阅读说明：本技术 一种2，4-二硝基苯胺制备方法 (Preparation method of 2, 4-dinitroaniline ) 是由 阮煜翔 王凯 于 2019-09-24 设计创作，主要内容包括：本发明公开了一种2,4-二硝基苯胺制备方法,具体步骤包括：使用甲酰胺或乙酰胺作溶剂,使2,4-二硝基氯苯和甲酰胺或乙酰胺的重量比为1∶1-10,吹入氨气1.5-2.5小时,待继续反应0.5小时后,将所得反应混合物经冷却,进行分离,制得2,4-二硝基苯胺,随后将2,4-二硝基苯胺收集在储存箱内保存。(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.)

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).

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