阅读说明：本技术 一种精细化工产品提纯方法 (Method for purifying fine chemical products ) 是由 董军辉 吴玉坤 王英 于 2019-10-12 设计创作，主要内容包括：本发明属于化工提纯技术领域,具体的说是一种精细化工产品提纯方法,该方法所使用的提纯设备包括壳体；壳体内部设有破碎桶,绞龙位于破碎桶内部,破碎桶底部设有多对锥形的凸起,破碎桶外壁与壳体内壁之间围成邻苯二胺蒸发后的结晶区,且结晶区底部开设多个出料口；壳体外圈下半部设有冷却腔,冷却腔内装有导热油,冷却腔外壁上设有控制器,且控制器用于控制提纯设备的工作；通过电机、绞龙和凸起,实现对投入壳体内部粗品邻苯二胺的破碎；本发明绞龙和锥形的凸起配合,将投入破碎桶内的粗品邻苯二胺破碎,再配合一号弹簧和推块,进一步对粗品邻苯二胺进行破碎,从而加快热离子水对粗品邻苯二胺的融化效率。(The invention belongs to the technical field of chemical purification, and particularly relates to a purification method of a fine chemical product, wherein purification equipment used in the method comprises a shell; a crushing barrel is arranged in the shell, the auger is positioned in the crushing barrel, a plurality of pairs of conical bulges are arranged at the bottom of the crushing barrel, a crystallization area after the o-phenylenediamine is evaporated is defined between the outer wall of the crushing barrel and the inner wall of the shell, and a plurality of discharge holes are formed at the bottom of the crystallization area; a cooling cavity is arranged at the lower half part of the outer ring of the shell, heat conducting oil is filled in the cooling cavity, and a controller is arranged on the outer wall of the cooling cavity and used for controlling the work of the purification equipment; the crushing of the crude o-phenylenediamine thrown into the shell is realized through the motor, the auger and the bulge; according to the invention, the auger is matched with the conical bulge, crude o-phenylenediamine thrown into the crushing barrel is crushed, and then the crude o-phenylenediamine is further crushed by matching with the first spring and the push block, so that the melting efficiency of hot ionized water on the crude o-phenylenediamine is accelerated.)

1. A method for purifying fine chemical products is characterized by comprising the following steps: the purification method comprises the following steps:

s1: firstly, adding azobenzene and derivatives thereof, a catalyst, an oxidant and a nitrating agent into a pressure-resistant sealed tube of an organic solvent for reaction, filtering to remove filter residues, washing the filter residues with dichloromethane, collecting filtrate and drying;

s2: spin-drying the solvent in the filtrate in S1, purifying by using a silica gel column, and eluting by using an eluent to obtain o-nitroazobenzene and derivatives thereof; carrying out reduction reaction on the obtained o-nitroazobenzene derivative and a reduction reagent at room temperature under an inert gas environment to obtain a crude product o-phenylenediamine and a derivative thereof;

s3: putting the crude o-phenylenediamine in the S2 into a purification device, melting the crude o-phenylenediamine by using hot ionized water, and then cooling, evaporating and crystallizing to obtain a final product o-phenylenediamine;

the purification apparatus used in the above purification method S3 includes a casing (1); an end cover (11) is arranged at the upper end of the shell (1), a motor (12) connected through a bolt is arranged in the center of the end cover (11), feed ports (13) are symmetrically arranged on the end covers (11) at two sides of the motor (12), an output shaft of the motor (12) penetrates through the end cover (11) to extend into the shell (1) and is fixedly connected with a central shaft of the packing auger (2), and the lower end of the central shaft of the packing auger (2) is connected to the bottom of the shell (1) through a bearing; a crushing barrel (3) is arranged in the shell (1), the packing auger (2) is positioned in the crushing barrel (3), the upper end opening of the crushing barrel (3) corresponds to the position of a feed opening (13) formed in the end cover (11), a plurality of pairs of conical bulges (31) are arranged at the bottom of the crushing barrel (3), a crystallization area (4) formed by evaporating o-phenylenediamine is enclosed between the outer wall of the crushing barrel (3) and the inner wall of the shell (1), and a plurality of discharge openings (41) are formed at the bottom of the crystallization area (4); a cooling cavity (14) is arranged at the lower half part of the outer ring of the shell (1), heat conducting oil is filled in the cooling cavity (14), a controller (15) is arranged on the outer wall of the cooling cavity (14), and the controller (15) is used for controlling the work of the purification equipment; the crude o-phenylenediamine thrown into the shell (1) is crushed through the motor (12), the auger (2) and the protrusion (31).

2. The purification method of fine chemical products according to claim 1, wherein: a push block (311) is arranged between each pair of the bulges (31), and the push block (311) is connected to the bottom of the crushing barrel (3) through a first spring (312); the crude o-phenylenediamine falling into the bottom of the crushing barrel (3) is bounced up through a first spring (312) and a push block (311).

3. The purification method of fine chemical products according to claim 1, wherein: a channel (211) is formed in the spiral blade (21) of the auger (2), the channel (211) is from bottom to top, and the aperture of the channel (211) is gradually reduced; a channel (211) is arranged in the spiral blade (21) to crush the crude o-phenylenediamine which rises spirally.

4. A purification method of fine chemical products according to claim 3, characterized in that: the upper end of the spiral blade (21) is provided with a steel ball (221) fixedly connected through a first rope (22); the upper quarter part of the crushing barrel (3) is formed by splicing a plurality of baffle plates (32) made of elastic materials; through the cooperation between a rope (22), a steel ball (221) and the baffle (32), the collision to the o-phenylenediamine crystal and the opening and closing of the baffle (32) are realized.

5. A purification method of fine chemical products according to claim 3, characterized in that: a second spring (212) is arranged in the channel (211), and the upper end of the second spring (212) is connected with a first rope (22); the first rope (22) pulls the second spring (212), so that the second spring (212) extrudes and crushes the crude o-phenylenediamine.

6. The purification method of fine chemical products according to claim 1, wherein: a first plate (42) arranged in an S shape is arranged on the wall of the crystallization area (4), and the first plate (42) is arranged in a downward direction in an inclined manner; the vapor crystallization of o-phenylenediamine is accelerated by passing it through a first plate (42).

Technical Field

The invention belongs to the technical field of chemical purification, and particularly relates to a purification method of a fine chemical product.

Background

O-phenylenediamine which is a colorless monoclinic crystal at normal temperature and darkens in air and sunlight; slightly soluble in cold water, soluble in hot water, and readily soluble in ethanol, diethyl ether and chloroform. Reacting with inorganic acid to generate salt which is easy to dissolve in water; is an intermediate of dye, pesticide, auxiliary agent, photosensitive material and the like; it is itself the dye fur yellow brown M; the method is used for preparing polyamide, polyurethane, carbendazim, thiophanate, vat scarlet GG, leveling agent, anti-aging agent MB, and is also used for preparing developing agent and surfactant.

The commercially available ortho-diamine starting material generally has a purity of 70 to 90% by weight and contains small amounts of meta-toluenediamine, monoamine and other impurities; if the impurities are not removed, the commercial raw materials directly react with sodium nitrite to prepare the tolyltriazole, and the impurities also react with the sodium nitrite to generate byproducts with very dark colors, which directly affect the quality of the tolyltriazole and lead to high impurity content. Therefore, a new purification technology needs to be developed to produce high-purity o-phenylenediamine, and the promotion of upgrading of such chemical products has profound significance.

Disclosure of Invention

Aiming at the defects of the prior art, the invention provides a method for purifying a fine chemical product, which solves the problems of low purification purity of the traditional crude o-phenylenediamine and low purification efficiency of the o-phenylenediamine.

The technical scheme adopted by the invention for solving the technical problems is as follows: the invention relates to a method for purifying fine chemical products, which comprises the following steps:

s1: firstly, adding azobenzene and derivatives thereof, a catalyst, an oxidant and a nitrating agent into a pressure-resistant sealed tube of an organic solvent for reaction, filtering to remove filter residues, washing the filter residues with dichloromethane, collecting filtrate and drying;

s2: spin-drying the solvent in the filtrate in S1, purifying by using a silica gel column, and eluting by using an eluent to obtain o-nitroazobenzene and derivatives thereof; carrying out reduction reaction on the obtained o-nitroazobenzene derivative and a reduction reagent at room temperature under an inert gas environment to obtain a crude product o-phenylenediamine and a derivative thereof;

s3: putting the crude o-phenylenediamine in the S2 into a purification device, melting the crude o-phenylenediamine by using hot ionized water, and then cooling, evaporating and crystallizing to obtain a final product o-phenylenediamine;

the purification apparatus used in the above purification method S3 includes a housing; an end cover is arranged at the upper end of the shell, a motor connected through a bolt is arranged in the center of the end cover, feed ports are symmetrically arranged on the end covers at two sides of the motor, an output shaft of the motor penetrates through the end covers to extend into the shell and is fixedly connected with a central shaft of the packing auger, and the lower end of the central shaft of the packing auger is connected to the bottom of the shell through a bearing; a crushing barrel is arranged in the shell, the auger is positioned in the crushing barrel, the upper end opening of the crushing barrel corresponds to the feed inlet arranged on the end cover, a plurality of pairs of conical bulges are arranged at the bottom of the crushing barrel, a crystallization area after o-phenylenediamine is evaporated is enclosed between the outer wall of the crushing barrel and the inner wall of the shell, and a plurality of discharge outlets are formed at the bottom of the crystallization area; a cooling cavity is arranged at the lower half part of the outer ring of the shell, heat conducting oil is filled in the cooling cavity, and a controller is arranged on the outer wall of the cooling cavity and used for controlling the work of the purification equipment; the crushing of the crude o-phenylenediamine thrown into the shell is realized through the motor, the auger and the bulge; when the crushing device works, crude o-phenylenediamine is firstly put into a crushing barrel from a feeding hole, the crude o-phenylenediamine is in a blade crystalline state, when the crude o-phenylenediamine falls into the bottom of the crushing barrel, a protrusion crushes the crude o-phenylenediamine, then a motor is started to rotate, an output shaft of the motor drives an auger to rotate, the crude o-phenylenediamine at the bottom of the crushing barrel is rotated and ascended on the auger, the crude o-phenylenediamine ascends to the upper end of the auger and descends, the crude o-phenylenediamine falls on the protrusion again, the protrusion crushes the crude o-phenylenediamine again, the auger repeatedly spirally ascends the crude o-phenylenediamine and then descends, the protrusion repeatedly crushes the crude o-phenylenediamine until the crude o-phenylenediamine is crushed to meet the requirement, hot ionized water is poured from a feeding hole, the crushed crude o-phenylenediamine is melted by the hot ionized water, and then the crude o-phenylenediamine ascends along the, then the steam flows into the crystallization area, the crystallization area is tightly attached to the cooling cavity, heat in the steam is absorbed by heat conduction oil in the cooling cavity, then the steam is crystallized into pure o-phenylenediamine and falls into the bottom of the crystallization area, and finally the steam is taken out from a discharge hole.

Preferably, a push block is arranged between each pair of the bulges and is connected to the bottom of the crushing barrel through a first spring; the bouncing of the crude o-phenylenediamine falling into the bottom of the crushing barrel is realized through a first spring and a push block; when the crushing barrel works, when crude o-phenylenediamine falls into the bottom of the crushing barrel, the protrusion crushes the crude o-phenylenediamine, when the crude o-phenylenediamine falls onto the push block, the first spring pushes up the push block, then the push block bounces up the crude o-phenylenediamine, the crude o-phenylenediamine falls onto the protrusion again after bounced up, and the protrusion further crushes the crude o-phenylenediamine; the crushing of the crude o-phenylenediamine is accelerated by the cooperation of the bulges, the first spring and the push block, so that the purification efficiency of the crude o-phenylenediamine is accelerated.

Preferably, a channel is formed in the spiral blade of the auger, and the aperture of the channel is gradually reduced from bottom to top; a channel is arranged in the spiral blade, and the crude o-phenylenediamine spirally lifted is extruded and crushed; when the auger rotates, the spiral blade of the auger brings crude o-phenylenediamine into the channel, and the channel is designed according to the mode that the aperture of the channel is gradually reduced from bottom to top, so the channel extrudes the crude o-phenylenediamine while lifting the crude o-phenylenediamine, the crude o-phenylenediamine is extruded and crushed in the channel, meanwhile, the channel extrudes the crude o-phenylenediamine, heat is generated by friction, the temperature of the crude o-phenylenediamine is increased, the later-stage hot ion water melting of the crude o-phenylenediamine is assisted, the melting of the crude o-phenylenediamine is accelerated, and the purification efficiency of the crude o-phenylenediamine is accelerated.

Preferably, the upper end of the spiral blade is provided with a steel ball fixedly connected through a first rope; one quarter of the upper end of the crushing barrel is formed by splicing a plurality of baffle plates made of elastic materials; through the cooperation of the first rope, the steel ball and the baffle, the collision of o-phenylenediamine crystals and the opening and closing of the baffle are realized; when the auger rotates, the spiral blade drives the steel ball to rotate through the first rope, when the steel ball collides with the baffle, the baffle bends towards the inner wall of the shell, a gap is leaked between adjacent baffles, and o-phenylenediamine steam flows to the crystallization area from the gap, so that the path of the o-phenylenediamine steam circulating to the crystallization area is reduced; when the purification equipment starts to work, the temperature of the baffle is low, when the o-phenylenediamine steam is attached to the baffle, the o-phenylenediamine is directly crystallized on the baffle, and therefore when the steel ball collides with the baffle, the o-phenylenediamine crystals on the baffle are collided and fall into a crystallization area.

Preferably, a second spring is arranged in the channel, and the upper end of the second spring is connected with a first rope; the No. two springs are pulled by the first rope, so that the No. two springs extrude and crush the crude o-phenylenediamine; the during operation, the steel ball is when rotating, and the steel ball drags a rope, and No. two springs are dragged to a rope, and No. two springs are dragged the in-process, and No. two springs are in time with crude o-phenylenediamine follow through-hole in push out to and No. two springs are pushing out crude o-phenylenediamine in-process, and No. two springs also extrude the breakage to crude o-phenylenediamine, further to crude o-phenylenediamine breakage, thereby accelerate crude o-phenylenediamine's purification efficiency.

Preferably, the wall of the crystallization area is provided with a first plate arranged in an S shape, and the first plate is arranged in a downward direction in an inclined manner; accelerating the steam crystallization of o-phenylenediamine through a first plate; when the device works, steam flows to a crystallization area, then o-phenylenediamine steam passes through a plurality of first plates, and the design of the first plates prolongs the flow path of the o-phenylenediamine steam, so that the temperature of the o-phenylenediamine steam at the upper half part of the crystallization area begins to drop, at the moment, the o-phenylenediamine steam is not crystallized yet, and the o-phenylenediamine steam begins to crystallize rapidly when the o-phenylenediamine steam falls into the lower half part of the crystallization area, therefore, the temperature of the o-phenylenediamine steam is reduced in advance by the design of the first plates, and preparation is made for crystallization of the o-phenylenediamine steam in advance.

The invention has the technical effects and advantages that:

1. according to the fine chemical product purification method, the auger is matched with the conical bulge, crude o-phenylenediamine thrown into the crushing barrel is crushed, and then the crude o-phenylenediamine is further crushed by matching with the spring and the push block, so that the melting efficiency of hot ionized water on the crude o-phenylenediamine is accelerated.

2. The invention relates to a fine chemical product purification method, wherein a steel ball pulls a second spring through a first rope, the second spring pushes out crude o-phenylenediamine from a through hole, and the crude o-phenylenediamine is extruded and crushed; the design of the through hole extrudes and crushes the crude o-phenylenediamine at one side, and the friction between the through hole and the crude o-phenylenediamine generates heat to assist the hot ion water to melt the crude o-phenylenediamine; the cloth swinging design of the first plate is beneficial to steam crystallization of o-phenylenediamine, thereby accelerating the purification efficiency of crude o-phenylenediamine.

Drawings

The invention will be further explained with reference to the drawings.

FIG. 1 is a flow chart of a method of the present invention;

FIG. 2 is a schematic perspective view of a purification apparatus used in the present invention;

FIG. 3 is an enlarged view of a portion of FIG. 2 at A;

FIG. 4 is an enlarged view of a portion of FIG. 2 at B;

in the figure: the device comprises a shell 1, an end cover 11, a motor 12, a feeding port 13, a cooling cavity 14, a controller 15, an auger 2, a spiral blade 21, a channel 211, a second spring 212, a first rope 22, a steel ball 221, a crushing barrel 3, a protrusion 31, a push block 311, a first spring 312, a baffle 32, a crystallization area 4, a discharge port 41 and a first plate 42.

Detailed Description

In order to make the technical means, the creation characteristics, the achievement purposes and the effects of the invention easy to understand, the invention is further described with the specific embodiments.

As shown in fig. 1 to 4, the method for purifying a fine chemical product according to the present invention comprises the following steps:

s1: firstly, adding azobenzene and derivatives thereof, a catalyst, an oxidant and a nitrating agent into a pressure-resistant sealed tube of an organic solvent for reaction, filtering to remove filter residues, washing the filter residues with dichloromethane, collecting filtrate and drying;

s2: spin-drying the solvent in the filtrate in S1, purifying by using a silica gel column, and eluting by using an eluent to obtain o-nitroazobenzene and derivatives thereof; carrying out reduction reaction on the obtained o-nitroazobenzene derivative and a reduction reagent at room temperature under an inert gas environment to obtain a crude product o-phenylenediamine and a derivative thereof;

s3: putting the crude o-phenylenediamine in the S2 into a purification device, melting the crude o-phenylenediamine by using hot ionized water, and then cooling, evaporating and crystallizing to obtain a final product o-phenylenediamine;

the purification apparatus used in the above purification method S3 includes a housing 1; an end cover 11 is arranged at the upper end of the shell 1, a motor 12 connected through a bolt is arranged in the center of the end cover 11, feed ports 13 are symmetrically arranged on the end covers 11 at two sides of the motor 12, an output shaft of the motor 12 penetrates through the end cover 11 to extend into the shell 1 and is fixedly connected with a central shaft of the packing auger 2, and the lower end of the central shaft of the packing auger 2 is connected to the bottom of the shell 1 through a bearing; a crushing barrel 3 is arranged in the shell 1, the auger 2 is positioned in the crushing barrel 3, the upper end opening of the crushing barrel 3 corresponds to the position of a feeding port 13 arranged on the end cover 11, a plurality of pairs of conical bulges 31 are arranged at the bottom of the crushing barrel 3, a crystallization area 4 after the o-phenylenediamine is evaporated is enclosed between the outer wall of the crushing barrel 3 and the inner wall of the shell 1, and a plurality of discharge ports 41 are formed at the bottom of the crystallization area 4; a cooling cavity 14 is arranged at the lower half part of the outer ring of the shell 1, heat conducting oil is filled in the cooling cavity 14, a controller 15 is arranged on the outer wall of the cooling cavity 14, and the controller 15 is used for controlling the work of the purification equipment; the crude o-phenylenediamine thrown into the shell 1 is crushed through the motor 12, the auger 2 and the protrusion 31; when the crushing device works, crude o-phenylenediamine is firstly put into the crushing barrel 3 from a feeding hole, the crude o-phenylenediamine is in a blade crystalline state, when the crude o-phenylenediamine falls into the bottom of the crushing barrel 3, the protrusion 31 crushes the crude o-phenylenediamine, then the motor 12 is started to rotate, the output shaft of the motor 12 drives the auger 2 to rotate, the crude o-phenylenediamine at the bottom of the crushing barrel 3 is rotated and ascended on the auger 2, the crude o-phenylenediamine ascends to the upper end of the auger 2 and falls down, the crude o-phenylenediamine falls on the protrusion 31 again, the protrusion 31 crushes the crude o-phenylenediamine again, the auger 2 repeatedly spirally ascends the crude o-phenylenediamine and then falls down, the protrusion 31 repeatedly crushes the crude o-phenylenediamine until the crude o-phenylenediamine is crushed to the requirement, hot ionized water is poured into the feeding hole 13, the crushed crude o-phenylenediamine is melted by the hot ionized water, and then the crude o-phenylenediamine ascends along the wall, then the steam flows into the crystallization area 4, the crystallization area 4 is tightly attached to the cooling cavity 14, heat in the steam is absorbed by heat conducting oil in the cooling cavity 14, then the steam is crystallized into pure o-phenylenediamine and falls into the bottom of the crystallization area 4, and finally the steam is taken out from the discharge hole 41.

As an embodiment of the present invention, a pushing block 311 is arranged between each pair of the protrusions 31, and the pushing block 311 is connected to the bottom of the crushing barrel 3 through a first spring 312; the bouncing of the crude o-phenylenediamine falling into the bottom of the crushing barrel 3 is realized through a first spring 312 and a push block 311; when the crushing barrel is in work, when crude o-phenylenediamine falls into the bottom of the crushing barrel 3, the protrusion 31 crushes the crude o-phenylenediamine, when the crude o-phenylenediamine falls onto the push block 311, the first spring 312 pushes up the push block 311, then the push block 311 bounces up the crude o-phenylenediamine, the crude o-phenylenediamine falls onto the protrusion 31 again after bounced up, and the protrusion 31 further crushes the crude o-phenylenediamine; the crushing of the crude o-phenylenediamine is accelerated by the cooperation of the bulge 31, the first spring 312 and the push block 311, so that the purification efficiency of the crude o-phenylenediamine is accelerated.

As an embodiment of the invention, a channel 211 is formed in the spiral blade 21 of the auger 2, and the aperture of the channel 211 is gradually reduced from bottom to top through the channel 211; a channel 211 is arranged in the spiral blade 21, and the crude o-phenylenediamine spirally lifted is extruded and crushed; when the screw conveyor 2 rotates, the spiral blade 21 of the screw conveyor 2 brings crude o-phenylenediamine into the channel 211, the channel 211 is designed in a mode that the aperture of the channel 211 is gradually reduced from bottom to top, so that the channel 211 extrudes the crude o-phenylenediamine and lifts the crude o-phenylenediamine at the same time, the crude o-phenylenediamine is extruded and crushed in the channel 211, meanwhile, the channel 211 extrudes the crude o-phenylenediamine to generate heat through friction, the temperature of the crude o-phenylenediamine is increased, the later-stage hot ion water melting of the crude o-phenylenediamine is assisted, the melting of the crude o-phenylenediamine is accelerated, and the purification efficiency of the crude o-phenylenediamine is accelerated.

As an embodiment of the invention, the upper end of the spiral blade 21 is provided with a steel ball 221 fixedly connected through a first rope 22; the upper quarter part of the crushing barrel 3 is formed by splicing a plurality of baffle plates 32 made of elastic materials; through the cooperation of the first rope 22, the steel ball 221 and the baffle 32, the collision of o-phenylenediamine crystals and the opening and closing of the baffle 32 are realized; when the auger 2 rotates, the spiral blade 21 drives the steel ball 221 to rotate through the first rope 22, when the steel ball 221 collides with the baffle 32, the baffle 32 bends towards the inner wall of the shell 1, gaps are leaked between adjacent baffles 32, and the o-phenylenediamine steam flows to the crystallization area 4 from the gaps, so that the path of the o-phenylenediamine steam flowing to the crystallization area 4 is reduced; when the purification equipment starts to work, the temperature of the baffle 32 is low, when the o-phenylenediamine vapor is attached to the baffle 32, the o-phenylenediamine vapor can be directly crystallized on the baffle 32, so that when the steel ball 221 collides with the baffle 32, the o-phenylenediamine crystals on the baffle 32 collide and fall into the crystallization area 4.

As an embodiment of the present invention, a second spring 212 is disposed in the channel 211, and the upper end of the second spring 212 is connected to the first rope 22; the first rope 22 pulls the second spring 212 to realize the extrusion and crushing of the second spring 212 on the crude o-phenylenediamine; during operation, steel ball 221 is when rotating, and steel ball 221 drags rope 22 for one number, and rope 22 drags spring 212 for two numbers, and spring 212 for two numbers is dragged the in-process, and spring 212 for two numbers in time pushes out crude o-phenylenediamine from the through-hole to and spring 212 for two numbers is pushing out crude o-phenylenediamine in-process, and spring 212 for two numbers also extrudees the breakage to crude o-phenylenediamine, further smashes crude o-phenylenediamine, thereby accelerates crude o-phenylenediamine's purification efficiency.

As an embodiment of the present invention, the first plate 42 is arranged in the shape of letter "S" on the wall of the crystallization zone 4, and the first plate 42 is arranged in the downward direction with an inclination; the steam crystallization of o-phenylenediamine is accelerated by a first plate 42; during operation, steam flows to the crystallization area 4, then o-phenylenediamine steam passes through the first plates 42, and the design of the first plates 42 prolongs the flow path of the o-phenylenediamine steam, so that the temperature of the o-phenylenediamine steam at the upper half part of the crystallization area 4 begins to decrease, at the moment, the o-phenylenediamine steam does not crystallize, and the o-phenylenediamine steam begins to crystallize rapidly when the o-phenylenediamine steam falls into the lower half part of the crystallization area 4, so that the temperature of the o-phenylenediamine steam is reduced in advance by the design of the first plates 42, and preparation is made for crystallization of the o-phenylenediamine steam in advance.

When the device works, crude o-phenylenediamine is firstly thrown into a crushing barrel 3 from a feeding hole, when the crude o-phenylenediamine falls into the bottom of the crushing barrel 3, the crude o-phenylenediamine is crushed by a protrusion 31, then a motor 12 is started to rotate, an output shaft of the motor 12 drives an auger 2 to rotate, the crude o-phenylenediamine at the bottom of the crushing barrel 3 is rotationally lifted up on the auger 2, the crude o-phenylenediamine rises to the upper end of the auger 2 and falls down, the crude o-phenylenediamine falls onto the protrusion 31 again, the protrusion 31 crushes the crude o-phenylenediamine again, the auger 2 repeatedly spirally lifts the crude o-phenylenediamine and then falls down, the protrusion 31 repeatedly crushes the crude o-phenylenediamine until the diameter of the crude o-phenylenediamine reaches the requirement, hot ionized water is poured into the device from a feeding hole 13, the crushed crude o-phenylenediamine is melted by the hot ionized water, and then the crude o-phenylenediamine rises along the wall of the, then the steam flows into the crystallization area 4, the crystallization area 4 is tightly attached to the cooling cavity 14, heat in the steam is absorbed by heat conduction oil in the cooling cavity 14, then the steam is crystallized into pure o-phenylenediamine and falls into the bottom of the crystallization area 4, and finally the steam is taken out from a discharge hole 41; when the crude o-phenylenediamine falls into the bottom of the crushing barrel 3, the protrusion 31 crushes the crude o-phenylenediamine, when the crude o-phenylenediamine falls onto the push block 311, the first spring 312 pushes up the push block 311, then the push block 311 bounces up the crude o-phenylenediamine, the crude o-phenylenediamine falls onto the protrusion 31 again after bounced up, and the protrusion 31 further crushes the crude o-phenylenediamine; the protrusions 31, the first springs 312 and the push blocks 311 are matched with one another, so that the crushing of the crude o-phenylenediamine is accelerated, and the purification efficiency of the crude o-phenylenediamine is accelerated; when the auger 2 rotates, the helical blade 21 of the auger 2 brings the crude o-phenylenediamine into the channel 211, and the channel 211 is designed in a mode that the aperture of the channel 211 is gradually reduced from bottom to top, so that the channel 211 extrudes the crude o-phenylenediamine while lifting the crude o-phenylenediamine, the crude o-phenylenediamine is extruded and crushed in the channel 211, meanwhile, the channel 211 generates heat by friction in the extrusion process of the crude o-phenylenediamine, the temperature of the crude o-phenylenediamine is increased, the later-stage hot ion water melting of the crude o-phenylenediamine is assisted, the melting of the crude o-phenylenediamine is accelerated, and the purification efficiency of the crude o-phenylenediamine is accelerated; when the auger 2 rotates, the spiral blade 21 drives the steel ball 221 to rotate through the first rope 22, when the steel ball 221 collides with the baffle 32, the baffle 32 bends towards the inner wall of the shell 1, gaps are leaked between adjacent baffles 32, and meanwhile, o-phenylenediamine steam flows to the crystallization area 4 from the gaps, so that the path of the o-phenylenediamine steam flowing to the crystallization area 4 is reduced; when the purification equipment starts to work, the temperature of the baffle 32 is low, when the o-phenylenediamine steam is attached to the baffle 32, the o-phenylenediamine is directly crystallized on the baffle 32, so that when the steel ball 221 collides with the baffle 32, the o-phenylenediamine crystals on the baffle 32 collide and fall into the crystallization area 4; when the steel ball 221 rotates, the steel ball 221 pulls the first rope 22, the first rope 22 pulls the second spring 212, the second spring 212 pushes the crude o-phenylenediamine out of the through hole in time in the process that the second spring 212 is pulled, and in the process that the second spring 212 pushes the crude o-phenylenediamine out, the second spring 212 also extrudes and crushes the crude o-phenylenediamine, the crude o-phenylenediamine is further crushed, and therefore the purification efficiency of the crude o-phenylenediamine is accelerated; the steam flows to the crystallization area 4, then the o-phenylenediamine steam passes through a plurality of first plates 42, and the design of the first plates 42 prolongs the flow path of the o-phenylenediamine steam, so that the temperature of the o-phenylenediamine steam at the upper half part of the crystallization area 4 begins to drop, at the moment, the o-phenylenediamine steam is not crystallized yet, and the o-phenylenediamine steam begins to crystallize rapidly when the o-phenylenediamine steam falls into the lower half part of the crystallization area 4, therefore, the temperature of the o-phenylenediamine steam is reduced in advance by the design of the first plates 42, and preparation is made for crystallization of the o-phenylenediamine steam in advance.

The foregoing illustrates and describes the principles, general features, and advantages of the present invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.