CN111167398A - Multifunctional high-purity seven-in-one chemical and pharmaceutical equipment and manufacturing process thereof - Google Patents
Multifunctional high-purity seven-in-one chemical and pharmaceutical equipment and manufacturing process thereof Download PDFInfo
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- CN111167398A CN111167398A CN202010042804.3A CN202010042804A CN111167398A CN 111167398 A CN111167398 A CN 111167398A CN 202010042804 A CN202010042804 A CN 202010042804A CN 111167398 A CN111167398 A CN 111167398A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/28—Moving reactors, e.g. rotary drums
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D9/00—Crystallisation
- B01D9/0004—Crystallisation cooling by heat exchange
- B01D9/0013—Crystallisation cooling by heat exchange by indirect heat exchange
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F33/00—Other mixers; Mixing plants; Combinations of mixers
- B01F33/80—Mixing plants; Combinations of mixers
- B01F33/83—Mixing plants specially adapted for mixing in combination with disintegrating operations
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J4/00—Feed or outlet devices; Feed or outlet control devices
- B01J4/001—Feed or outlet devices as such, e.g. feeding tubes
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F16—ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
- F16J—PISTONS; CYLINDERS; SEALINGS
- F16J15/00—Sealings
- F16J15/02—Sealings between relatively-stationary surfaces
- F16J15/06—Sealings between relatively-stationary surfaces with solid packing compressed between sealing surfaces
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F16—ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
- F16J—PISTONS; CYLINDERS; SEALINGS
- F16J15/00—Sealings
- F16J15/16—Sealings between relatively-moving surfaces
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F26—DRYING
- F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
- F26B11/00—Machines or apparatus for drying solid materials or objects with movement which is non-progressive
- F26B11/02—Machines or apparatus for drying solid materials or objects with movement which is non-progressive in moving drums or other mainly-closed receptacles
- F26B11/04—Machines or apparatus for drying solid materials or objects with movement which is non-progressive in moving drums or other mainly-closed receptacles rotating about a horizontal or slightly-inclined axis
- F26B11/0445—Machines or apparatus for drying solid materials or objects with movement which is non-progressive in moving drums or other mainly-closed receptacles rotating about a horizontal or slightly-inclined axis having conductive heating arrangements, e.g. heated drum wall
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F26—DRYING
- F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
- F26B3/00—Drying solid materials or objects by processes involving the application of heat
- F26B3/18—Drying solid materials or objects by processes involving the application of heat by conduction, i.e. the heat is conveyed from the heat source, e.g. gas flame, to the materials or objects to be dried by direct contact
- F26B3/22—Drying solid materials or objects by processes involving the application of heat by conduction, i.e. the heat is conveyed from the heat source, e.g. gas flame, to the materials or objects to be dried by direct contact the heat source and the materials or objects to be dried being in relative motion, e.g. of vibration
- F26B3/24—Drying solid materials or objects by processes involving the application of heat by conduction, i.e. the heat is conveyed from the heat source, e.g. gas flame, to the materials or objects to be dried by direct contact the heat source and the materials or objects to be dried being in relative motion, e.g. of vibration the movement being rotation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D9/00—Crystallisation
- B01D2009/0086—Processes or apparatus therefor
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00049—Controlling or regulating processes
- B01J2219/00051—Controlling the temperature
- B01J2219/00074—Controlling the temperature by indirect heating or cooling employing heat exchange fluids
- B01J2219/00087—Controlling the temperature by indirect heating or cooling employing heat exchange fluids with heat exchange elements outside the reactor
- B01J2219/00094—Jackets
Abstract
The invention relates to the technical field of chemical and pharmaceutical equipment, and provides multifunctional high-purity seven-in-one chemical and pharmaceutical equipment and a manufacturing process thereof, wherein the equipment comprises a rack and a barrel rotatably arranged on the rack; the barrel is sleeved with a jacket, sleeves are arranged on two sides of the barrel, and the two sleeves are rotatably connected in a bearing seat arranged on the rack; and a driving wheel is arranged on the sleeve on the left side and connected with a driving shaft of a barrel speed reducer through a belt, and the barrel speed reducer is connected with a driving shaft of a barrel rotating motor. The invention overcomes the defects of the prior art, has reasonable design and compact structure, solves the problems of low pharmaceutical efficiency, large occupied area and large investment of the existing pharmaceutical equipment, combines multiple processes together through simple structural combination, improves the chemical and pharmaceutical efficiency, and has small occupied area, small investment, good sealing effect and strong practicability.
Description
Technical Field
The invention relates to the technical field of pharmaceutical equipment, in particular to multifunctional high-purity seven-in-one chemical and pharmaceutical equipment and a manufacturing process thereof.
Background
In the process of pharmacy in chemical and pharmaceutical industries, a plurality of processes such as reaction, concentration, crystallization, filtration, washing, drying, crushing and the like need to be completed.
The current pharmaceutical process also has the following problems:
1. needs multiple three-in-one, two-in-one and other pharmaceutical equipment to cooperate, leads to the pharmacy inefficiency, the area of system is big and the investment is huge.
2. The rotary motion of barrel owing to need keeping to current multi-functional pharmaceutical equipment, uses rotation type combination seal more and separates evacuation end and barrel, because rotary seal has the not good problem of sealing performance, reveals a little seriously and influence product quality, when handling poisonous and strong corrosive material, reveals a little and not only can cause equipment to damage, and can cause the harm to environment and human body.
3. The existing equipment can not simultaneously rotate and work by stirring and crushing knives in the rotating process of a cylinder body, and the performance and the efficiency of the equipment are seriously influenced.
Therefore, a multifunctional high-purity seven-in-one chemical and pharmaceutical device and a manufacturing process thereof are provided.
Disclosure of Invention
Technical problem to be solved
Aiming at the defects of the prior art, the invention provides multifunctional high-purity seven-in-one chemical and pharmaceutical equipment and a manufacturing process thereof, overcomes the defects of the prior art, has reasonable design and compact structure, solves the problems of low pharmaceutical efficiency, large occupied area and large investment of the prior pharmaceutical equipment, combines multiple processes together through simple structural combination, improves the chemical and pharmaceutical efficiency, and has small occupied area, small investment, good sealing effect and strong practicability.
(II) technical scheme
In order to achieve the purpose, the invention is realized by the following technical scheme:
a multifunctional high-purity seven-in-one chemical and pharmaceutical equipment and its manufacturing process comprises a frame;
and a cylinder rotatably arranged on the frame;
the barrel is sleeved with a jacket, sleeves are arranged on two sides of the barrel, and the two sleeves are rotatably connected in a bearing seat arranged on the rack;
the driving wheel is arranged on the sleeve on the left side and is connected with a driving shaft of the barrel speed reducer through a belt, and the barrel speed reducer is connected with a driving shaft of the barrel rotating motor;
one end of the sleeve positioned on the left side is communicated with the jacket, the other end of the sleeve positioned on the left side is movably inserted with a jacket liquid inlet and a jacket liquid outlet respectively, the jacket liquid inlet and the jacket liquid outlet are connected to the rack through a first support, a feed pipe is arranged in the sleeve positioned on the right side, one end of the feed pipe extends into the cylinder and is connected with a plurality of filter rods in a penetrating manner, the other end of the feed pipe is movably inserted with a feed port and a vacuum port respectively, and the feed port and the vacuum port are connected to the rack through a second support;
the upper end through connection of barrel has the discharge gate, and is provided with sealed lid on the discharge gate, through connection has the fluid-discharge tube on the diapire of barrel, the other end through connection sleeve pipe on right side of fluid-discharge tube, and the activity has cup jointed sealed quiet seat on the sleeve pipe on right side, and has seted up the through-hole corresponding with sealed quiet seat on the sleeve pipe, and the lower extreme through connection of sealed quiet seat has the liquid suction pipe, and the liquid suction pipe passes the frame and is connected with the suction filtration mouth.
Furthermore, a shallow concave-pit-shaped structure corresponding to the jacket is arranged on the cylinder body.
Furthermore, a jacket end mechanical sealing ring is arranged at the movable insertion end of the sleeve positioned on the left side, and a vacuum port mechanical sealing ring is arranged at the movable insertion end of the feeding pipe.
Furthermore, a suction filtration port mechanical sealing ring is arranged between the sealing static seat and the sleeve.
Furthermore, a filter screen disc is arranged at the lower end of the inner wall of the cylinder body.
Further, still include agitating unit, agitating unit is located the lateral wall of barrel, and agitating unit includes agitator motor, agitator speed reducer and stirring rake, and the agitator speed reducer is connected to the drive shaft of agitator motor, and the drive shaft of agitator speed reducer passes the lateral wall of pressing from both sides cover and barrel and is connected with a plurality of stirring rakes.
Further, still include breaker, breaker is located the barrel, and breaker and agitating unit set up relatively, and breaker includes broken sword motor, broken sword speed reducer and broken sword, and the drive shaft of broken sword motor is connected with broken sword speed reducer, and the drive shaft of broken sword speed reducer passes the lateral wall of pressing from both sides cover and barrel and is connected with a plurality of broken swoves.
Furthermore, a crushing cutter mechanical sealing ring is arranged at the joint of the crushing cutter speed reducer and the barrel.
Furthermore, a rotating shaft power transmission device corresponding to the crushing knife motor and the stirrer motor is arranged on the sleeve.
Further, the process steps of the multifunctional high-purity seven-in-one chemical pharmacy comprise the following steps:
step 1: reacting, wherein materials enter the cylinder through the feed inlet, a heating medium is introduced into the jacket through the jacket liquid inlet according to process requirements, the heating medium with the temperature required by the process flows in the jacket in a circulating manner through the jacket liquid inlet and the jacket liquid outlet, the cylinder is rotated by a proper angle through a driving shaft of the cylinder speed reducer, a plurality of groups of mechanical seals act on the rotation process of the cylinder to keep the cylinder stable, meanwhile, a stirring paddle required by material reaction is positioned at the bottom of the cylinder, the rotation speed of the stirring paddle can be adjusted within the range of 0-480r/min, and the materials are fully reacted in the cylinder through the mixing action of the stirring paddles.
Step 2: concentration and filtration, after the material reaction is accomplished, start or stop the stirring, the heat medium that continuously lets in the required temperature of technology circulates in the clamp cover, meanwhile, carry out interior evacuation operation through the suction filter mouth to the barrel, will heat the liquid material that produces in the concentrated process and take out, if there are vapor and impurity gas to produce in the concentrated process, also can carry out the vacuum pumping operation simultaneously through suction filter mouth and vacuum port this moment, the inside filter screen dish that is provided with of device, can prevent to discharge the crystal when concentrating the vacuum pumping operation. The heating and vacuumizing time is determined according to the process requirements, and whether the sample meets the concentration requirement or not can be detected by sampling a small amount of the sample at the discharge port.
And step 3: and (4) crystallizing, wherein the barrel can complete dynamic crystallization and static crystallization operations. During dynamic crystallization, the stirring paddle is started, a refrigerant is continuously and circularly introduced into the jacket, and the temperature of the refrigerant is determined according to the required process; during static crystallization, the stirring paddle stops rotating, and the crystallization process is completed in the jacket through refrigerant circulation.
And 4, step 4: washing, wherein various impurities still exist in crystals generated after crystallization, washing liquid required by the process is introduced through the feed inlet, the barrel is rotated at the moment, and the stirring paddle is started simultaneously, so that the detergent and the materials are fully mixed, and the best washing effect is achieved after multiple times of washing.
And 5: filtering, stopping the rotation of the cylinder body, enabling the filter screen disc to be positioned at the bottom of the cylinder body, and enabling the discharge hole to be screwed to the upper part. At the moment, the equipment can realize the filtration of impurities and detergents under pressure, normal pressure and negative pressure. Specifically, the cylinder body is kept static during normal pressure filtration; the pressure filtration is that the pressure is injected through the feed inlet, and the washing liquid and the impurities are filtered out through the suction filtration port under the action of the pressure; the negative pressure filtration is that the vacuum pumping is carried out through the suction filtration port, the washing liquid and impurities in the material are subjected to negative pressure suction filtration, and the filtrate can be directly discharged from the bottom and also can pass through the feeding pipeline on the side of the cylinder body.
Step 6: drying and breakage, drying the material, keeping the heat medium circulation in the clamp cover, through lasting rotatory barrel, making the material and section of thick bamboo wall fully contact the heat transfer and dry, in the drying process, the vacuum port lasts the evacuation operation and takes out impurity gas from in order to guarantee crystal purity, and breaker opens in the whole drying process, and the bold crystal passes through the broken even fritter crystal that becomes of broken sword.
(III) advantageous effects
The embodiment of the invention provides multifunctional high-purity seven-in-one chemical and pharmaceutical equipment and a manufacturing process thereof. The method has the following beneficial effects:
1. the whole machine integrated process can complete a plurality of process flows of reaction, concentration, crystallization, filtration, washing, drying, crushing and the like, can improve the working efficiency, and simultaneously has small occupied area and small investment and is convenient to implement.
2. The sealing performance can be improved. The sealing performance of the whole device is improved by adding the crushing cutter mechanical sealing ring, the clamping sleeve end mechanical sealing ring, the suction filtration port mechanical sealing ring and the vacuum port mechanical sealing ring. The material business turn over, the business turn over of cold and hot medium and the business turn over of inside liquid are all separated each other, have improved the sealed effect of each tie point simultaneously, have greatly improved the holistic sealing performance of equipment, and product purity is higher simultaneously.
3. Through setting up rotation axis power transmission device and making its stirring of barrel in rotatory process and breaker can open the operation simultaneously, equipment efficiency is high and product purity is higher.
4. Be provided with on the barrel and press from both sides the corresponding shallow dimple column structure of cover, effectively improved the heat transfer of clamp cover side and barrel inboard, scale deposit and blocking phenomenon have been avoided to less protrusion height simultaneously, and the whole heat exchange efficiency of equipment greatly improves, makes crystallization, concentration, drying efficiency obtain improving.
Drawings
FIG. 1 is a schematic structural view of the present invention;
FIG. 2 is a schematic cross-sectional view of the structure of the present invention;
FIG. 3 is a schematic cross-sectional view of the filter device according to the present invention;
fig. 4 is an enlarged schematic view of the structure of the present invention.
In the figure: the device comprises a stirrer motor 1, a stirrer speed reducer 2, a stirring paddle 3, a crushing knife 4, a crushing knife motor 5, a crushing knife speed reducer 6, a jacket liquid inlet 7, a crushing knife mechanical seal ring 8, a jacket end mechanical seal ring 9, a barrel 10, a barrel speed reducer 11, a barrel rotating motor 12, a jacket liquid outlet 13, a driving wheel 14, a bearing seat 15, a discharge hole 16, a suction filtration rod 17, a jacket 18, a sealing static seat 19, a suction filtration port mechanical seal ring 19.1, a vacuum port mechanical seal ring 20, a feed hole 21, a vacuum port 22, a filter screen disc 23, a liquid discharge pipe 24, a frame 25 and a suction filtration port 26.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all, embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Referring to the attached drawings 1-4, the multifunctional high-purity seven-in-one chemical and pharmaceutical equipment comprises a rack 25 and a barrel 10 rotatably arranged on the rack 25, wherein a jacket 18 is sleeved on the barrel 10, so that jacket liquid, namely cold and hot media, can heat and cool the barrel 10 conveniently, sleeves are arranged on two sides of the barrel 10, and the two sleeves are rotatably connected in a bearing seat 15 arranged on the rack 25.
In this embodiment, as shown in fig. 1, a driving wheel 14 is disposed on the sleeve on the left side, the driving wheel 14 is connected to the driving shaft of the barrel speed reducer 11 through a belt, the barrel speed reducer 11 is connected to the driving shaft of the barrel rotating motor 12, and the rotation of the barrel rotating motor 12 is reduced by disposing the barrel speed reducer 11, so that the torque of the barrel rotating motor 12 is increased and the rotation effect is improved.
In this embodiment, as shown in fig. 1, one end of the sleeve on the left side is communicated with the jacket 18, the other end of the sleeve on the left side is movably inserted with the jacket liquid inlet 7 and the jacket liquid outlet 13, the jacket liquid inlet 7 and the jacket liquid outlet 13 are connected to the frame 25 through the first support, the movable insertion end of the sleeve on the left side is provided with the jacket end mechanical seal ring 9, the sleeve on the right side is provided with the feed pipe, one end of the feed pipe extends into the cylinder 10 and is connected with the plurality of filter rods 17 in a penetrating manner, the other end of the feed pipe is movably inserted with the feed port 21 and the vacuum port 22, the feed port 21 and the vacuum port 22 are connected to the frame 25 through the second support, and the movable insertion end of the feed pipe is provided with the vacuum port mechanical.
In this embodiment, as shown in fig. 1, a discharge port 16 is connected to the upper end of the cylinder 10 in a penetrating manner, a sealing cover is disposed on the discharge port 16, a liquid discharge pipe 24 is connected to the bottom wall of the cylinder 10 in a penetrating manner, the other end of the liquid discharge pipe 24 is connected to the right casing pipe in a penetrating manner, a sealing stationary seat 19 is movably sleeved on the right casing pipe, a through hole corresponding to the sealing stationary seat 19 is formed in the casing pipe, a liquid suction pipe is connected to the lower end of the sealing stationary seat 19 in a penetrating manner, the liquid suction pipe penetrates through the frame 25 and is connected with a suction port 26, a mechanical sealing ring 19.1 of the suction port is disposed.
In this embodiment, as shown in fig. 1, a filter screen disc 23 is provided at the lower end of the inner wall of the cylinder 10 for solid-liquid separation.
In this embodiment, as shown in fig. 2, be provided with agitating unit and breaker on the both ends lateral wall respectively around barrel 10, agitating unit includes agitator motor 1, agitator speed reducer 2 and stirring rake 3, agitator motor 1's drive shaft connection agitator speed reducer 2, the drive shaft of agitator speed reducer 2 passes the lateral wall that presss from both sides cover 18 and barrel 10 and is connected with a plurality of stirring rakes 3, can drive stirring rake 3 through agitator motor 1 and rotate, can stir the material after stirring rake 3 rotates, can reduce the rotational speed improvement moment of torsion of agitator motor 1 through agitator speed reducer 2.
In this embodiment, as shown in fig. 2, the breaker includes broken sword motor 5, broken sword speed reducer 6 and broken sword 4, the drive shaft of broken sword motor 5 is connected with broken sword speed reducer 6, the drive shaft of broken sword speed reducer 6 passes the lateral wall that presss from both sides cover 18 and barrel 10 and is connected with a plurality of broken sword 4, can drive broken sword 4 through broken sword motor 5 and rotate, thereby make broken sword 4 rotate and carry out the breakage to the material, can reduce the rotational speed improvement moment of torsion of broken sword motor 5 through broken sword speed reducer 6, and the junction of broken sword speed reducer 6 and barrel 10 is provided with broken sword mechanical seal 8, and sealing performance is improved.
In this embodiment, be provided with rotation axis power transmission device on the sleeve pipe, rotation axis power transmission device in this scheme is the same with the rotation axis power transmission device among the multi-functional drying equipment with explosion-proof type rotation axis power transmission device that china utility model CN200520043844.0 discloses, rotation axis power transmission device can make barrel 10 at rotatory in-process, broken sword motor 5 and agitator motor 1's electric line can not follow the commentaries on classics because of the rotation, the stirring thick liquid 3 and the work of opening simultaneously of broken sword 4 of having guaranteed that barrel 10 installs, the equipment efficiency has greatly been improved.
The sealing performance of the whole device is improved by adding the crushing cutter mechanical sealing ring 8, the jacket end mechanical sealing ring 9, the suction filtration port mechanical sealing ring 19.1 and the vacuum port mechanical sealing ring 20. The material business turn over, the business turn over of cold and hot medium and the business turn over of inside liquid are all separated each other, have improved the sealed effect of each tie point simultaneously, have greatly improved the holistic sealing performance of equipment, and product purity is higher simultaneously.
In this embodiment, as shown in fig. 4, the barrel 10 is provided with a dimple structure corresponding to the jacket 18, so that heat exchange between the jacket 18 side and the inner side of the barrel 10 is effectively improved, and meanwhile, the small protruding height avoids scaling and blocking, the overall heat exchange efficiency of the equipment is greatly improved, and the crystallization, concentration and drying efficiency is improved.
In this embodiment, in the drying process, barrel 10 lasts rotatoryly, treats the inner wall contact heat transfer of dry crystal and barrel 10, and broken sword is opened simultaneously, because barrel 10 keeps rotatory, and its drying efficiency is showing and is improving during consequently broken, simultaneously because barrel 10 is rotatory the broken sword constantly with the bulk crystal breakage simultaneously, consequently the drying effect of final device is good and the purity of product is higher.
The specific pharmaceutical process steps are as follows:
first step reaction
The material enters the cylinder 10 through the feed inlet 21, a heating medium is introduced into the jacket 18 through the jacket liquid inlet 7 according to the process requirement, at the moment, the heating medium with the temperature required by the process flows in the jacket 18 in a circulating manner through the jacket liquid inlet 7 and the jacket liquid outlet 13, the cylinder 10 is rotated by a proper angle through the driving shaft of the cylinder speed reducer 11, a plurality of groups of mechanical seals act in the rotating process of the cylinder 10 to keep the cylinder 10 stable, meanwhile, the stirring paddle 3 required by the material reaction is positioned at the bottom of the cylinder 10 at the moment, the rotating speed adjustable range of the stirring paddle 3 is 0-480r/min, and the material is fully reacted in the cylinder 10 through the mixing action of the stirring paddle 3.
Second step concentration and filtration
After the material reaction is finished, stirring is stopped or started, the heat medium with the temperature required by the process is continuously introduced into the jacket 18 for circulation, meanwhile, the inner vacuumizing operation is carried out on the cylinder 10 through the vacuumizing port 26, liquid substances generated in the heating and concentrating process are pumped away, if water vapor and impurity gas are generated in the concentrating process, the simultaneous vacuumizing operation can also be carried out through the vacuumizing port 26 and the vacuum port 22, the filter screen disc 23 is arranged in the device, and crystals can be prevented from being discharged during the concentrating and vacuumizing operation. The heating and vacuumizing time is determined according to the process requirements, and whether the sample meets the concentration requirement or not can be detected by sampling a small amount of the sample at the discharge port.
Third step of crystallization
The barrel 10 can perform both dynamic crystallization and static crystallization operations. During dynamic crystallization, the stirring paddle 3 is started, a refrigerant is continuously and circularly introduced into the jacket 18, and the temperature of the refrigerant is determined according to the required process; during static crystallization, the stirring paddle 3 stops rotating, and the crystallization process is completed in the jacket 18 through refrigerant circulation.
The fourth step of washing
The crystal produced after crystallization still has a plurality of impurities, the washing liquid required by the process is introduced through the feed inlet 21, at the moment, the cylinder 10 is rotated, and the stirring paddle 3 is started simultaneously, so that the washing agent and the materials are fully mixed, and the best washing effect is achieved after multiple times of washing.
The fifth step of filtration
The rotation of the cylinder 10 is stopped, so that the filter screen disc 23 is positioned at the bottom of the cylinder 10, and the discharge port 16 is screwed to the upper part. At the moment, the equipment can realize the filtration of impurities and detergents under pressure, normal pressure and negative pressure. Specifically, the cylinder 10 is kept still during normal pressure filtration; the pressure filtration is that the pressure is injected through the feed inlet 21, and the washing liquid and the impurities are filtered out through the suction filtration port 26 due to the pressure; the negative pressure filtration is that the vacuum pumping is carried out through the pumping port 26, the washing liquid, impurities and the like in the materials are subjected to negative pressure pumping filtration, and the filtrate can be directly discharged from the bottom or discharged through a feeding pipeline on the side of the cylinder 10.
The sixth step of drying and crushing
The material is dried, the heat medium circulation is kept in the jacket 18, the material is dried by fully contacting and exchanging heat with the cylinder wall through continuously rotating the cylinder body 10, the vacuum port 22 continuously performs vacuum pumping operation to pump away impurity gas so as to ensure the purity of crystals, the crushing device is opened in the whole drying process, and large crystals are crushed into uniform small crystals through the crushing knife 4.
It is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising an … …" does not exclude the presence of other identical elements in a process, method, article, or apparatus that comprises the element.
The above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (10)
1. A multifunctional high-purity seven-in-one chemical and pharmaceutical equipment and its manufacturing process comprises a frame;
and a cylinder rotatably arranged on the frame;
the method is characterized in that: the barrel is sleeved with a jacket, sleeves are arranged on two sides of the barrel, and the two sleeves are rotatably connected in a bearing seat arranged on the rack;
the driving wheel is arranged on the sleeve on the left side and is connected with a driving shaft of the barrel speed reducer through a belt, and the barrel speed reducer is connected with a driving shaft of the barrel rotating motor;
one end of the sleeve positioned on the left side is communicated with the jacket, the other end of the sleeve positioned on the left side is movably inserted with a jacket liquid inlet and a jacket liquid outlet respectively, the jacket liquid inlet and the jacket liquid outlet are connected to the rack through a first support, a feed pipe is arranged in the sleeve positioned on the right side, one end of the feed pipe extends into the cylinder and is connected with a plurality of filter rods in a penetrating manner, the other end of the feed pipe is movably inserted with a feed port and a vacuum port respectively, and the feed port and the vacuum port are connected to the rack through a second support;
the upper end through connection of barrel has the discharge gate, and is provided with sealed lid on the discharge gate, through connection has the fluid-discharge tube on the diapire of barrel, the other end through connection sleeve pipe on right side of fluid-discharge tube, and the activity has cup jointed sealed quiet seat on the sleeve pipe on right side, and has seted up the through-hole corresponding with sealed quiet seat on the sleeve pipe, and the lower extreme through connection of sealed quiet seat has the liquid suction pipe, and the liquid suction pipe passes the frame and is connected with the suction filtration mouth.
2. The multifunctional high-purity seven-in-one chemical and pharmaceutical equipment according to claim 1, characterized in that: the barrel is provided with a shallow concave-pit structure corresponding to the jacket.
3. The multifunctional high-purity seven-in-one chemical and pharmaceutical equipment according to claim 1, characterized in that: the movable insertion end of the sleeve positioned on the left side is provided with a jacket end mechanical sealing ring, and the movable insertion end of the feeding pipe is provided with a vacuum port mechanical sealing ring.
4. The multifunctional high-purity seven-in-one chemical and pharmaceutical equipment according to claim 1, characterized in that: and a suction filtration port mechanical seal ring is arranged between the sealed static seat and the sleeve.
5. The multifunctional high-purity seven-in-one chemical and pharmaceutical equipment and the manufacturing process thereof as claimed in claim 1, wherein: and a filter screen disc is arranged at the lower end of the inner wall of the cylinder body.
6. The multifunctional high-purity seven-in-one chemical and pharmaceutical equipment according to claim 1, characterized in that: still include agitating unit, agitating unit is located the lateral wall of barrel, and agitating unit includes agitator motor, agitator speed reducer and stirring rake, and the agitator speed reducer is connected to the drive shaft of agitator motor, and the drive shaft of agitator speed reducer passes the lateral wall that presss from both sides cover and barrel and is connected with a plurality of stirring rakes.
7. The multifunctional high-purity seven-in-one chemical and pharmaceutical equipment according to claim 1, characterized in that: still include breaker, breaker is located the barrel, and breaker sets up with agitating unit relatively, and breaker includes broken sword motor, broken sword speed reducer and broken sword, and the drive shaft of broken sword motor is connected with broken sword speed reducer, and the drive shaft of broken sword speed reducer passes the lateral wall of pressing from both sides cover and barrel and is connected with a plurality of broken swoves.
8. The multifunctional high-purity seven-in-one chemical and pharmaceutical equipment according to claim 7, characterized in that: and a crushing cutter mechanical sealing ring is arranged at the joint of the crushing cutter speed reducer and the barrel.
9. The multifunctional high-purity seven-in-one chemical and pharmaceutical equipment according to claim 7 or 8, characterized in that: and a rotating shaft power transmission device corresponding to the crushing knife motor and the stirrer motor is arranged on the sleeve.
10. The multifunctional high-purity seven-in-one chemical and pharmaceutical manufacturing process steps of claims 1-9, characterized by comprising the following steps:
step 1: reacting, wherein materials enter the cylinder through the feed inlet, a heating medium is introduced into the jacket through the jacket liquid inlet according to process requirements, the heating medium with the temperature required by the process flows in the jacket in a circulating manner through the jacket liquid inlet and the jacket liquid outlet, the cylinder is rotated by a proper angle through a driving shaft of the cylinder speed reducer, a plurality of groups of mechanical seals act on the rotation process of the cylinder to keep the cylinder stable, meanwhile, a stirring paddle required by material reaction is positioned at the bottom of the cylinder, the rotation speed of the stirring paddle can be adjusted within the range of 0-480r/min, and the materials are fully reacted in the cylinder through the mixing action of the stirring paddles.
Step 2: concentration and filtration, after the material reaction is accomplished, start or stop the stirring, the heat medium that continuously lets in the required temperature of technology circulates in the clamp cover, meanwhile, carry out interior evacuation operation through the suction filter mouth to the barrel, will heat the liquid material that produces in the concentrated process and take out, if there are vapor and impurity gas to produce in the concentrated process, also can carry out the vacuum pumping operation simultaneously through suction filter mouth and vacuum port this moment, the inside filter screen dish that is provided with of device, can prevent to discharge the crystal when concentrating the vacuum pumping operation. The heating and vacuumizing time is determined according to the process requirements, and whether the sample meets the concentration requirement or not can be detected by sampling a small amount of the sample at the discharge port.
And step 3: and (4) crystallizing, wherein the barrel can complete dynamic crystallization and static crystallization operations. During dynamic crystallization, the stirring paddle is started, a refrigerant is continuously and circularly introduced into the jacket, and the temperature of the refrigerant is determined according to the required process; during static crystallization, the stirring paddle stops rotating, and the crystallization process is completed in the jacket through refrigerant circulation.
And 4, step 4: washing, wherein various impurities still exist in crystals generated after crystallization, washing liquid required by the process is introduced through the feed inlet, the barrel is rotated at the moment, and the stirring paddle is started simultaneously, so that the detergent and the materials are fully mixed, and the best washing effect is achieved after multiple times of washing.
And 5: filtering, stopping the rotation of the cylinder body, enabling the filter screen disc to be positioned at the bottom of the cylinder body, and enabling the discharge hole to be screwed to the upper part. At the moment, the equipment can realize the filtration of impurities and detergents under pressure, normal pressure and negative pressure. Specifically, the cylinder body is kept static during normal pressure filtration; the pressure filtration is that the pressure is injected through the feed inlet, and the washing liquid and the impurities are filtered out through the suction filtration port under the action of the pressure; the negative pressure filtration is that the vacuum pumping is carried out through the suction filtration port, the washing liquid and impurities in the material are subjected to negative pressure suction filtration, and the filtrate can be directly discharged from the bottom and also can pass through the feeding pipeline on the side of the cylinder body.
Step 6: drying and breakage, drying the material, keeping the heat medium circulation in the clamp cover, through lasting rotatory barrel, making the material and section of thick bamboo wall fully contact the heat transfer and dry, in the drying process, the vacuum port lasts the evacuation operation and takes out impurity gas from in order to guarantee crystal purity, and breaker opens in the whole drying process, and the bold crystal passes through the broken even fritter crystal that becomes of broken sword.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202010042804.3A CN111167398A (en) | 2020-01-15 | 2020-01-15 | Multifunctional high-purity seven-in-one chemical and pharmaceutical equipment and manufacturing process thereof |
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| CN202010042804.3A CN111167398A (en) | 2020-01-15 | 2020-01-15 | Multifunctional high-purity seven-in-one chemical and pharmaceutical equipment and manufacturing process thereof |
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| CN111167398A true CN111167398A (en) | 2020-05-19 |
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| CN112057890A (en) * | 2020-08-27 | 2020-12-11 | 江苏恒安化工有限公司 | Purification method of 2, 3-difluoro-5-chloropyridine |
| CN112206736A (en) * | 2020-10-23 | 2021-01-12 | 王柳琴 | Multifunctional high-purity seven-in-one chemical and pharmaceutical equipment and manufacturing process thereof |
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