BAGS, BARRELS, BOTTLES, BOXES, CANS, CARTONS, CRATES, DRUMS, JARS, TANKS, HOPPERS, FORWARDING CONTAINERS; ACCESSORIES, CLOSURES, OR FITTINGS THEREFOR; PACKAGING ELEMENTS; PACKAGES
- B65D25/00—Details of other kinds or types of rigid or semi-rigid containers
- B65D25/02—Internal fittings
- B65D25/10—Devices to locate articles in containers
- B65D25/106—Elements projecting into a recess or through a hole in the articles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B65—CONVEYING; PACKING; STORING; HANDLING THIN OR FILAMENTARY MATERIAL
- B65D—CONTAINERS FOR STORAGE OR TRANSPORT OF ARTICLES OR MATERIALS, e.g. BAGS, BARRELS, BOTTLES, BOXES, CANS, CARTONS, CRATES, DRUMS, JARS, TANKS, HOPPERS, FORWARDING CONTAINERS; ACCESSORIES, CLOSURES, OR FITTINGS THEREFOR; PACKAGING ELEMENTS; PACKAGES
- B65D81/00—Containers, packaging elements, or packages, for contents presenting particular transport or storage problems, or adapted to be used for non-packaging purposes after removal of contents
- B65D81/18—Containers, packaging elements, or packages, for contents presenting particular transport or storage problems, or adapted to be used for non-packaging purposes after removal of contents providing specific environment for contents, e.g. temperature above or below ambient
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B65—CONVEYING; PACKING; STORING; HANDLING THIN OR FILAMENTARY MATERIAL
- B65D—CONTAINERS FOR STORAGE OR TRANSPORT OF ARTICLES OR MATERIALS, e.g. BAGS, BARRELS, BOTTLES, BOXES, CANS, CARTONS, CRATES, DRUMS, JARS, TANKS, HOPPERS, FORWARDING CONTAINERS; ACCESSORIES, CLOSURES, OR FITTINGS THEREFOR; PACKAGING ELEMENTS; PACKAGES
- B65D85/00—Containers, packaging elements or packages, specially adapted for particular articles or materials
- B65D85/30—Containers, packaging elements or packages, specially adapted for particular articles or materials for articles particularly sensitive to damage by shock or pressure
- B65D85/302—Containers, packaging elements or packages, specially adapted for particular articles or materials for articles particularly sensitive to damage by shock or pressure for carboys
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- Mechanical Engineering (AREA)
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- Organic Chemistry (AREA)
- Medical Preparation Storing Or Oral Administration Devices (AREA)
Abstract
The invention discloses a preparation method of 2, 4-dinitroaniline, which comprises the following specific steps: using formamide or acetamide as solvent, making the weight ratio of 2, 4-dinitrochlorobenzene and formamide or acetamide be 1: 1-10, blowing ammonia gas for 1.5-2.5 hours, after continuing reaction for 0.5 hour, cooling the obtained reaction mixture, separating to obtain 2, 4-dinitroaniline, and then collecting the 2, 4-dinitroaniline in a storage tank for storage.
Description
Technical Field
The invention belongs to the technical field of chemicals, and particularly relates to a preparation method of 2, 4-dinitroaniline.
Background
2, 4-dinitroaniline is a chemical substance with the molecular formula of C6H5N3O 4. Yellow needle-shaped crystals; insoluble in water, slightly soluble in ethanol, soluble in hot hydrochloric acid; relative density (water ═ 1) 1.62; relative density (air ═ 1) 6.31; the property is stable; toxic and harmful substances; mainly used as azo dye intermediate, corrosion inhibitor and analytical reagent.
At present, 2, 4-dinitroaniline is generally collected in a mode of bottling and the like, a plurality of bottled 2, 4-dinitroanilines have the problem of inconvenient movement, are easy to collide and damage due to foreign objects when placed, and cause damage to the internal 2, 4-dinitroaniline, and the existing storage device has single function and low practicability.
Disclosure of Invention
The invention provides a method for preparing 2, 4-dinitroaniline, aiming at overcoming the defects of the prior art.
In order to achieve the purpose, the invention adopts the following technical scheme: a preparation method of 2, 4-dinitroaniline comprises the following specific steps: using formamide or acetamide as a solvent, leading the weight ratio of 2, 4-dinitrochlorobenzene to formamide or acetamide to be 1: 1-10, blowing ammonia gas for 1.5-2.5 hours, cooling and separating the obtained reaction mixture after continuing to react for 0.5 hour to obtain 2, 4-dinitroaniline, and collecting the 2, 4-dinitroaniline in a storage tank for storage;
the storage box comprises a box body and a box cover, one end of the box cover is rotatably connected to the side wall of the box body, a material carrying plate is arranged in the box body, the material carrying plate and the inner wall of the box body form a first cavity, and clear water is filled in the first cavity; the bottom of the box body is provided with a first connecting block, the first connecting block is provided with a first connecting groove, and the bottom of the material carrying plate is provided with a first connecting ring matched with the connecting groove; a plurality of material loading grooves are formed in the material loading plate, and medicament bottles are inserted into the material loading grooves; the 2, 4-dinitroaniline is placed in a reagent bottle after being prepared, then the reagent bottle is placed in a material carrying groove, clean water is injected into the first cavity, the whole first cavity is filled with the clean water, the clean water is directly contacted with the material carrying plate, a box cover is covered, and the packaging treatment of the 2, 4-dinitroaniline is completed.
The storage box is always in a room temperature state by injecting clear water into the first cavity, so that a suitable temperature environment is provided for the storage of the 2, 4-dinitroaniline, and the storage of the 2, 4-dinitroaniline is facilitated; under the mutual matching of the material loading groove and the medicament bottle, the medicament bottle is fixed, so that the medicament bottle is prevented from moving in the storage box when the storage box is collided, and the 2, 4-dinitroaniline is prevented from falling out due to the crushing of the medicament bottle; under the mutual cooperation of first connecting groove and first connecting ring, promote the connection effect of year flitch and box, increase the leakproofness of first cavity simultaneously, prevent that the rivers from spilling from first cavity to 2, 4-dinitroaniline provides the low temperature storage environment under the clear water effect.
The solvent is formamide.
The weight ratio of the 2, 4-dinitrochlorobenzene to formamide or acetamide is 1: 3.
And pouring the cooled reaction mixture into water, and separating or directly filtering the cooled reaction mixture by suction to obtain a filter cake as a product.
And the filtrate obtained by suction filtration is used as a reaction solvent for recycling.
A first movable groove is formed in the side wall of the material carrying groove, a fixed ring is arranged in the material carrying groove, a movable block matched with the first movable groove is arranged on the side wall of the fixed ring, a fixed spring is arranged on the side wall of the movable block, and a first push plate is rotatably connected in the first movable groove; the medicament bottle comprises an upper bottle body and a lower bottle body, and the diameter of the upper bottle body is smaller than that of the lower bottle body; when a medicament bottle is placed into the storage tank, the bottom end of the medicament bottle is in contact with the first push plate, the medicament bottle pushes one end of the first push plate to move downwards, so that the first push plate rotates around the connecting point, the first push plate pushes the movable block to move towards the first movable groove, the movable block drives the fixing ring to move towards the side wall of the material carrying groove, after the bottom end of the lower bottle body moves to one side of the fixing ring, the first push plate is in an inclined state again under the pushing of the lower bottle body, so that the first push plate at one end of the material carrying groove inclines downwards, the fixing spring pushes the movable block to move towards the outer side of the first movable groove, and the fixing ring clamps the medicament bottle; when the medicament bottle is taken out of the material carrying groove, the top end of the lower bottle body is contacted with one end of the first push plate in the material carrying groove, the lower bottle body pushes the first push plate to rotate around a connecting point along with the taking-out of the medicament bottle, so that one end of the first push plate in the material carrying groove is inclined upwards again, and the resetting action of the first push plate is completed; the fixing spring provides thrust for the fixing ring, so that the fixing ring generates a trend of moving towards the middle of the material carrying groove, the medicament bottle is fixed in the material carrying groove after being placed in the material carrying groove, the matching effect of the medicament bottle and the material carrying groove is increased, and the 2, 4-dinitroaniline in the medicament bottle is well protected; under the mutual matching of the first push plate and the medicament bottle, the medicament bottle pushes the fixing ring to the inner wall of the material carrying groove when being in contact with the fixing ring, the distance between the fixing rings is increased, so that the medicament bottle can be directly placed on one side of the fixing ring, and the problem that the fixing ring obstructs the placement of the medicament bottle is avoided; through the setting of the different diameters of bottle about the medicament bottle to promote first push pedal and rotate toward not equidirectional under the effect of medicament bottle, need not unnecessary action and can accomplish the fixed of medicament bottle and the reseing of first push pedal, make the use of bin more convenient.
A second connecting block is arranged on the side wall of the box cover, a second movable groove is arranged on the second connecting block, a fixed plate is arranged on one side of the second connecting block, a second push plate matched with the second movable groove is arranged on the side wall of the fixed plate, a third push plate is arranged at one end of the fixed plate, a limiting groove is arranged on the fixed plate, a third connecting block is arranged on the side wall of the box body, and a limiting block matched with the limiting groove is arranged on the third connecting block; a limiting spring is arranged on the inner wall of the second movable groove, and a pressing plate is arranged at one end of the limiting spring; after the medicament bottle is placed into the material carrying groove, the box cover is covered on the box body, the third push plate is pushed along the second movable groove, the third push plate pushes the fixed plate to move downwards, the fixed plate moves to one side of the limiting block, the limiting block is embedded into the limiting groove, and the limiting block fixes the fixed plate so as to seal the storage box; when the storage box is opened to collect the medicament bottles, the second push plate is pushed to the top of the second movable groove, so that the second push plate drives the fixing plate to move away from the limiting block, the limiting block is separated from the limiting groove, and the box cover is directly opened to collect the medicament bottles; under the mutual matching of the limiting block and the limiting groove, the box cover and the box body are fixed together, so that the storage box forms a closed space, and the protection effect on the medicament bottle is improved; the pressing plate provides pressure for the second push plate, and the second push plate is pressed at the bottom of the second movable groove, so that the second push plate can stably move in the second movable groove, and the matching effect of the limiting block and the limiting groove is ensured; the limiting block is separated from the limiting groove by pushing the second push plate, so that the box cover can be easily opened from the box body, the medicine bottles can be collected more conveniently, and the use convenience of the storage box is improved.
The invention has the following advantages: the storage box is always in a room temperature state by injecting clear water into the first cavity, so that a suitable temperature environment is provided for the storage of the 2, 4-dinitroaniline, and the storage of the 2, 4-dinitroaniline is facilitated; under the mutually supporting of year feed chute and medicament bottle, play the fixed action to the medicament bottle, the medicament bottle removes in the bin when avoiding the bin to bump, avoids the broken 2, 4-dinitroaniline that makes of medicament bottle to fall out.
Drawings
Fig. 1 is a schematic view showing the structure of the storage box of the present invention.
Fig. 2 is a first cross-sectional view of the storage box of the present invention.
Fig. 3 is a second sectional view of the storage box of the present invention.
Fig. 4 is an enlarged view of a portion a in fig. 3.
Fig. 5 is an enlarged view of fig. 3 at B.
Fig. 6 is a third sectional view of the storage box of the present invention.
Fig. 7 is an enlarged view of fig. 6 at C.
Fig. 8 is a fourth sectional view of the storage box of the present invention.
Fig. 9 is an enlarged view of fig. 8 at D.
Fig. 10 is a schematic sectional view of the storage box of the present invention.
Fig. 11 is an enlarged view of fig. 10 at E.
Fig. 12 is an enlarged view of fig. 10 at F.
Detailed Description
Example 1:
a preparation method of 2, 4-dinitroaniline comprises the following specific steps: using formamide or acetamide as a solvent, leading the weight ratio of 2, 4-dinitrochlorobenzene to formamide or acetamide to be 1: 1, blowing ammonia gas for 1.5 hours, cooling and separating the obtained reaction mixture after continuing to react for 0.5 hour to obtain 2, 4-dinitroaniline, and collecting the 2, 4-dinitroaniline in a storage tank for storage; the solvent is formamide; the weight ratio of the 2, 4-dinitrochlorobenzene to formamide or acetamide is 1: 3; pouring the cooled reaction mixture into water, separating or directly filtering the cooled reaction mixture by suction, wherein a filter cake is a product; and the filtrate obtained by suction filtration is used as a reaction solvent for recycling.
As shown in fig. 1-12, the storage box includes a box body 1 and a box cover 2, a handle 11 is provided on a side wall of the box body, one end of the box cover 2 is rotatably connected to the side wall of the box body 1, a material carrying plate 12 is provided in the box body 1, the material carrying plate 12 and an inner wall of the box body 1 form a first cavity, the first cavity is filled with clear water, and the clear water is preferably well water; a first connecting block 13 is arranged at the bottom of the box body 1, a first connecting groove is formed in the first connecting block 13, and a first connecting ring 127 matched with the first connecting groove is arranged at the bottom of the material carrying plate 12; a plurality of material loading grooves are formed in the material loading plate 12, and the medicament bottles 3 are inserted into the material loading grooves; the 2, 4-dinitroaniline is placed in a reagent bottle 3 after being prepared, then the reagent bottle 3 is placed in a material loading groove, clean water is injected into the first cavity, the whole first cavity is filled with the clean water, the clean water is directly contacted with a material loading plate 12, a box cover 2 is covered, and the packing treatment of the 2, 4-dinitroaniline is completed.
The storage box is always in a room temperature state by injecting clear water into the first cavity, so that a suitable temperature environment is provided for the storage of the 2, 4-dinitroaniline, and the storage of the 2, 4-dinitroaniline is facilitated; under the mutual matching of the material loading groove and the medicament bottle, the medicament bottle is fixed, so that the medicament bottle is prevented from moving in the storage box when the storage box is collided, and the 2, 4-dinitroaniline is prevented from falling out due to the crushing of the medicament bottle; under the mutual cooperation of first connecting groove and first connecting ring, promote the connection effect of year flitch and box, increase the leakproofness of first cavity simultaneously, prevent that the rivers from spilling from first cavity to 2, 4-dinitroaniline provides the low temperature storage environment under the clear water effect.
A first water inlet is formed in the side wall of the box body, a first sealing plug is arranged in the first water inlet, a third movable groove is formed in the side wall of the box body, a first sliding groove is formed in the inner wall of the third movable groove, and a first baffle is arranged in the first sliding groove; clear water enters the first cavity through the first water inlet to complete the water injection operation of the first cavity; play sealed effect to first water inlet under the effect of first sealing plug, prevent that the rivers from leaking from first water inlet department, first baffle removes to first sealing plug one side, for first sealing plug provides the holding power, prevents that water pressure from pushing out first sealing plug from first water inlet department, promotes the sealed effect of first sealing plug to first water inlet.
The first connecting block is provided with a first connecting hole, the material carrying plate is provided with a second connecting hole matched with the first connecting hole, a fixing bolt penetrates through the second connecting hole, and the material carrying plate is fixed in the box body through the fixing bolt; when the inner wall of the box body is cleaned, the fixing bolt is rotated out of the second connecting hole, so that the material carrying plate is separated from the box body to be in contact with the box body, clean water is poured out of the box body to clean the inner wall of the box body, and the using sanitary condition of the storage box is improved; the bottom of the material carrying plate is provided with the groove, the thickness of the material carrying plate is reduced under the arrangement of the groove, so that the cooling effect of water flow on the material carrying plate is more obvious, and the storage effect of the 2, 4-dinitroaniline is improved.
A first movable groove is formed in the side wall of the material carrying groove, a fixed ring 121 is arranged in the material carrying groove, a movable block 122 matched with the first movable groove is arranged on the side wall of the fixed ring 121, a fixed spring 123 is arranged on the side wall of the movable block 122, and a first push plate 126 is rotatably connected in the first movable groove; the medicament bottle 3 comprises an upper bottle body and a lower bottle body, and the diameter of the upper bottle body is smaller than that of the lower bottle body; when the medicine bottle 3 is placed into the storage trough, the bottom end of the medicine bottle 3 is in contact with the first push plate 126, the medicine bottle 3 pushes one end of the first push plate 126 to move downwards, so that the first push plate 126 rotates around a connecting point, the first push plate 126 pushes the movable block 122 to move towards the first movable trough, the movable block 122 drives the fixed ring 121 to move towards the side wall of the material carrying trough, after the bottom end of the lower bottle body moves to one side of the fixed ring 121, the first push plate 126 is in an inclined state again under the pushing of the lower bottle body, so that the first push plate 126 at one end of the material carrying trough inclines downwards, the fixed spring 123 pushes the movable block 122 to move towards the outer side of the first movable trough, and the fixed ring 121 tightly clamps the medicine bottle 3; when the medicine bottle 3 is taken out of the material carrying groove, the top end of the lower bottle body is contacted with one end of the first push plate 126 in the material carrying groove, the lower bottle body pushes the first push plate 126 to rotate around a connecting point along with the extraction of the medicine bottle 3, so that one end of the first push plate 126 in the material carrying groove is inclined upwards again, and the resetting action of the first push plate 126 is completed; the fixing spring provides thrust for the fixing ring, so that the fixing ring generates a trend of moving towards the middle of the material carrying groove, the medicament bottle is fixed in the material carrying groove after being placed in the material carrying groove, the matching effect of the medicament bottle and the material carrying groove is increased, and the 2, 4-dinitroaniline in the medicament bottle is well protected; under the mutual matching of the first push plate and the medicament bottle, the medicament bottle pushes the fixing ring to the inner wall of the material carrying groove when being in contact with the fixing ring, the distance between the fixing rings is increased, so that the medicament bottle can be directly placed on one side of the fixing ring, and the problem that the fixing ring obstructs the placement of the medicament bottle is avoided; through the setting of the different diameters of bottle about the medicament bottle to promote first push pedal and rotate toward not equidirectional under the effect of medicament bottle, need not unnecessary action and can accomplish the fixed of medicament bottle and the reseing of first push pedal, make the use of bin more convenient.
A sleeve 124 is arranged on the inner wall of the first movable groove, a connecting rod 125 penetrates through the lantern ring, one end of the connecting rod is fixedly connected to the side wall of the fixed ring, and under the mutual matching of the sleeve and the connecting rod, the movement of the fixed ring is positioned, so that the fixed ring moves on a straight line, and the matching effect of the fixed ring and the medicament bottle is ensured; the medicament bottle top is equipped with apron 31, and the apron passes through threaded connection on the medicament bottle, is equipped with fourth push pedal 32 on the medicament bottle, and after the medicament bottle was arranged in and is carried the silo, the fourth push pedal was in and carries the silo top, provides the impetus for the medicament bottle to take out the medicament bottle from carrying the silo.
A second connecting block 21 is arranged on the side wall of the box cover 2, a second movable groove is arranged on the second connecting block 21, a fixing plate 22 is arranged on one side of the second connecting block 21, a second push plate 221 matched with the second movable groove is arranged on the side wall of the fixing plate 22, a third push plate is arranged at one end of the fixing plate 221, a limiting groove is arranged on the fixing plate 22, a third connecting block is arranged on the side wall of the box body 1, and a limiting block 14 matched with the limiting groove is arranged on the third connecting block; a limiting spring 212 is arranged on the inner wall of the second movable groove, and a pressing plate 211 is arranged at one end of the limiting spring 212; after the medicament bottle 3 is placed into the material carrying groove, the box cover 2 is covered on the box body 1, the third push plate is pushed along the second movable groove, the third push plate pushes the fixing plate 22 to move downwards, the fixing plate 22 moves to one side of the limiting block 14, the limiting block 14 is embedded into the limiting groove, and the limiting block 14 fixes the fixing plate 22 to seal the storage box; when the storage box is opened to collect the medicine bottles 3, the second push plate 221 is pushed to the top of the second movable groove, so that the second push plate 221 drives the fixing plate 22 to move away from the limiting block 14, the limiting block 14 is separated from the limiting groove, and the box cover 2 is directly opened to collect the medicine bottles 3; under the mutual matching of the limiting block and the limiting groove, the box cover and the box body are fixed together, so that the storage box forms a closed space, and the protection effect on the medicament bottle is improved; the pressing plate provides pressure for the second push plate, and the second push plate is pressed at the bottom of the second movable groove, so that the second push plate can stably move in the second movable groove, and the matching effect of the limiting block and the limiting groove is ensured; the limiting block is separated from the limiting groove by pushing the second push plate, so that the box cover can be easily opened from the box body, the medicine bottles can be collected more conveniently, and the use convenience of the storage box is improved.
The limiting grooves and the limiting blocks are multiple groups, the top ends of the limiting blocks are of arc structures, and when the fixing plate is pushed downwards, the fixing plate can gradually move downwards under the action of the cambered surfaces of the limiting blocks, so that the fixing plate can only move in a single direction under the action of the limiting blocks, and the box body and the box cover are fixed; under the cooperation of multiunit spacing groove and stopper, promote the cooperation effect of fixed plate and stopper, effectually fix box and case lid together to fix the medicament bottle in the bin.
The box cover is provided with a connecting plate 25, the connecting plate is provided with a plurality of positioning grooves corresponding to the material carrying grooves, a second cavity is formed between the connecting plate and the box cover, clean water is also filled in the second cavity, the side wall of the box cover is provided with a second water inlet, a second sealing plug is inserted in the second water inlet, the side wall of the box cover is provided with a fourth movable groove, a second baffle is arranged in the fourth movable groove, the structures of the second water inlet, the second sealing plug and the second baffle are the same as the structures of the first water inlet, the first sealing plug and the first baffle, and the connecting mode of the connecting plate and the box cover is the same as the connecting mode of the material carrying plate and the box; through the arrangement of the two cavities on the box body and the box cover, clear water is filled on the box body and the box cover, a good cooling effect is provided for the storage box, and an indicative temperature environment is provided for the storage of the 2, 4-dinitroaniline.
Example 2:
a preparation method of 2, 4-dinitroaniline comprises the following specific steps: using formamide or acetamide as a solvent, leading the weight ratio of 2, 4-dinitrochlorobenzene to formamide or acetamide to be 1: 10, blowing ammonia gas for 2.5 hours, cooling and separating the obtained reaction mixture after continuing to react for 0.5 hour to obtain 2, 4-dinitroaniline, and collecting the 2, 4-dinitroaniline in a storage tank for storage; the solvent is formamide; the weight ratio of the 2, 4-dinitrochlorobenzene to formamide or acetamide is 1: 3; pouring the cooled reaction mixture into water, separating or directly filtering the cooled reaction mixture by suction, wherein a filter cake is a product; the filtrate obtained by suction filtration is used as a reaction solvent for recycling; the storage box structure is the same as that in embodiment 1.
Example 3:
a preparation method of 2, 4-dinitroaniline comprises the following specific steps: using formamide or acetamide as a solvent, leading the weight ratio of 2, 4-dinitrochlorobenzene to formamide or acetamide to be 1: 5, blowing ammonia gas for 2 hours, cooling and separating the obtained reaction mixture after continuing to react for 0.5 hour to obtain 2, 4-dinitroaniline, and collecting the 2, 4-dinitroaniline in a storage tank for storage; the solvent is formamide; the weight ratio of the 2, 4-dinitrochlorobenzene to formamide or acetamide is 1: 3; pouring the cooled reaction mixture into water, separating or directly filtering the cooled reaction mixture by suction, wherein a filter cake is a product; the filtrate obtained by suction filtration is used as a reaction solvent for recycling; the storage box structure is the same as that in embodiment 1.
Claims (7)
1. A preparation method of 2, 4-dinitroaniline is characterized by comprising the following steps: the method comprises the following specific steps: using formamide or acetamide as a solvent, leading the weight ratio of 2, 4-dinitrochlorobenzene to formamide or acetamide to be 1: 1-10, blowing ammonia gas for 1.5-2.5 hours, cooling and separating the obtained reaction mixture after continuing to react for 0.5 hour to obtain 2, 4-dinitroaniline, and collecting the 2, 4-dinitroaniline in a storage tank for storage;
the storage box comprises a box body (1) and a box cover (2), one end of the box cover (2) is rotatably connected to the side wall of the box body (1), a material carrying plate (12) is arranged in the box body (1), the material carrying plate (12) and the inner wall of the box body (1) form a first cavity, and clear water is filled in the first cavity; a first connecting block (13) is arranged at the bottom of the box body (1), a first connecting groove is formed in the first connecting block (13), and a first connecting ring (127) matched with the first connecting groove is arranged at the bottom of the material carrying plate (12); a plurality of material loading grooves are formed in the material loading plate (12), and the medicament bottles (3) are inserted into the material loading grooves; the 2, 4-dinitroaniline is placed in a reagent bottle (3) after being prepared, then the reagent bottle (3) is placed in a material carrying groove, clean water is injected into the first cavity, the whole first cavity is filled with the clean water, the clean water is directly contacted with a material carrying plate (12), a box cover (2) is covered, and the packing treatment of the 2, 4-dinitroaniline is completed.
2. A process for the preparation of 2, 4-dinitroaniline according to claim 1 wherein: the solvent is formamide.
3. A process for the preparation of 2, 4-dinitroaniline according to claim 1 wherein: the weight ratio of the 2, 4-dinitrochlorobenzene to formamide or acetamide is 1: 3.
4. A process for the preparation of 2, 4-dinitroaniline according to claim 1 wherein: and pouring the cooled reaction mixture into water, and separating or directly filtering the cooled reaction mixture by suction to obtain a filter cake as a product.
5. A process for the preparation of 2, 4-dinitroaniline according to claim 4 wherein: and the filtrate obtained by suction filtration is used as a reaction solvent for recycling.
6. A process for the preparation of 2, 4-dinitroaniline according to claim 1 wherein: a first movable groove is formed in the side wall of the material carrying groove, a fixing ring (121) is arranged in the material carrying groove, a movable block (122) matched with the first movable groove is arranged on the side wall of the fixing ring (121), a fixed spring (123) is arranged on the side wall of the movable block (122), and a first push plate (126) is rotatably connected in the first movable groove; the medicament bottle (3) comprises an upper bottle body and a lower bottle body, and the diameter of the upper bottle body is smaller than that of the lower bottle body; when a medicament bottle (3) is placed into the storage trough, the bottom end of the medicament bottle (3) is in contact with a first push plate (126), the medicament bottle (3) pushes one end of the first push plate (126) to move downwards, so that the first push plate (126) rotates around a connecting point, the first push plate (126) pushes a movable block (122) to move towards a first movable trough, the movable block (122) drives a fixing ring (121) to move towards the side wall of a material carrying trough, after the bottom end of a lower bottle body moves to one side of the fixing ring (121), the first push plate (126) is in an inclined state again under the pushing of the lower bottle body, so that the first push plate (126) at one end of the material carrying trough inclines downwards, and a fixing spring (123) pushes the movable block (122) to move towards the outer side of the first movable trough, so that the fixing ring (121) clamps the medicament bottle (3); when the medicine bottle (3) is taken out of the material carrying groove, the top end of the lower bottle body is contacted with one end of the first push plate (126) in the material carrying groove, the lower bottle body pushes the first push plate (126) to rotate around the connecting point along with the pulling of the medicine bottle (3), so that one end of the first push plate (126) in the material carrying groove is inclined upwards again, and the resetting action of the first push plate (126) is completed.
7. A process for the preparation of 2, 4-dinitroaniline according to claim 1 wherein: a second connecting block (21) is arranged on the side wall of the box cover (2), a second movable groove is formed in the second connecting block (21), a fixing plate (22) is arranged on one side of the second connecting block (21), a second push plate (221) matched with the second movable groove is arranged on the side wall of the fixing plate (22), a third push plate is arranged at one end of the fixing plate (221), a limiting groove is formed in the fixing plate (22), a third connecting block is arranged on the side wall of the box body (1), and a limiting block (14) matched with the limiting groove is arranged on the third connecting block; a limiting spring (212) is arranged on the inner wall of the second movable groove, and a pressing plate (211) is arranged at one end of the limiting spring (212); after the medicament bottle (3) is placed into the material carrying groove, the box cover (2) is covered on the box body (1), the third push plate is pushed along the second movable groove, the third push plate pushes the fixing plate (22) to move downwards, the fixing plate (22) moves to one side of the limiting block (14), the limiting block (14) is embedded into the limiting groove, and the limiting block (14) fixes the fixing plate (22) to seal the storage box; when opening the bin and collecting medicament bottle (3), promote second push pedal (221) toward second activity groove top, make second push pedal (221) drive fixed plate (22) and keep away from stopper (14) motion, stopper (14) deviate from the spacing inslot, directly open case lid (2) and collect medicament bottle (3).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910904206.XA CN110668954A (en) | 2019-09-24 | 2019-09-24 | Preparation method of 2, 4-dinitroaniline |
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| CN201910904206.XA CN110668954A (en) | 2019-09-24 | 2019-09-24 | Preparation method of 2, 4-dinitroaniline |
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| CN110668954A true CN110668954A (en) | 2020-01-10 |
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Address after: 312300 No. 7 Weisan Road, Shangyu Economic and Technological Development Zone, Hangzhou Bay, Shaoxing City, Zhejiang Province Applicant after: Zhejiang Huixiang New Material Technology Co.,Ltd. Address before: 312000 No.7, Weisan Road, Shangyu economic and Technological Development Zone, Hangzhou Bay, Shangyu District, Shaoxing City, Zhejiang Province Applicant before: ZHEJIANG HUIXIANG CHEMICAL INDUSTRY Co.,Ltd. |
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Application publication date: 20200110 |