CN112090101B - Preparation process of chemical raw material capable of carrying out fractionation and crystallization production simultaneously - Google Patents

Preparation process of chemical raw material capable of carrying out fractionation and crystallization production simultaneously Download PDF

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Publication number
CN112090101B
CN112090101B CN202011088448.5A CN202011088448A CN112090101B CN 112090101 B CN112090101 B CN 112090101B CN 202011088448 A CN202011088448 A CN 202011088448A CN 112090101 B CN112090101 B CN 112090101B
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crystallization
fractionation
wall
raw materials
fixed mounting
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CN112090101A (en
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张宝甫
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Shandong Yubin New Material Co.,Ltd.
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Shandong Yubin New Material Co ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D3/00Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/009Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping in combination with chemical reactions
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D3/00Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/14Fractional distillation or use of a fractionation or rectification column
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D3/00Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/14Fractional distillation or use of a fractionation or rectification column
    • B01D3/32Other features of fractionating columns ; Constructional details of fractionating columns not provided for in groups B01D3/16 - B01D3/30
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D3/00Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/42Regulation; Control
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D9/00Crystallisation
    • B01D9/004Fractional crystallisation; Fractionating or rectifying columns
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D9/00Crystallisation
    • B01D9/0063Control or regulation

Abstract

The invention discloses a preparation process of chemical raw materials capable of carrying out fractionation and crystallization production simultaneously, which specifically comprises the following steps: s1, material preparation, S2, reaction, S3, evaporative crystallization treatment or fractionation treatment, S4 and raw material collection, and the invention relates to the technical field of chemical raw material production. This can carry out the industrial chemicals preparation technology of fractionating and crystallization production simultaneously, can realize that the production facility integration who will fractionate and evaporation crystallization process is integrated as integration treatment facility, come to handle industrial chemicals simultaneously, low in production cost, the construction of production facility is laborsaving, thereby save manufacturing cost, can realize through adopting mechanical type intermittent type working structure, come to replace to use the solenoid valve to carry out long-time continuation work, can realize simultaneously carrying out the processing production to different types of industrial chemicals through adopting a production facility, fine reaching uses production facility in a flexible way to carry out the purpose of different types of raw materials production, wide in use range.

Description

Preparation process of chemical raw material capable of carrying out fractionation and crystallization production simultaneously
Technical Field
The invention relates to the technical field of chemical raw material production, in particular to a preparation process of a chemical raw material, which can carry out fractional distillation and crystallization production simultaneously.
Background
The chemical raw materials can be generally divided into two categories, namely organic chemical raw materials and inorganic chemical raw materials, wherein the organic chemical raw materials can be divided into alkanes and derivatives thereof, alkenes and derivatives thereof, alkynes and derivatives thereof, quinones, aldehydes, alcohols, ketones, phenols, ethers, anhydrides, esters, organic acids and carboxylates, the inorganic chemical raw materials mainly comprise chemical minerals such as sulfur, sodium, phosphorus, potassium and calcium, coal, petroleum, natural gas, air and water, the chemical raw materials have different forms at normal temperature, so that the processing technology of the chemical raw materials is greatly different, wherein the chemical raw materials dissolved in a solvent need to be prepared into solid crystalline chemical raw materials by adopting a processing method of evaporative crystallization, and a plurality of organic solvents dissolved in the solvent need to be prepared by adopting a multi-stage fractionation mode.
In the existing equipment for producing chemical raw materials, most of the evaporation crystallization process and the fractionation process are directly and separately processed by two mutually independent production equipment, and the processing method has the following defects:
1) the production cost is high, the construction of production facility is time-consuming and laborious, can not realize that the production facility integration of fractionating and evaporative crystallization process is integrated into integrated treatment facility, comes to handle industrial chemicals simultaneously, can not reach through adopting centralized fractionation evaporation equipment, produces the purpose of solid and organic liquid industrial chemicals to production cost can not be saved.
2) Present fractional crystallization technology is when adopting the fractional evaporation tower to carry out raw materials processing, adopt solenoid valve control feed inlet to carry out intermittent type formula blowout atomizing pending raw materials mostly, thereby make the raw materials after the atomizing evaporate or the fractional evaporation handle in high temperature environment, carry out the mode of control through the continuation switch that adopts the solenoid valve, the long-time use of solenoid valve is damaged appears easily, incessant on-off control in long-time high temperature environment, can make the life sharply decline of solenoid valve, consequently, need often carry out the maintenance of solenoid valve and change, waste time and energy, can not realize through adopting mechanical type intermittent type work structure, replace using the solenoid valve to carry out long-time continuation work, thereby bring very big inconvenience for producers's use.
3) The application range is comparatively limited, can only produce same kind of industrial chemicals, and to producing different kinds of industrial chemicals, need change production facility in addition and produce, can not realize carrying out the processing production to different kinds of industrial chemicals simultaneously through adopting a production facility, can't reach the purpose that uses production facility in a flexible way to carry out different kinds of raw materials production to it is very unfavorable to the chemical production enterprise.
Disclosure of Invention
Technical problem to be solved
Aiming at the defects of the prior art, the invention provides a chemical raw material preparation process capable of simultaneously carrying out fractionation and crystallization production, and solves the problems that the conventional chemical raw material fractionation and evaporation process is high in production cost, time and labor are wasted in the construction of production equipment, the production equipment of the fractionation and evaporation and crystallization processes cannot be integrated into integrated treatment equipment to simultaneously treat the chemical raw materials, the maintenance and replacement of an electromagnetic valve are required frequently, the time and the labor are wasted, and the application range is limited.
(II) technical scheme
In order to achieve the purpose, the invention is realized by the following technical scheme: a preparation process of chemical raw materials capable of carrying out fractionation and crystallization production simultaneously comprises the following steps:
s1, weighing and batching raw materials through batching equipment;
s2, adding the raw materials prepared in the step S1 into a reaction vessel, and heating and pressurizing to carry out reaction;
s3, transferring the product of the reaction in the step S2 to a fractional crystallization integrated device, and selecting evaporation crystallization treatment or fractional crystallization treatment according to the type of the preparation raw material;
and S4, after crystallization or fractionation is finished, collecting crystallization solid or collecting the fractionated raw material.
Wherein, the fractionation and crystallization integrated equipment in the step S3 comprises a base pre-embedded and built on the ground, a treatment tower, a fractionation collecting unit and a high-pressure high-temperature steam unit, wherein the top of the base is sequentially and fixedly installed from right to left, a tee cooling unit is fixedly installed on one side of the treatment tower through an installation frame, the top of an inner cavity of the treatment tower is separated by a control chamber through a transverse plate, the bottom of the inner cavity of the treatment tower and the transverse plate are separated into a fractionation chamber and a crystallization chamber through a vertical plate, three leakage nets are fixedly installed on the inner wall of the fractionation chamber, heating components are fixedly installed on the tops of the three leakage nets, a filtering component is arranged on the inner wall of the crystallization chamber, a crystallization collecting box matched with the filtering component is fixedly installed on one side of the treatment tower, a communicated discharge port is arranged on one side of the crystallization collecting box and one side of the inner wall of the treatment tower, and a discharge component matched with the discharge port is fixedly installed on one side of the inner wall of the crystallization collecting box, the top of the treatment tower is respectively communicated with two feeding pipes, and the bottom of the inner wall of the control chamber is provided with an intermittent material control mechanism for controlling the discharging of the two feeding pipes.
Intermittent type formula accuse material mechanism includes fixed mounting seal assembly between the both sides of the install bin and install bin between two inlet pipes of fixed mounting, the bottom of install bin inner wall is connected with the worm through the leg joint, and the equal fixed mounting in both ends of worm has the carousel, the outside of carousel all rotates through rotating and is connected with the movable rod, and the one end of movable rod rotates through the pin and is connected with the baffle, install bin, seal assembly and two inlet pipes are run through in proper order to one side of baffle, and the upper and lower surface of baffle all is stained with sealing rubber pad, there is driving motor one side of install bin inner wall through support fixed mounting, and driving motor's output fixed mounting has the worm wheel with worm engaged with.
Preferably, the sealing assembly comprises a sealing box fixedly installed between the installation box and the feeding pipe, and sealing air bags are fixedly installed at the top and the bottom of the inner wall of the sealing box.
Preferably, the inflator is fixedly installed inside the installation box, and a vent hole of the inflator is communicated with the sealed airbag through a gas guide tube.
Preferably, the heating assembly comprises an installation block fixedly installed on the drain net and an exhaust pipe network fixedly installed at the top of the installation block, an installation groove is formed in the installation block, a steam pipe communicated with the exhaust pipe network is fixedly installed in the installation groove, and at least three exhaust pipe networks are installed on a single heating assembly.
Preferably, one end of the steam pipe, which is far away from the mounting block, is communicated with an air outlet of the high-pressure steam unit, and the air outlet of the high-pressure steam unit is also communicated with the crystallization chamber through an air inlet pipe.
Preferably, the filtering component includes that the filter screen of being connected is rotated with crystallization cavity inner wall one side through rotating the piece and rotates the double cylinder of being connected with crystallization cavity inner wall opposite side through rotating the piece, there is the movable block one side of filter screen bottom through slider sliding connection, and the end that stretches out of double cylinder rotates through the bottom of pin with the movable block to be connected, the inner wall of crystallization cavity and the top fixed mounting that is located double cylinder have the arc dog the same with filter screen movement track.
Preferably, the discharging assembly comprises a discharging cylinder fixedly mounted on one side of the inner wall of the crystallization collecting box, and the extending end of the discharging cylinder is fixedly connected with a sealing stop dog matched with the discharging port.
Preferably, the top of the inner cavity of the crystallization collecting box is fixedly provided with an air pressure unit through a fixing plate, and an air vent of the air pressure unit is respectively communicated with air cylinders in the filtering component and the discharging component through air guide pipes.
Preferably, the bottom of the fractionation chamber is fixedly provided with a discharge inclined plate, the bottom of the crystallization chamber is provided with a material receiving cylinder, and the air inlet of the three-way cooling unit is communicated with the fractionation chamber through an air duct.
Preferably, the bottom of the inner wall of the fractionation collection unit is respectively and fixedly provided with three collection tanks communicated with the three-way cooling unit, the top of the fractionation collection unit is respectively and fixedly provided with a central processing unit and a time relay, and the front of the fractionation collection unit is fixedly provided with a control panel.
(III) advantageous effects
The invention provides a preparation process of chemical raw materials, which can carry out fractionation and crystallization production simultaneously. Compared with the prior art, the method has the following beneficial effects:
(1) the chemical raw material preparation process capable of simultaneously carrying out fractionation and crystallization production comprises the steps of dividing a space between the bottom of an inner cavity of a treatment tower and a transverse plate into a fractionation chamber and a crystallization chamber through a vertical plate, wherein three leakage nets are fixedly arranged on the inner wall of the fractionation chamber, heating components are fixedly arranged on the tops of the three leakage nets, a filtering component is arranged on the inner wall of the crystallization chamber, a crystallization collecting box matched with the filtering component is fixedly arranged on one side of the treatment tower, communicated discharge ports are formed in one side of the crystallization collecting box and one side of the treatment tower, a discharge component matched with the discharge ports is fixedly arranged on one side of the inner wall of the crystallization collecting box, production equipment for fractionating, evaporating and crystallizing processes can be integrated into integrated treatment equipment to simultaneously treat chemical raw materials, and the purpose of producing solid and organic liquid chemical raw materials by adopting centralized fractionation evaporation equipment is well achieved, the production cost is low, and the construction of the production equipment is trouble-saving and labor-saving, so that the production cost is saved.
(2) This can fractionate simultaneously and crystallization production's industrial chemicals preparation technology, intermittent type formula accuse material mechanism includes fixed mounting seal assembly between the both sides of the installation box and the installation box between two inlet pipes of fixed mounting between two inlet pipes and two inlet pipes, the bottom of installation box inner wall is connected with the worm through the leg joint, and the equal fixed mounting in both ends of worm has the carousel, the outside of carousel all rotates through rotating the piece and is connected with the movable rod, and the one end of movable rod is connected with the baffle through the pin rotation, can realize through adopting mechanical type intermittent type work structure, replace to use the solenoid valve to carry out long-time continuation work, fine having avoided the condition emergence that the solenoid valve used for a long time to damage or life sharply descends, need not often to carry out the maintenance of solenoid valve and change, time saving and labor saving, thereby manufacturer's use has been made things convenient for greatly.
(3) This can be fractionated simultaneously and chemical industry raw materials preparation technology of crystallization production can realize carrying out the processing production to different types of chemical industry raw materials simultaneously through adopting a production facility, fine reaching and using the purpose that production facility carries out different types of raw materials production in a flexible way, application range is wide, need not to trade production facility in addition and produce, just can produce different types of chemical industry raw materials, and to producing different types of chemical industry raw materials to it is very useful to the chemical production enterprise.
Drawings
FIG. 1 is a schematic structural view of the present invention;
FIG. 2 is a cross-sectional view of a tower construction of the present invention;
FIG. 3 is an enlarged view of a portion of the invention at A in FIG. 2;
FIG. 4 is an enlarged view of a portion of the present invention at B of FIG. 2;
FIG. 5 is a cross-sectional view of an intermittent material control mechanism of the present invention;
FIG. 6 is an enlarged view of a portion of the invention at C of FIG. 5;
FIG. 7 is a schematic view of the worm gear and worm of the present invention;
FIG. 8 is a top plan view of the worm and dial arrangement of the present invention;
FIG. 9 is a schematic view of the heating assembly of the present invention;
FIG. 10 is a schematic view of the filter net according to the present invention;
FIG. 11 is a cross-sectional view of a fractionation collector unit according to the present invention;
FIG. 12 is a schematic structural diagram of the three-way cooling unit of the present invention.
In the figure, 1 base, 2 treatment tower, 3 fractionation collection unit, 4 high pressure high temperature steam unit, 5 three-way cooling unit, 6 control room, 7 fractionation chamber, 8 crystallization chamber, 9 leakage net, 10 heating component, 101 mounting block, 102 exhaust net pipe, 103 mounting groove, 104 steam pipe, 11 filtering component, 111 filter net, 112 two-way cylinder, 113 movable block, 114 arc block, 12 crystallization collection box, 13 discharge hole, 14 discharge component, 141 discharge cylinder, 142 sealing block, 15 feed pipe, 16 intermittent material control mechanism, 161 mounting box, 162 sealing component, 1621 sealing box, 1622 sealing air bag, 163 worm, 164 rotary disc, 165 movable rod, 166 baffle, 167 sealing rubber pad, 168 driving motor, 169 worm wheel, 1610 inflator, 17 air inlet pipe, 18 air pressure unit, 19 inclined plate, 20 material receiving cylinder, 21 collection tank, 22 central processing unit, 23 time relay, And 24, a control panel.
Detailed Description
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 only a part of the embodiments of the present invention, and not all of the embodiments. 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 fig. 1-12, an embodiment of the present invention provides a technical solution: a preparation process of chemical raw materials capable of carrying out fractionation and crystallization production simultaneously comprises the following steps:
s1, weighing and batching raw materials through batching equipment;
s2, adding the raw materials prepared in the step S1 into a reaction vessel, and heating and pressurizing to carry out reaction;
s3, transferring the product of the reaction in the step S2 to a fractional crystallization integrated device, and selecting evaporation crystallization treatment or fractional crystallization treatment according to the type of the preparation raw material;
s4, after crystallization or fractionation is finished, collecting crystallization solids or collecting fractionated raw materials;
wherein, the fractionation and crystallization integrated equipment in the step S3 comprises a base 1 pre-buried and built on the ground, a processing tower 2, a fractionation and collection unit 3 and a high-pressure high-temperature steam unit 4 which are fixedly installed on the top of the base 1 from right to left in sequence, the fractionation and collection unit 3 comprises a collection box and a liquid pump installed on the top of the collection box, the high-pressure high-temperature steam unit 4 is a multi-stage temperature control multi-output high-temperature steam engine with the model of LS-2588S, a three-way cooling unit 5 is fixedly installed on one side of the processing tower 2 through a mounting rack, the three-way cooling unit 5 is a condenser with three built-in cooling mechanisms with the model of SKLN, the top of the inner cavity of the processing tower 2 is separated by a transverse plate to form a control chamber 6, a fractionation chamber 7 and a crystallization chamber 8 are separated by a vertical plate between the bottom of the inner cavity of the processing tower 2 and the transverse plate, and three leakage nets 9 are fixedly installed on the inner wall of the fractionation chamber 7, the top of the three leakage nets 9 is fixedly provided with a heating component 10, the inner wall of the crystallization chamber 8 is provided with a filtering component 11, one side of the treatment tower 2 is fixedly provided with a crystallization collecting box 12 matched with the filtering component 11, one side of the crystallization collecting box 12 and one side of the treatment tower 2 are provided with a communicated discharging port 13, one side of the inner wall of the crystallization collecting box 12 is fixedly provided with a discharging component 14 matched with the discharging port 13, the top of the treatment tower 2 is respectively communicated with two feeding pipes 15, the bottom of the inner wall of the control chamber 6 is provided with an intermittent material control mechanism 16 for controlling the discharging of the two feeding pipes 15, the top of the inner cavity of the crystallization collecting box 12 is fixedly provided with an air pressure unit 18 through a fixing plate, the air pressure unit 18 adopts an air pump with the model of AST-230, and air vents of the air pressure unit 18 are respectively communicated with air cylinders in the filtering component 11 and the discharging component 14 through air ducts, the bottom fixed mounting of fractionation chamber 7 has ejection of compact swash plate 19, and the bottom of crystallization chamber 8 has been placed and has been connect material jar 20, the air inlet of tee bend cooling unit 5 all communicates with fractionation chamber 7 through the air duct, the bottom of fractionation collection unit 3 inner wall respectively fixed mounting have with the three accumulator tank 21 that tee bend cooling unit 5 is linked together, and the top of fractionation collection unit 3 respectively fixed mounting have central processing unit 22 and time relay 23, central processing unit 22's model is ARM9, time relay 23's model is DS-21, the front fixed mounting of fractionation collection unit 3 has control panel 24.
As shown in fig. 5-8, the intermittent material control mechanism 16 includes a mounting box 161 fixedly mounted between the two feeding pipes 15, and a sealing assembly 162 fixedly mounted between two sides of the mounting box 161 and the two feeding pipes 15, a worm 163 is rotatably connected to the bottom of the inner wall of the mounting box 161 through a bracket, and both ends of the worm 163 are fixedly provided with a turntable 164, the outer side of the turntable 164 is rotatably connected with a movable rod 165 through a rotating member, and one end of the movable rod 165 is rotatably connected with a baffle 166 through a pin, one side of the baffle 166 sequentially penetrates through the installation box 161, the sealing assembly 162 and the two feeding pipes 15, sealing rubber pads 167 are adhered to the upper and lower surfaces of the baffle 166, a driving motor 168 is fixedly installed on one side of the inner wall of the installation box 161 through a bracket, the driving motor 168 is a servo motor with the model number of 40CB010C-500000, and a worm wheel 169 engaged with the worm 163 is fixedly installed at an output end of the driving motor 168.
As shown in fig. 6, the sealing assembly 162 includes a sealing case 1621 fixedly installed between the installation case 161 and the feeding pipe 15, sealing airbags 1622 fixedly installed at the top and bottom of the inner wall of the sealing case 1621, an inflator 1610 fixedly installed inside the installation case 161, the inflator 1610 being of a model FAQ3-AE2A, and a vent hole of the inflator 1610 communicating with the sealing airbag 1622 through a gas guide tube.
As shown in fig. 2 and 9, the heating assembly 10 includes an installation block 101 fixedly installed on the leakage net 9 and an exhaust pipe network 102 fixedly installed on the top of the installation block 101, an installation groove 103 is opened inside the installation block 101, a steam pipe 104 communicated with the exhaust pipe network 102 is fixedly installed inside the installation groove 103, at least three exhaust pipe networks 102 are installed on a single heating assembly 10, one end of the steam pipe 104 far away from the installation block 101 is communicated with the air outlet of the high-pressure steam unit 4, and the air outlet of the high-pressure steam unit 4 is further communicated with the crystallization chamber 8 through an air inlet pipe 17.
As shown in fig. 3 and 10, the filtering assembly 11 includes a filtering net 111 rotatably connected to one side of the inner wall of the crystallization chamber 8 through a rotating member, and a double-stroke cylinder 112 rotatably connected to the other side of the inner wall of the crystallization chamber 8 through a rotating member, the double-stroke cylinder 112 is a double-forming cylinder of SMC type, one side of the bottom of the filtering net 111 is slidably connected to a movable block 113 through a sliding member, an extending end of the double-stroke cylinder 112 is rotatably connected to the bottom of the movable block 113 through a pin, and an arc-shaped stopper 114 having the same movement track as that of the filtering net 111 is fixedly installed on the inner wall of the crystallization chamber 8 and on the top of the double-stroke cylinder 112.
As shown in FIG. 4, the discharging assembly 14 includes a discharging cylinder 141 fixedly installed on one side of the inner wall of the crystallization collecting box 12, the discharging cylinder 141 is a cylinder with CDQ2A25-5DMZ, and the extending end of the discharging cylinder 141 is fixedly connected with a sealing stopper 142 adapted to the discharging port 13.
The specific operation flow is as follows:
before use, firstly, the whole system is electrified through an external power supply, then a control program is recorded into the central processing unit 22 and the time relay 23 through the control panel 24, the control program comprises temperature values of four high-temperature steams discharged by the high-pressure steam unit 4, wherein the steam temperature value in the crystallization cavity 8 is the lowest and is recorded as the temperature T1The temperature values discharged into the fractionating chamber 7 are increased from top to bottom in sequence and are marked as T2、T3And T4Three cooling temperature values of the three-way cooling unit 5, the working time of the driving motor 168 and the working time of the two-way cylinder 112 are recorded.
And (3) fractional distillation treatment: firstly, chemical raw materials to be fractionated are sprayed into a fractionation chamber 7 through a feeding pipe 15 and an atomizing nozzle at the front end of the feeding pipe 15, at the moment, a control panel 24 is operated, a central processing unit 22 controls a driving motor 168 to start working, the driving motor 168 drives two rotary tables 164 to rotate through a worm wheel 169 and a worm 163 respectively, the rotary tables 164 drive two movable rods 165 to pull a baffle 166 to slide left and right in the feeding pipe 15, the movable ends of the two movable rods 165 are arranged on the two rotary tables 164 at positions 180 degrees apart, so that the two baffle 166 synchronously retract and extend, the two feeding pipes 15 are closed or opened simultaneously, the raw materials in the two feeding pipes 15 are fed intermittently along with the continuous movement of the driving motor 168, and the central processing unit 22 controls a high-pressure steam unit 4 to make three groups of temperature T and T have the same temperature2、T3And T4The high-temperature gas is sequentially introduced into the three heating assemblies 10 arranged in the fractionating chamber 7 from top to bottom, and enters the exhaust pipe network 102 of the three groups of heating assemblies 10 through the steam pipe 104The body is introduced into the fractionating chamber 7 through the exhaust pipe network 102, the temperature of the sprayed atomized raw material passing through the uppermost part of the fractionating chamber 7 is T2The heating assembly 10 of (1) makes the most easily gasified raw material changed into gas and steam to be pumped out and condensed by the three-way cooling unit 5 together, then the gas is collected by the collecting tank 21 and passes through the middle part of the fractionating chamber 7 with the temperature T3The heating unit 0 of (1) makes the most easily gasified raw material changed into gas and steam to be pumped out and condensed by the three-way cooling unit 5 together, and then collected by the collecting tank 21, and the temperature of the uppermost part passing through the fractionating chamber 7 is T4The heating component 10 of (1) makes the most easily gasified raw material become gas and be pumped away and condensed by the three-way cooling unit 5 together with steam, then collect through the collection tank 21, and the raw material that does not gasify can flow into the bottommost of the fractionating chamber 7 under the action of gravity, flows into the recovery pipe through the discharge sloping plate 19, exports and recycles.
And (3) evaporation crystallization treatment: chemical raw materials to be subjected to evaporative crystallization treatment are sprayed into the crystallization chamber 8 through the feeding pipe 15 and an atomizing nozzle at the front end of the feeding pipe 15, the control panel 24 is operated at the moment, the central processor 22 controls the driving motor 168 to start working, the driving motor 168 can drive the two turntables 164 to rotate through the worm wheel 169 and the worm 163 respectively, the turntables 164 drive the two movable rods 165 to pull the baffle 166 to slide left and right in the feeding pipe 15, the positions of the movable ends of the two movable rods 165 mounted on the two turntables 164 are 180 degrees apart, therefore, the two baffle 166 move synchronously, the two feeding pipes 15 are closed or opened, the raw materials in the two feeding pipes 15 are fed intermittently along with the continuous movement of the driving motor 168, and the central processor 22 controls the high-pressure steam unit 4 to set the temperature T1The high-temperature gas let in and install in crystallization cavity 8, the raw materials can be contacted with high-temperature steam closely, moisture is gasified fast, the crystal of appearing can fall into on filter screen 111, operation control panel 24 this moment, make central processing unit 22 control atmospheric pressure unit 18 and the inside solenoid valve of double-stroke cylinder 112 intercommunication pipeline begin to work, make double-stroke cylinder 112 begin to carry out the circulation of little stroke and stretch out and withdraw, thereby drive filter screen 111 through movable block 113 and carry out the vibration of small angle, this vibration rangeEnclose lessly, can not appear big crystallization raw materials and fall into from the gap between filter screen 111 and the 8 inner walls of crystallization chamber, can realize vibrating the screening to the raw materials that the crystallization got off like this, avoid piling up, make the crystallization of small particle size fall into through filter screen 111 in connecing material jar 20, open the sealing door of handling tower 2 bottom take away connect material jar 20 can, and the large granule crystallization that does not pass through filter screen 111 can be on filter screen 111, after the whole crystallization process of raw materials is finished, control double-stroke cylinder 112 carries out the large formation and stretches out, and control ejection of compact cylinder 141 withdraws, make sealed dog 142 slide from discharge gate 13, can open discharge gate 13, the large granule crystallization that does not filter slides in crystal collecting box 12, the clearance is accomplished the back, control ejection of compact cylinder 141 and double-stroke cylinder 112 reset, can accomplish the evaporation crystallization process.
And those not described in detail in this specification are well within the skill of those in the art.
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.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.

Claims (4)

1. A preparation process of chemical raw materials capable of carrying out fractionation and crystallization production simultaneously is characterized in that: the preparation process specifically comprises the following steps:
s1, weighing and batching raw materials through batching equipment;
s2, adding the raw materials prepared in the step S1 into a reaction vessel, and heating and pressurizing to carry out reaction;
s3, transferring the product of the reaction in the step S2 to a fractional crystallization integrated device, and selecting evaporation crystallization treatment or fractional crystallization treatment according to the type of the preparation raw material;
s4, after crystallization or fractionation is finished, collecting crystallization solids or collecting fractionated raw materials;
wherein, step S3 in fractionation crystallization integration equipment, including pre-buried base (1) of building on the ground and base (1) top from the right side to left fixed mounting' S processing tower (2), fractionation collection unit (3) and high-pressure high temperature steam unit (4) in proper order, there are tee bend cooling unit (5) one side of processing tower (2) through mounting bracket fixed mounting, and there is control room (6) at the top of processing tower (2) inner chamber through the diaphragm partition, cut apart into fractionation cavity (7) and crystallization cavity (8) through the riser between the bottom of processing tower (2) inner chamber and the diaphragm, and the inner wall fixed mounting of fractionation cavity (7) has three to leak net (9), three the equal fixed mounting in top of leaking net (9) has heating element (10), and the inner wall of crystallization cavity (8) is provided with filtering element (11), one side fixed mounting of processing tower (2) has the crystallization collection box (S) with filtering element (11) looks adaptation (11) (3), (11) looks adaptation 12) One side of the crystallization collection box (12) and one side of the treatment tower (2) are provided with a communicated discharge port (13), one side of the inner wall of the crystallization collection box (12) is fixedly provided with a discharge component (14) matched with the discharge port (13), the top of the treatment tower (2) is respectively communicated with two feed pipes (15), and the bottom of the inner wall of the control chamber (6) is provided with an intermittent material control mechanism (16) for controlling the discharge of the two feed pipes (15);
the intermittent type formula accuse material mechanism (16) including fixed mounting in the both sides of installing bin (161) and installing bin (161) between two inlet pipes (15) and fixed mounting seal assembly (162) between two inlet pipes (15), the bottom of installing bin (161) inner wall is connected with worm (163) through the support rotation, and the equal fixed mounting in both ends of worm (163) has carousel (164), the outside of carousel (164) all is connected with movable rod (165) through the rotation of rotating, and the one end of movable rod (165) is connected with baffle (166) through the pin rotation, install bin (161), seal assembly (162) and two inlet pipes (15) are run through in proper order to one side of baffle (166), and the upper and lower surface of baffle (166) all is stained with sealing rubber pad (167), there is driving motor (168) one side of installing bin (161) inner wall through support fixed mounting, a worm wheel (169) meshed with the worm (163) is fixedly arranged at the output end of the driving motor (168);
the sealing assembly (162) comprises a sealing box (1621) fixedly installed between the installation box (161) and the feeding pipe (15), sealing air bags (1622) are fixedly installed at the top and the bottom of the inner wall of the sealing box (1621), an inflator (1610) is fixedly installed in the installation box (161), and a vent hole of the inflator (1610) is communicated with the sealing air bags (1622) through an air guide pipe;
the heating assembly (10) comprises an installation block (101) fixedly installed on the leakage net (9) and an exhaust pipe network (102) fixedly installed at the top of the installation block (101), an installation groove (103) is formed in the installation block (101), a steam pipe (104) communicated with the exhaust pipe network (102) is fixedly installed in the installation groove (103), at least three exhaust pipe networks (102) are installed on a single heating assembly (10), one end, far away from the installation block (101), of the steam pipe (104) is communicated with a gas outlet of the high-pressure steam unit (4), and the gas outlet of the high-pressure steam unit (4) is communicated with the crystallization chamber (8) through a gas inlet pipe (17);
the filtering component (11) comprises a filtering net (111) which is rotatably connected with one side of the inner wall of the crystallization cavity (8) through a rotating piece and a double-stroke cylinder (112) which is rotatably connected with the other side of the inner wall of the crystallization cavity (8) through a rotating piece, one side of the bottom of the filtering net (111) is slidably connected with a movable block (113) through a sliding piece, the extending end of the double-stroke cylinder (112) is rotatably connected with the bottom of the movable block (113) through a pin, and an arc-shaped stop block (114) which has the same movement track as that of the filtering net (111) is fixedly arranged on the inner wall of the crystallization cavity (8) and is positioned at the top of the double-stroke cylinder (112);
the discharging assembly (14) comprises a discharging cylinder (141) fixedly mounted on one side of the inner wall of the crystallization collecting box (12), and the extending end of the discharging cylinder (141) is fixedly connected with a sealing stop block (142) matched with the discharging port (13).
2. The process for preparing chemical raw materials capable of being simultaneously fractionated and crystallized according to claim 1, wherein: the top of the inner cavity of the crystallization collecting box (12) is fixedly provided with an air pressure unit (18) through a fixing plate, and the air vent of the air pressure unit (18) is respectively communicated with the air cylinders in the filtering component (11) and the discharging component (14) through air ducts.
3. The process for preparing chemical raw materials capable of being simultaneously fractionated and crystallized according to claim 1, wherein: the bottom of the fractionation chamber (7) is fixedly provided with a discharge sloping plate (19), the bottom of the crystallization chamber (8) is provided with a material receiving cylinder (20), and the air inlet of the three-way cooling unit (5) is communicated with the fractionation chamber (7) through an air duct.
4. The process for preparing chemical raw materials capable of being simultaneously fractionated and crystallized according to claim 1, wherein: the bottom of fractionation collection unit (3) inner wall respectively fixed mounting have with three accumulator tank (21) that tee bend cooling unit (5) are linked together, and the top of fractionation collection unit (3) respectively fixed mounting have central processing unit (22) and time relay (23), the front fixed mounting of fractionation collection unit (3) has control panel (24).
CN202011088448.5A 2020-10-13 2020-10-13 Preparation process of chemical raw material capable of carrying out fractionation and crystallization production simultaneously Active CN112090101B (en)

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