CN115282914A - Epoxy resin production process - Google Patents

Epoxy resin production process Download PDF

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Publication number
CN115282914A
CN115282914A CN202210970390.XA CN202210970390A CN115282914A CN 115282914 A CN115282914 A CN 115282914A CN 202210970390 A CN202210970390 A CN 202210970390A CN 115282914 A CN115282914 A CN 115282914A
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CN
China
Prior art keywords
stirring
kettle
oil
seat
liquid
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Pending
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CN202210970390.XA
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Chinese (zh)
Inventor
刘明星
孙学武
周静静
杨敏
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Anhui Jiangxing Lianchuang New Materials Technology Co ltd
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Anhui Jiangxing Lianchuang New Materials Technology Co ltd
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Priority to CN202210970390.XA priority Critical patent/CN115282914A/en
Publication of CN115282914A publication Critical patent/CN115282914A/en
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/18Stationary reactors having moving elements inside
    • 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
    • B01D3/10Vacuum distillation
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01FMIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F27/00Mixers with rotary stirring devices in fixed receptacles; Kneaders
    • B01F27/80Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a substantially vertical axis
    • B01F27/95Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a substantially vertical axis with stirrers having planetary motion, i.e. rotating about their own axis and about a sun axis
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01FMIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F33/00Other mixers; Mixing plants; Combinations of mixers
    • B01F33/80Mixing plants; Combinations of mixers
    • B01F33/82Combinations of dissimilar mixers
    • B01F33/821Combinations of dissimilar mixers with consecutive receptacles
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01FMIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F35/00Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
    • B01F35/10Maintenance of mixers
    • B01F35/12Maintenance of mixers using mechanical means
    • B01F35/123Maintenance of mixers using mechanical means using scrapers for cleaning mixers
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01FMIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F35/00Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
    • B01F35/30Driving arrangements; Transmissions; Couplings; Brakes
    • B01F35/31Couplings
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0006Controlling or regulating processes
    • B01J19/0013Controlling the temperature of the process
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0053Details of the reactor
    • B01J19/0066Stirrers

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)

Abstract

The invention belongs to the technical field of resin production, in particular to an epoxy resin production process, and a reaction kettle used in the process of preparing epoxy resin, which comprises a kettle body, a motor, a coil, a fixed seat, a supporting seat, a protective cover and a stirring part, wherein the kettle body is provided with a stirring part; according to the invention, the barrel body is heated through the coil, so that the solution is heated, meanwhile, the motor rotates to drive the stirring shaft to rotate, so that the first stirring rod and the second stirring rod are driven to rotate, the first stirring rod rotates, the rotation direction is opposite to that of the stirring shaft, so that surrounding liquid is driven to rotate and be thrown out, and then the liquid in different flow directions can collide with each other, so that the mutual mixing of the liquid in the middle is increased, meanwhile, the second stirring rod stirs the outer ring and a human body, the mixing degree of the alkali liquor and the liquid dripped into the reaction kettle is improved under the combined action, the reaction speed is accelerated, and the production of epoxy resin is facilitated.

Description

Epoxy resin production process
Technical Field
The invention belongs to the technical field of resin production, and particularly relates to an epoxy resin production process.
Background
The epoxy resin is a high molecular polymer, is a general name of a polymer containing more than two epoxy groups in a molecule, and is a polycondensation product of epichlorohydrin and bisphenol A or polyol; the bisphenol A epoxy resin has the largest yield and the most complete variety, and new modified varieties are continuously increased, so that the quality is continuously improved; 1, when resin with larger molecular weight is needed, firstly dissolving bisphenol A in alkali liquor, and then adding epoxy chloropropane; 2. when resin with medium molecular weight is needed, firstly dissolving bisphenol A in alkali liquor, and then adding the solution into epoxy chloropropane; 3. when the molecular weight is required to be smaller, firstly dissolving the bisphenol A in the epichlorohydrin, and then dropwise adding the alkali liquor.
In-process at epoxy production preparation, no matter be large molecular weight or small molecular weight, all need go on in reation kettle, in order to accelerate the reaction, generally need the stirring to mix, because reaction unit's central point puts in mostly to stirring paddle leaf, liquid in the reaction unit all can produce the tangential flow when stirring paddle leaf rotates, make liquid rotatory around the (mixing) shaft, can make liquid gush to the cauldron wall under the effect of centrifugal force, make the liquid level of cauldron wall department rise, the liquid of (mixing) shaft department simultaneously descends, and then form a big swirl, the swirl can reduce the speed of mutual flow between liquid, serious can form the bad mixed region of "solid gyration portion", and then lead to the fact the poor problem of mixed effect, and then influence epoxy's production efficiency.
Disclosure of Invention
In order to make up the defects of the prior art, the invention provides an epoxy resin production process. The invention is mainly used for solving the problems that stirring is needed in order to fully mix alkali liquor and liquid in a reaction kettle in the existing epoxy resin production process, and a large vortex is formed on the upper surface of the liquid during stirring, so that the mixing effect is influenced, and the production efficiency is influenced.
The technical scheme adopted by the invention for solving the technical problem is as follows: the invention provides an epoxy resin production process, which comprises the following steps:
s1: firstly, putting a certain amount of bisphenol A into a dissolving kettle, then introducing epoxy chloropropane for dissolving, heating the dissolving kettle, controlling the dissolving temperature to be 72 +/-2 ℃, and controlling the dissolving time to be 30min;
s2: after the dissolution is finished, pressing the liquid in the dissolution kettle into a reaction kettle with stirring by a pump, then stirring, dropwise adding alkali liquor, controlling the reaction temperature in the reaction kettle at 52 +/-2 ℃, preserving heat after the alkali liquor is added for the first time, preserving heat for a certain time, controlling the heat preservation temperature at 57 +/-2 ℃, then carrying out reduced pressure distillation to recover excessive epichlorohydrin for recycling, and stopping recovering and cooling until the distillate is clear and transparent;
s3: when the temperature is cooled to 52 +/-2 ℃, dropwise adding alkali liquor for the second time, preserving heat again after dropwise adding is finished, controlling the heat preservation temperature to 52 +/-2 ℃, adding benzene for dissolving after heat preservation is finished, heating to 74 +/-1 ℃, dissolving for 30min, then cooling to 50 ℃ and standing for 30min;
s4: after standing, pumping the upper resin benzene solution into a reflux benzene-removing kettle, then discharging the lower salt water, heating the reflux benzene-removing kettle to remove benzene-water azeotropic mixture until effluent liquid is clear and transparent, and stopping distillation and cooling;
s5: and (3) after the temperature is cooled to 52 +/-2 ℃, standing and filtering, storing the filtrate in a resin benzene solution storage tank for sedimentation, pumping the filtrate into a benzene removal kettle after the sedimentation is finished, heating to remove benzene until no distillate exists, and stopping benzene removal to obtain the epoxy resin finished product.
Preferably, the reaction kettle in the step S2 comprises a kettle body, a motor, a coil, a fixed seat, a supporting seat, a protecting cover and a stirring part; one end of the kettle body is provided with the supporting seat; the other end of the kettle body is provided with the fixed seat; the fixed seat is fixedly connected with the motor; the kettle body comprises a cylinder, a kettle cover and a kettle bottom; the kettle cover is arranged on the end face, located at one end of the fixed seat, of the barrel; the kettle cover is fixedly connected to the cylinder; the fixed seat is fixedly connected to the kettle cover; the kettle cover is provided with a feeding interface, a manhole and other functional interfaces; the kettle bottom is arranged on the end face of one end, located on the supporting seat, of the barrel; the kettle bottom is fixedly connected to the cylinder; a discharging interface and other function interfaces are arranged on the kettle bottom; the supporting seat is fixedly connected to the bottom of the kettle; the coil is spirally wound outside the side wall of the barrel; the coil is sleeved with the protective cover; the protective cover is connected to the kettle body;
the stirring component comprises a stirring shaft, a first stirring rod, a second stirring rod, a first gear ring, a first gear, a fixed connecting seat, a first stirring seat and a second stirring seat; the middle part of the kettle cover is rotationally connected with the stirring shaft; one end of the stirring shaft, which is positioned at the side of the kettle cover, penetrates through the kettle cover and is fixedly connected with a rotating shaft of the motor; a cylindrical boss is arranged in the middle of the inner wall of the kettle cover; the free end of the cylindrical boss is fixedly connected with the fixed connecting seat; the first gear ring is fixedly connected to the fixed connecting seat; the first stirring seat is arranged on one side, close to the kettle cover, of the stirring shaft; a second stirring seat is arranged on one side, close to the bottom of the kettle, of the stirring shaft; the first stirring seat and the second stirring seat are fixedly connected to the stirring shaft; the first stirring rod and the second stirring rod are uniformly arranged between the first stirring seat and the second stirring seat at intervals around the circumferential direction of the stirring shaft; the first stirring rod is close to the stirring shaft; the second stirring rod is close to the inner wall of the cylinder body; two ends of the first stirring rod are respectively and rotatably connected to the first stirring seat and the second stirring seat; the first stirring rod is positioned at one end of the kettle cover and is fixedly connected with the first gear; the first gear is in meshing transmission with the first gear ring; the two ends of the second stirring rod are connected to the first stirring seat and the second stirring seat.
When the device works, the alkali liquor is dripped into the reaction kettle, and in order to ensure that the alkali liquor is fully mixed in the liquid for reaction, the stirring component is additionally arranged in the reaction kettle to accelerate the mixing, so that the reaction speed is improved, and the stirring component is mostly arranged at the axis position of the reaction kettle, so that the liquid in the reaction kettle can generate tangential flow in the process of quick stirring and mixing, and further the liquid can rotate around the stirring shaft, so that the liquid can flow towards the kettle wall under the action of centrifugal force, the liquid level at the kettle wall is raised, one side of the liquid at the stirring shaft descends, and a large vortex is formed, the vortex can reduce the mutual flowing speed of the liquid, and if serious, a poor mixing area of a solid rotary part can be formed, so that the mixing effect is poor, and the reaction speed is low; therefore, after the liquid dissolved in the dissolving kettle is pumped into the reaction kettle, the coil and the motor are connected with a power supply, the coil is electrified with alternating current, the cylinder body is heated, further heating the solution to make the liquid temperature reach the temperature required by the reaction, and simultaneously rotating the motor, thereby driving the stirring shaft to rotate, further driving the first stirring seat and the second stirring seat to rotate, further driving the first stirring rod and the second stirring rod to rotate, because the second stirring rod is close to the side wall of the cylinder body, the liquid absorbing the heat emitted from the side wall of the cylinder body leaves the side wall of the cylinder body under the action of the second stirring rod, thereby the temperature of the liquid at the side wall is lower than that of the side wall of the cylinder body, the temperature rise of the liquid is accelerated, simultaneously, the liquids flow and mix with each other under the action of the stirring component, so that the temperature of the liquids in each position in the reaction kettle is increased, because the first stirring rod is close to the stirring shaft, the first stirring shaft is positioned in the middle of the reaction kettle, further, when the first stirring rod rotates around the stirring shaft, the first gear also rotates around the stirring shaft, because the first gear is meshed with the first gear ring, the first stirring rod rotates automatically, the rotation direction of the first stirring rod is opposite to that of the stirring shaft, the rotating first stirring rod drives the surrounding liquid to rotate along with the rotation, so as to drive the liquid to flow in the opposite direction when the first stirring rod and the second stirring rod rotate around the stirring shaft, thereby increasing the flow speed and the flow direction of the liquid in the middle part, further leading the liquids in different flow directions to collide with each other, thereby eliminating the poor mixing area of the solid rotary part formed in the middle part, further increasing the mutual mixing of the liquid in the middle part, thereby improving the mixing degree of the alkali liquor and the liquid dripped into the reaction kettle and being beneficial to the production of the epoxy resin; a puddler rotation drives liquid and flows and has reduced reation kettle middle part liquid around (mixing) shaft pivoted speed, and then has reduced liquid tangential flow speed and to the centrifugal force of cauldron body side wall, and then has eliminated the swirl at middle part, and then has improved reation kettle's volume utilization ratio, has avoided the swirl to inhale the air and has formed the bubble in liquid simultaneously and cause the (mixing) shaft to receive the impact, has reduced stirring part's vibrations.
Preferably, the outer cylindrical surface of the second stirring rod is provided with stirring bulges at uniform intervals along the axis direction; two ends of the second stirring rod are rotatably connected to the first stirring seat and the second stirring seat; a second gear is arranged at one end, located on the kettle cover, of the second stirring rod; the second gear is fixedly connected to the second stirring rod; a second gear ring is arranged on one side of the kettle cover of the cylinder; the second gear ring is fixedly connected to the cylinder body; and the second gear is in meshing transmission with the second gear ring.
When the stirring device works, liquid in the reaction kettle rotates along with the stirring component in the stirring process, when the rotating speed of the liquid close to the inner wall of the cylinder body around the stirring shaft is close to the rotating speed of the second stirring rod, the stirring and mixing capacity of the second stirring rod on the liquid is lost, and meanwhile, the liquid level height close to the inner wall of the cylinder body is also increased, so that the probability of generating vortexes is increased; therefore, the end part of the second stirring rod on one side of the kettle cover is provided with the second gear, the second gear is meshed with the second gear ring fixedly connected to the barrel, the stirring shaft drives the second stirring rod to rotate in the process, so that the second stirring rod rotates in the opposite direction to the rotation direction of the stirring shaft, and the second stirring rod is provided with the stirring protrusions.
Preferably, stirring scrapers are arranged in the kettle body at uniform intervals along the circumferential direction of the stirring shaft; the stirring scraper is obliquely arranged; one side of the stirring scraper is fixedly connected to the second stirring seat; the other side of the stirring scraper is in contact with the inner wall of the kettle bottom.
When the stirring device works, the liquid in the reaction kettle is weaker in flowing capability in the axial direction under the action of the stirring component and is not beneficial to the integral mixing of the liquid, so that the stirring scraper is fixedly connected to the second stirring seat and is obliquely arranged, when the stirring shaft drives the second stirring seat to rotate, the oblique stirring scraper rotates along with the second stirring seat, the liquid above the stirring scraper is subjected to component force in the axial direction, the liquid above the stirring scraper is further pushed in the axial direction, the flowing capability of the liquid in the kettle in the axial direction is further increased, the integral flowing property of the liquid in the kettle is further increased, the mixing effect among the liquids is further improved, and the generation of epoxy resin is further facilitated to be accelerated; because the stirring scraper blade contacts with the bottom of the kettle, and then drives liquid to the discharge outlet through the rotatory stirring scraper blade when arranging the material, and then is convenient for arrange the material.
Preferably, the stirring bulge spirally rises along the axis of the second stirring rod; the pitch of the stirring bulge is 1-5 times of the length of the second stirring rod.
When the stirring device works, the stirring protrusions are arranged to spirally rise along the axial direction of the second stirring rod, so that liquid contacting with the stirring bosses is subjected to a force in the opposite direction of the tangential direction and a force downward along the axial direction, the liquid is thrown out along the tangential direction and flows downward, the flow of the liquid near the inner wall of the kettle body is increased, the mixing of the liquid is accelerated, meanwhile, the flowing speed of the liquid in the kettle body along the axial direction is accelerated due to the matching of the spirally rising stirring protrusions and the stirring scrapers, the mixing speed of the liquid in the kettle body is accelerated, the reaction speed is accelerated, and the generation of epoxy resin is accelerated; the pitch of the stirring bulge is set to be 1-5 times of the length of the second stirring rod, so that the situation that the component force in the tangential direction is too small or the component force in the axial direction is too small due to the fact that the pitch of the stirring bulge is larger or smaller is avoided, the tangential rotating speed of liquid in the reaction kettle is reduced, the axial flowing speed of the liquid is increased, and the liquid mixing effect is improved.
Preferably, two ends of the protective cover are respectively and fixedly connected to the kettle bottom and the cylinder; a closed cavity is formed among the cylinder, the kettle bottom and the protective cover; one side of the closed cavity, which is close to the kettle cover, is sequentially communicated with a first electromagnetic valve and a vacuum pump through an air pipe; one side of the closed cavity close to the kettle bottom is sequentially communicated with a second electromagnetic valve and an oil storage tank through an oil pipe; the oil storage tank is positioned below the kettle bottom; the oil storage tank is fixedly connected to the supporting leg of the supporting seat; and an electro-optical liquid sensor is arranged in the closed cavity.
When the reaction kettle works, the reaction kettle needs to be heated, cooled and insulated repeatedly during reaction, and the heat in the reaction kettle is easy to be quickly dissipated into the air through the side wall of the cylinder body, so that the temperature of the reaction kettle liquid is reduced, and the heat insulation is not facilitated; therefore, a closed cavity is formed among the barrel, the kettle bottom and the protective cover, when heating and heat preservation are needed, the controller controls the first electromagnetic valve to be opened (at the moment, the second electromagnetic valve is in a closed state), the vacuum pump operates for a set time to pump out gas in the closed cavity, the vacuum pump stops operating after the set time is up, the first electromagnetic valve is closed, vacuum is formed in the closed cavity, during heating, the coil is electrified to enable the barrel to generate heat, further heat loss is reduced, further temperature rise of liquid in the kettle is accelerated, further the liquid quickly reaches the temperature required by reaction, the reaction speed is accelerated, during heat preservation, the heat loss of the kettle is slowed down by the vacuum closed cavity, further time interval for reheating to prevent the temperature from being reduced to be below the heat preservation temperature is increased, and further the heat preservation effect is improved; when cooling is needed, the second electromagnetic valve is opened to enable the closed space to be communicated with the oil storage tank, and due to the fact that the pressure intensity in the closed space is small, cold oil in the oil storage tank enters the closed cavity, heat dissipation of the barrel is accelerated, cooling time is shortened, and epoxy resin production efficiency is accelerated; when need reheating or heat preservation, open the solenoid valve No. one, and then make airtight cavity and atmosphere intercommunication, because the batch oil tank is less than airtight cavity, and then under the effect of gravity, the oil in the airtight cavity flows back to the batch oil tank through No. two solenoid valves, when treating that photoelectric liquid sensor detects the liquid level and drops to the setting value, no. two solenoid valves of controller control are closed the door, and the vacuum pump operation is treated again and is closed the solenoid valve after vacuumizing in the airtight cavity simultaneously for airtight cavity is in vacuum state again.
Preferably, one end of the stirring shaft, which is positioned at the kettle bottom, penetrates through the kettle bottom and is then rotatably connected to the oil storage tank; an annular boss is arranged on one side, located at the bottom of the kettle, of the second stirring seat; the annular boss penetrates through the kettle bottom; the annular boss is rotationally connected to the kettle bottom; an oil inlet channel is formed in the end face, located at one end of the oil storage tank, of the stirring shaft; a spiral impeller is arranged in the oil inlet channel; an oil pipe is arranged between the spiral impeller and the oil inlet channel; one end of the oil pipe is fixedly connected to the oil storage tank; an oil inlet hole is formed in the side wall, located in the oil storage tank, of the oil through pipe; one end of the spiral impeller is fixedly connected to the bottom surface of the oil inlet channel; the other end of the spiral impeller is rotationally connected to the oil pipe; the first stirring rod is of a hollow structure; an oil through hole is formed in the first stirring seat; the oil through hole is communicated with the oil inlet channel and the hollow structure of the first stirring rod; an oil return hole is formed in the second stirring seat; the oil return hole is communicated with the hollow structure of the first stirring rod; an oil return groove is formed in the end face of the annular boss; the oil return groove is communicated with the oil return hole; an oil return gathering piece is arranged in the oil return groove; one end of the oil return gathering piece is rotationally connected with the oil return groove; the other end of the oil return gathering piece is fixedly connected to the bottom of the kettle; the return oil gathering piece is communicated with an external oil supply loop through an oil pipe; the oil storage tank is communicated with external oil supply equipment.
When the heating kettle works, external oil supply equipment is used for introducing hot oil into the oil storage tank, so that the hot oil in the oil storage tank submerges an oil inlet hole in an oil through pipe, the motor drives the stirring shaft to rotate so as to drive the spiral impeller to rotate, the oil through pipe is fixedly connected to the oil storage tank, the spiral impeller drives the hot oil to flow to the bottom of the oil inlet channel, the hot oil sequentially passes through the oil through hole, a hollow structure of the first stirring rod, the oil return hole, the oil return groove and the oil return gathering piece and then enters an external oil supply loop, automatic circulation of the hot oil during stirring is realized, the maximum flow speed of the hot oil flowing from the oil inlet hole into the hollow structure of the first stirring rod is greater than the maximum flow speed of the hot oil flowing from the hollow structure of the first stirring rod to the oil return hole, the hot oil gradually fills a cavity in the first stirring rod during heating, the first stirring rod is further heated, the first stirring rod is further used for heating the liquid in the middle of the kettle, the kettle body is further heated by matching with the hot oil, the heating effect is further improved, and the liquid heating efficiency is further improved, so that the liquid in the heating kettle is further suitable for increasing the liquid heating efficiency and the liquid heating efficiency of the heating kettle body, and the liquid heating efficiency is further improved; when needs cool off, at first replace into cold oil through outside fuel feeding equipment with the liquid in the oil storage tank, stirring part rotates and gets into mutually supporting in the airtight cavity with cold oil, and then accelerates cooling rate, shortens the cooling required time, and then further improves epoxy's production efficiency.
Preferably, the first stirring rod is of a serpentine structure.
The during operation sets up to snakelike structure through a puddler, and then has increased area of contact between puddler and the liquid, and then has increased a puddler to liquid heating or refrigerated speed, and then has increased liquid by heating or refrigerated efficiency, and then has improved epoxy's production efficiency, has increased the stirring of a puddler to middle part liquid simultaneously, and then has improved the effect of liquid mixture.
Preferably, the side wall of the cylinder 11 is provided with annular arc grooves at uniform intervals along the axial direction; the ratio of the chord length of the section of the arc-shaped groove to the maximum height of the distance chord on the arc is less than 0.5.
When the device works, the arc-shaped grooves are formed in the side wall of the cylinder body along the axis direction, so that the contact area of the side wall of the cylinder body and oil is increased, the liquid cooling speed in the reaction kettle is increased, the cooling time is shortened, and the production efficiency of epoxy resin is improved; the ratio of the chord length of the section of the arc-shaped groove to the maximum height of the arc-shaped groove from the chord is smaller than 0.5, so that the oil is completely contacted with the side wall of the cylinder when entering the closed cavity, the heat dissipation speed is guaranteed, and the heat dissipation efficiency is improved.
The invention has the following beneficial effects:
1. in the invention, after the liquid dissolved in the dissolving kettle is pumped into the reaction kettle, the coil and the motor are connected with a power supply, alternating current is introduced into the coil, so that the cylinder body heats, further heating the solution to make the liquid temperature reach the temperature required by the reaction, and simultaneously rotating the motor, thereby driving the stirring shaft to rotate, further driving the first stirring seat and the second stirring seat to rotate, further driving the first stirring rod and the second stirring rod to rotate, because the second stirring rod is close to the side wall of the cylinder body, the liquid absorbing the heat emitted from the side wall of the cylinder body leaves the side wall of the cylinder body under the action of the second stirring rod, thereby the temperature of the liquid at the side wall is lower than that of the side wall of the cylinder body, the temperature rise of the liquid is accelerated, simultaneously, the liquids flow and mix with each other under the action of the stirring component, so that the temperature of the liquids in each part of the reaction kettle is raised, because the first stirring rod is close to the stirring shaft, the first stirring shaft is positioned in the middle of the reaction kettle, further, when the first stirring rod rotates around the stirring shaft, the first gear also rotates around the stirring shaft, because the first gear is meshed with the first gear ring, the first stirring rod rotates automatically, the rotation direction of the first stirring rod is opposite to that of the stirring shaft, the rotating first stirring rod drives the surrounding liquid to rotate along with the rotation, so as to drive the liquid to flow in the opposite direction when the first stirring rod and the second stirring rod rotate around the stirring shaft, thereby increasing the flow speed and the flow direction of the liquid in the middle part, further leading the liquids in different flow directions to collide with each other, thereby eliminating the poor mixing area of the solid rotary part formed in the middle part, further increasing the mutual mixing of the liquid in the middle part, further improving the mixing degree of the alkali liquor and the liquid dripped into the reaction kettle, and being beneficial to the production of the epoxy resin; a puddler rotation drives liquid and flows and has reduced reation kettle middle part liquid around (mixing) shaft pivoted speed, and then has reduced liquid tangential flow speed and to the centrifugal force of cauldron body side wall, and then has eliminated the swirl at middle part, and then has improved reation kettle's volume utilization ratio, has avoided the swirl to inhale the air and has formed the bubble in liquid simultaneously and cause the (mixing) shaft to receive the impact, has reduced the vibrations of stirring part.
2. According to the invention, the second gear is arranged at the end part of the second stirring rod, which is positioned on one side of the kettle cover, and is meshed with the second gear ring fixedly connected to the barrel, so that in the process that the stirring shaft drives the second stirring rod to rotate, the second stirring rod rotates towards the opposite direction of the rotation of the stirring shaft, and the second stirring rod is provided with the stirring protrusion, so that in the process of rotating the second stirring rod, liquid near the second stirring rod is stirred to rotate and is thrown out along the tangential direction, and then the liquid thrown out from different directions near the second stirring rod collides with the liquid at the edge of the side wall of the kettle body, so that the rotating speed of the liquid near the inner wall of the kettle body around the stirring shaft is further reduced, so that a rotation speed difference exists between the second stirring rod and the liquid, the second stirring rod is further ensured to stir the liquid at the edge, the liquid mixing capability is improved, and meanwhile, the liquid near the second stirring rod and the liquid in different directions collide with each other and are mixed with each other, so that the mixing between the liquids is further enhanced, and the generation of epoxy resin is further accelerated.
3. According to the invention, the stirring scraper is fixedly connected to the second stirring seat and is obliquely arranged, when the stirring shaft drives the second stirring seat to rotate, the oblique stirring scraper rotates along with the second stirring seat, so that the liquid above the stirring scraper is subjected to component force along the axial direction, and the liquid above the stirring scraper is pushed along the axial direction, so that the flowing capacity of the liquid in the kettle body in the axial direction is increased, the integral flowing property of the liquid in the kettle body is increased, the mixing effect among the liquids is improved, and the generation of epoxy resin is accelerated; because the stirring scraper blade contacts with the bottom of the kettle, and then drives liquid to the discharge outlet through the rotatory stirring scraper blade when arranging the material, and then is convenient for arrange the material.
4. According to the invention, the stirring bulge is arranged to spirally rise along the axial direction of the second stirring rod, so that liquid contacting with the stirring boss is subjected to tangential reverse upward force and axial downward force, and the liquid is thrown out tangentially and flows downwards, so that the flow of the liquid near the inner wall of the kettle body is increased, the mixing of the liquid is accelerated, meanwhile, the spirally rising stirring bulge and the stirring scraper plate are matched to accelerate the flow speed of the liquid in the kettle body along the axial direction, the mixing speed of the liquid in the kettle body is accelerated, the reaction speed is accelerated, and the generation of epoxy resin is accelerated; the pitch of the stirring bulge is set to be 1-5 times of the length of the second stirring rod, so that the situation that the tangential component force is too small or the axial component force is too small due to the fact that the pitch of the stirring bulge is larger or smaller is avoided, the tangential rotating speed of liquid in the reaction kettle is reduced by the second stirring rod, the axial flowing speed of the liquid is increased, and the liquid mixing effect is improved.
5. According to the invention, the closed cavity is formed among the barrel, the kettle bottom and the protective cover, when heating and heat preservation are needed, the controller controls the first electromagnetic valve to be opened (at the moment, the second electromagnetic valve is in a closed state), the vacuum pump operates for a set time to pump out gas in the closed cavity, the vacuum pump stops operating after the set time is up, and the first electromagnetic valve is closed, so that vacuum is formed in the closed cavity, during heating, the coil is electrified to enable the barrel to generate heat, so that heat loss is reduced, temperature rise of liquid in the kettle body is accelerated, so that the liquid can quickly reach temperature required by reaction, reaction speed is accelerated, during heat preservation, the heat loss of the kettle body is slowed down by the vacuum closed cavity, so that a time interval that reheating is needed to prevent the temperature from being reduced to be below a heat preservation temperature is increased, and a heat preservation effect is improved; when cooling is needed, the second electromagnetic valve is opened to enable the closed space to be communicated with the oil storage tank, and due to the fact that the pressure intensity in the closed space is small, cold oil in the oil storage tank enters the closed cavity, heat dissipation of the barrel is accelerated, cooling time is shortened, and epoxy resin production efficiency is accelerated; when need reheating or heat preservation, open the solenoid valve No. one, and then make airtight cavity and atmosphere intercommunication, because the batch oil tank is less than airtight cavity, and then under the effect of gravity, the oil in the airtight cavity flows back to the batch oil tank through No. two solenoid valves, when treating that photoelectric liquid sensor detects the liquid level and drops to the setting value, no. two solenoid valves of controller control are closed the door, and the vacuum pump operation is treated again and is closed the solenoid valve after vacuumizing in the airtight cavity simultaneously for airtight cavity is in vacuum state again.
Drawings
The invention will be further explained with reference to the drawings.
FIG. 1 is a process flow diagram for the production of epoxy resins in accordance with the present invention;
FIG. 2 is a schematic view of the overall structure of the reaction vessel in the present invention;
FIG. 3 is an exploded view of the reaction vessel of the present invention;
FIG. 4 is a schematic view of the internal structure of a reaction vessel in accordance with the present invention;
FIG. 5 is a schematic view of the connection between the bottom of the kettle and a second stirring seat in the invention;
FIG. 6 is a schematic structural view of a first stirring rod in the present invention;
FIG. 7 is an enlarged view of a portion of FIG. 6 at A;
fig. 8 is a partial enlarged view at B in fig. 6;
FIG. 9 is a schematic view of the arrangement of the first stirring rod and the second stirring rod and the flowing direction of the driving liquid in the present invention;
in the figure: the stirring device comprises a kettle body 1, a cylinder body 11, an arc-shaped groove 111, a kettle cover 12, a cylindrical boss 121, a kettle bottom 13, a motor 2, a coil 21, a fixed seat 22, a supporting seat 23, a protective cover 24, a stirring component 3, a stirring shaft 30, an oil inlet channel 301, a first stirring rod 31, a second stirring rod 32, a stirring protrusion 321, a first gear ring 33, a first gear 34, a fixed connecting seat 35, a first stirring seat 36, an oil through hole 361, a second stirring seat 37, an annular boss 371, an oil return hole 372, an oil return groove 373, a second gear 38, a second gear ring 39, a stirring scraper 4, a first electromagnetic valve 5, a vacuum pump 51, a second electromagnetic valve 52, an oil storage tank 53, a spiral impeller 6, an oil through pipe 61, an oil inlet hole 611 and an oil return piece 62.
Detailed Description
The present invention will be further described with reference to the following detailed description so that the technical means, the creation features, the achievement purposes and the effects of the present invention can be easily understood.
As shown in FIG. 1, a process for producing epoxy resin comprises the following steps:
s1: putting a certain amount of bisphenol A into a dissolving kettle, then introducing epoxy chloropropane for dissolving, heating the dissolving kettle, controlling the dissolving temperature to be 72 +/-2 ℃, and controlling the dissolving time to be 30min;
s2: after the dissolution is finished, pressing the liquid in the dissolution kettle into a reaction kettle with stirring by a pump, then stirring, dropwise adding alkali liquor, controlling the reaction temperature in the reaction kettle at 52 +/-2 ℃, preserving heat after the alkali liquor is added for the first time, preserving heat for a certain time, controlling the heat preservation temperature at 57 +/-2 ℃, then carrying out reduced pressure distillation to recover excessive epichlorohydrin for recycling, and stopping recovering and cooling until the distillate is clear and transparent;
s3: when the temperature is cooled to 52 +/-2 ℃, dropwise adding alkali liquor for the second time, preserving heat again after dropwise adding is finished, controlling the heat preservation temperature to 52 +/-2 ℃, adding benzene for dissolving after heat preservation is finished, heating to 74 +/-1 ℃, dissolving for 30min, then cooling to 50 ℃ and standing for 30min;
s4: after standing, pumping the upper resin benzene solution into a reflux benzene-removing kettle, then discharging the lower salt water, heating the reflux benzene-removing kettle to remove benzene-water azeotropic mixture until effluent liquid is clear and transparent, and stopping distillation and cooling;
s5: and (3) after the temperature is cooled to 52 +/-2 ℃, standing and filtering, storing the filtrate in a resin benzene solution storage tank for sedimentation, pumping the filtrate into a benzene removal kettle after the sedimentation is finished, heating to remove benzene until no distillate exists, and stopping benzene removal to obtain the epoxy resin finished product.
As shown in fig. 2 to 9, the reaction kettle described in step S2 includes a kettle body 1, a motor 2, a coil 21, a fixing seat 22, a supporting seat 23, a protecting cover 24, and a stirring component 3; one end of the kettle body 1 is provided with the supporting seat 23; the other end of the kettle body 1 is provided with the fixed seat 22; the fixed seat 22 is fixedly connected with the motor 2; the kettle body 1 comprises a cylinder body 11, a kettle cover 12 and a kettle bottom 13; the kettle cover 12 is arranged on the end face of the barrel 11, which is positioned at one end of the fixed seat 22; the kettle cover 12 is fixedly connected to the barrel 11; the fixed seat 22 is fixedly connected to the kettle cover 12; the kettle cover 12 is provided with a feeding interface, a manhole and other functional interfaces; the kettle bottom 13 is arranged on the end face, located at one end of the supporting seat 23, of the barrel 11; the kettle bottom 13 is fixedly connected to the barrel 11; a discharging interface and other function interfaces are arranged on the kettle bottom 13; the supporting seat 23 is fixedly connected to the kettle bottom 13; the coil 21 is spirally wound outside the side wall of the barrel 11; the coil 21 is sleeved with the protective cover 24; the protective cover 24 is connected to the kettle body 1;
the stirring component 3 comprises a stirring shaft 30, a first stirring rod 31, a second stirring rod 32, a first gear ring 33, a first gear 34, a fixed connecting seat 35, a first stirring seat 36 and a second stirring seat 37; the middle part of the kettle cover 12 is rotationally connected with the stirring shaft 30; one end of the stirring shaft 30, which is positioned at the side of the kettle cover 12, penetrates through the kettle cover 12 and is fixedly connected with a rotating shaft of the motor 2; a cylindrical boss 121 is arranged in the middle of the inner wall of the kettle cover 12; the free end of the cylindrical boss 121 is fixedly connected with the fixed connecting seat 35; the first gear ring 33 is fixedly connected to the fixed connecting seat 35; the first stirring seat 36 is arranged on one side, close to the kettle cover 12, of the stirring shaft 30; a second stirring seat 37 is arranged on one side of the stirring shaft 30 close to the kettle bottom 13; the first stirring seat 36 and the second stirring seat 37 are both fixedly connected to the stirring shaft 30; the first stirring rods 31 and the second stirring rods 32 are uniformly arranged between the first stirring seat 36 and the second stirring seat 37 at intervals around the circumferential direction of the stirring shaft 30; the first stirring rod 31 is close to the stirring shaft 30; the second stirring rod 32 is close to the inner wall of the cylinder 11; two ends of the first stirring rod 31 are respectively and rotatably connected to the first stirring seat 36 and the second stirring seat 37; the first stirring rod 31 is positioned at one end of the kettle cover 12 and is fixedly connected with the first gear 34; the first gear 34 is in meshed transmission with the first gear ring 33; the two ends of the second stirring rod 32 are connected to the first stirring seat 36 and the second stirring seat 37.
During operation, the alkali liquor is dripped into the reaction kettle, in order to enable the alkali liquor to be fully mixed and react in the liquid, the stirring component 3 is additionally arranged in the reaction kettle to accelerate mixing and further improve the reaction rate, because the stirring component 3 is mostly arranged at the axis position of the reaction kettle, in the process of rapid stirring and mixing, the liquid in the reaction kettle can generate tangential flow, and further the liquid can rotate around the stirring shaft 30, the liquid can flow towards the kettle wall under the action of centrifugal force, so that the liquid level at the kettle wall is raised, the liquid at the stirring shaft 30 descends, and further a large vortex is formed, the vortex can reduce the speed of mutual flow of the liquid, and if serious, a poor mixing area of a solid rotary part can be formed, so that the mixing effect is poor, and the reaction rate is low; therefore, after the liquid dissolved in the dissolving kettle is pumped into the reaction kettle, the coil 21 and the motor 2 are powered on, alternating current is introduced into the coil 21 to heat the cylinder 11, and then the solution is heated, so that the temperature of the liquid reaches the temperature required by the reaction, meanwhile, the motor 2 rotates to drive the stirring shaft 30 to rotate, and further drive the first stirring seat 36 and the second stirring seat 37 to rotate, and further drive the first stirring rod 31 and the second stirring rod 32 to rotate, because the second stirring rod 32 is close to the side wall of the cylinder 11, the liquid absorbing the heat emitted from the side wall of the cylinder 11 is separated from the side wall of the cylinder 11 under the action of the second stirring rod 32, and further the temperature of the liquid at the side wall is lower than that of the side wall of the cylinder 11, so that the temperature of the liquid is increased, meanwhile, the liquid flows and is mixed everywhere under the action of the stirring component 3, and further the temperature of the liquid in the reaction kettle is increased, because the first stirring rod 31 is close to the stirring shaft 30, the first stirring shaft 30 is positioned in the middle of the reaction kettle, and further, in the process that the first stirring rod 31 rotates around the stirring shaft 30, the first gear 34 also rotates around the stirring shaft 30, because the first gear 34 is meshed with the first gear ring 33, the first stirring rod 31 rotates, and the rotation direction is opposite to the rotation direction of the stirring shaft 30, the rotating first stirring rod 31 drives surrounding liquid to rotate, and further, the first stirring rod 31 and the second stirring rod 32 drive the liquid to flow in opposite directions when rotating around the stirring shaft 30, so that the flow speed and the liquid flow direction of the liquid in the middle are increased, further, the liquid in different flow directions collide with each other, further, the poor mixing region of a solid rotation part formed in the middle is eliminated, and the mutual mixing of the liquid in the middle is increased, thereby improving the mixing degree of the alkali liquor and the liquid dripped into the reaction kettle and being beneficial to the production of the epoxy resin; stirring rod 31 rotation drives liquid flow and has reduced reation kettle middle part liquid around (mixing) shaft 30 pivoted speed, and then has reduced liquid tangential flow speed and to the centrifugal force of the 1 lateral wall of the cauldron body, and then has eliminated the swirl at middle part, and then has improved reation kettle's volume utilization ratio, has avoided the swirl to inhale the air and has formed the bubble in liquid simultaneously and cause (mixing) shaft 30 to receive the impact, has reduced the vibrations of stirring part 3.
As shown in fig. 4, 6, 7 and 9, the second stirring rod 32 is provided with stirring protrusions 321 on the outer cylindrical surface at uniform intervals along the axial direction; two ends of the second stirring rod 32 are rotatably connected to the first stirring seat 36 and the second stirring seat 37; a second gear 38 is arranged at one end of the second stirring rod 32, which is positioned at the kettle cover 12; the second gear 38 is fixedly connected to the second stirring rod 32; a second gear ring 39 is arranged on one side of the kettle cover 12 of the barrel 11; the second gear ring 39 is fixedly connected to the cylinder 11; the second gear 38 is in meshed transmission with the second gear ring 39.
When the stirring device works, in the stirring process, liquid in the reaction kettle rotates along with the stirring component 3, when the rotating speed of the liquid close to the inner wall of the cylinder body 11 around the stirring shaft 30 is close to the rotating speed of the second stirring rod 32, the stirring and mixing capacity of the second stirring rod 32 on the liquid disappears, and meanwhile, the liquid level height close to the inner wall of the cylinder body 11 is also increased, so that the probability of generating vortexes is increased; therefore, the second gear 38 is arranged at the end part of the second stirring rod 32 on one side of the kettle cover 12, because the second gear 38 is meshed with the second gear ring 39 fixedly connected to the cylinder 11, and further in the process that the stirring shaft 30 drives the second stirring rod 32 to rotate, the second stirring rod 32 rotates towards the opposite direction of the rotation of the stirring shaft 30, and because the second stirring rod 32 is provided with the stirring protrusions 321, further in the process of the rotation of the second stirring rod 32, the liquid near the second stirring rod 32 is stirred to rotate and is thrown out along the tangential direction, further the liquid thrown out in different directions near the second stirring rod 32 collides with the liquid at the edge of the side wall of the kettle body 1, the rotating speed of the liquid near the inner wall of the kettle body 1 around the stirring shaft 30 is further reduced, so that the rotation speed difference always exists between the second stirring rod 32 and the liquid, further, the liquid at the edge of the second stirring rod 32 is ensured to be stirred, the liquid mixing capability of the kettle body 1 is improved, meanwhile, the liquid near the liquid in different directions and the kettle body 1 are mixed, further, the liquid in the collision are strengthened, and the mixing speed of the epoxy resin is further increased.
As shown in fig. 3, 4, 8 and 9, stirring scrapers 4 are uniformly arranged at intervals along the circumferential direction of the stirring shaft 30 in the kettle body 1; the stirring scraper 4 is obliquely arranged; one side of the stirring scraper 4 is fixedly connected to the second stirring seat 37; the other side of the stirring scraper 4 is contacted with the inner wall of the kettle bottom 13.
When the reactor is in operation, the liquid in the reactor is weaker in flowing capability in the axial direction under the action of the stirring component 3, and the whole mixing of the liquid is not facilitated, so that the stirring scraper 4 is fixedly connected to the second stirring seat 37, and the stirring scraper 4 is obliquely arranged, when the stirring shaft 30 drives the second stirring seat 37 to rotate, the oblique stirring scraper 4 rotates along with the second stirring seat 37, and further the liquid above the stirring scraper 4 is subjected to component force along the axial direction, so that the liquid above the stirring scraper 4 is pushed along the axial direction, and further the flowing capability in the axial direction of the liquid in the reactor body 1 is increased, so that the whole flowing capability of the liquid in the reactor body 1 is increased, the mixing effect among the liquids is further improved, and the generation of epoxy resin is facilitated to be accelerated; because stirring scraper blade 4 and the contact of cauldron bottom 13, and then drive liquid to the bin outlet through rotatory stirring scraper blade 4 when arranging the material, and then be convenient for arrange the material.
The stirring protrusion 321 spirally rises along the axis of the second stirring rod 32; the pitch of the stirring protrusion 321 is 1-5 times of the length of the second stirring rod 32.
When the stirring kettle works, the stirring protrusions 321 are arranged to spirally rise along the axial direction of the second stirring rod 32, so that liquid contacting with the stirring bosses is subjected to tangential reverse upward force and axial downward force, the liquid is thrown out tangentially and flows downwards, the flow of the liquid near the inner wall of the kettle body 1 is increased, the mixing of the liquid is accelerated, meanwhile, the flowing speed of the liquid in the kettle body 1 along the axial direction is accelerated by the matching of the spirally rising stirring protrusions 321 and the stirring scrapers 4, the mixing speed of the liquid in the kettle body 1 is accelerated, the reaction speed is accelerated, and the generation of epoxy resin is accelerated; the screw pitch of the stirring protrusion 321 is set to be 1-5 times of the length of the second stirring rod 32, so that the situation that the tangential component force is too small or the axial component force is too small due to the fact that the screw pitch of the stirring protrusion 321 is large or small is avoided, the tangential rotating speed of liquid in the reaction kettle is reduced by the second stirring rod 32, the axial flowing speed of the liquid is increased, and the liquid mixing effect is improved.
As shown in fig. 2, fig. 3, fig. 4 and fig. 6, two ends of the protective cover 24 are respectively and fixedly connected to the kettle bottom 13 and the cylinder 11; a closed cavity is formed among the cylinder 11, the kettle bottom 13 and the protective cover 24; one side of the closed cavity, which is close to the kettle cover 12, is sequentially communicated with a first electromagnetic valve 5 and a vacuum pump 51 through an air pipe; one side of the closed cavity, which is close to the kettle bottom 13, is sequentially communicated with a second electromagnetic valve 52 and an oil storage tank 53 through oil pipes; the oil storage tank 53 is positioned below the kettle bottom 13; the oil storage tank 53 is fixedly connected to the support leg of the support seat 23; and an electro-optical liquid sensor is arranged in the closed cavity.
When the reaction kettle works, the reaction kettle needs to be heated, cooled and insulated repeatedly during reaction, and the heat in the reaction kettle is easy to be quickly dissipated into the air through the side wall of the cylinder body 11, so that the temperature of the reaction kettle liquid is reduced, and the heat insulation is not facilitated; therefore, a closed cavity is formed among the barrel 11, the kettle bottom 13 and the protective cover 24, when heating and heat preservation are needed, the controller controls the first electromagnetic valve 5 to be opened (at the moment, the second electromagnetic valve 52 is in a closed state), the vacuum pump 51 operates for a set time to pump out gas in the closed cavity, after the set time is up, the vacuum pump 51 stops operating, and meanwhile, the first electromagnetic valve 5 is closed to further form vacuum in the closed cavity; when cooling is needed, the second electromagnetic valve 52 is opened to enable the closed space to be communicated with the oil storage tank 53, and due to the fact that the pressure intensity in the closed space is small, cold oil in the oil storage tank 53 enters the closed space, heat dissipation of the cylinder 11 is accelerated, cooling time is shortened, and epoxy resin production efficiency is accelerated; when reheating or heat preservation is needed, the first electromagnetic valve 5 is opened, the closed cavity is communicated with the atmosphere, the oil storage tank 53 is lower than the closed cavity, oil in the closed cavity flows back to the oil storage tank 53 through the second electromagnetic valve 52 under the action of gravity, when the photoelectric liquid sensor detects that the liquid level drops to a set value, the controller controls the second electromagnetic valve 52 to close the door, meanwhile, the vacuum pump 51 operates, and the first electromagnetic valve 5 is closed after the closed cavity is vacuumized again, so that the closed cavity is in a vacuum state again.
As shown in fig. 4 to 8, one end of the stirring shaft 30 located at the kettle bottom 13 penetrates through the kettle bottom 13 and then is rotatably connected to the oil storage tank 53; an annular boss 371 is arranged on one side, located at the kettle bottom 13, of the second stirring seat 37; the annular boss 371 penetrates through the kettle bottom 13; the annular boss 371 is rotatably connected to the kettle bottom 13; an oil inlet channel 301 is formed in the end face, located at one end of the oil storage tank 53, of the stirring shaft 30; a spiral impeller 6 is arranged in the oil inlet channel 301; an oil pipe 61 is arranged between the spiral impeller 6 and the oil inlet channel 301; one end of the oil pipe 61 is fixedly connected to the oil storage tank 53; an oil inlet hole 611 is formed in the side wall of the oil pipe 61 in the oil storage tank 53; one end of the spiral impeller 6 is fixedly connected to the bottom surface of the oil inlet channel 301; the other end of the spiral impeller 6 is rotationally connected to the oil through pipe 61; the first stirring rod 31 is of a hollow structure; an oil through hole 361 is formed in the first stirring seat 36; the oil through hole 361 is communicated with the oil inlet channel 301 and the hollow structure of the first stirring rod 31; an oil return hole 372 is formed in the second stirring seat 37; the oil return hole 372 is communicated with the hollow structure of the first stirring rod 31; an oil return groove 373 is formed in the end face of the annular boss 371; the oil return groove 373 is communicated with the oil return hole 372; an oil return gathering piece 62 is arranged in the oil return groove 373; one end of the return oil gathering piece 62 is rotatably connected with the return oil groove 373; the other end of the return oil gathering piece 62 is fixedly connected to the kettle bottom 13; the return oil gathering piece 62 is communicated with an external oil supply loop through an oil pipe; the oil reservoir 53 communicates with an external oil supply apparatus.
During operation, when heating, an external oil supply device introduces hot oil into the oil storage tank 53, so that the hot oil in the oil storage tank 53 submerges the oil inlet hole 611 on the oil through pipe 61, the motor 2 drives the stirring shaft 30 to rotate, and further drives the helical impeller 6 to rotate, because the oil through pipe 61 is fixedly connected to the oil storage tank 53, and further the helical impeller 6 drives the hot oil to flow to the bottom of the oil inlet channel 301, and further the hot oil enters an external oil supply loop after sequentially passing through the oil through hole 361, the hollow structure of the first stirring rod 31, the oil return hole 372, the oil return groove 373, and the oil return gathering member 62, thereby realizing automatic circulation of the hot oil during stirring, and because the maximum flow speed of the hot oil flowing from the oil inlet hole 611 into the hollow structure of the first stirring rod 31 is greater than the maximum flow speed of the hot oil flowing from the hollow structure of the first stirring rod 31 to the oil return hole 372, therefore, when the heating is carried out, the cavity in the first stirring rod 31 is gradually filled with the hot oil, the hot oil heats the first stirring rod 31, the first stirring rod 31 heats the liquid in the middle of the kettle body 1, and the first stirring rod 31 revolves and also rotates, so that the uniformity of heating the liquid is improved, the heating effect is improved, meanwhile, the first stirring rod is matched with the cylinder 11 in a heating way, the liquid in the whole kettle body 1 is heated, the temperature increasing speed of the liquid in the kettle body 1 is increased, the temperature of the liquid in the kettle body 1 is enabled to quickly reach the temperature suitable for reaction, the heating effect is further enhanced, the heating time is shortened, and the production efficiency of the epoxy resin is improved; when needs cool off, at first replace the liquid in the oil storage tank 53 into cold oil through outside fuel feeding equipment, stirring part 3 rotates and gets into to mutually support in the airtight cavity with cold oil, and then accelerates cooling rate, shortens the cooling required time, and then further improves epoxy's production efficiency.
As shown in fig. 3, 4 and 6, the first stirring rod 31 has a serpentine structure.
The during operation sets up to serpentine structure through puddler 31, and then has increased area of contact between puddler 31 and the liquid, and then has increased puddler 31 to liquid heating or refrigerated speed, and then has increased liquid by heating or refrigerated efficiency, and then has improved epoxy's production efficiency, has increased the stirring to middle part liquid of puddler 31 simultaneously, and then has improved the effect of liquid mixing.
As shown in fig. 3, 5 and 8, annular arc-shaped grooves 111 are uniformly arranged on the side wall of the cylinder 11 at intervals along the axial direction; the ratio of the chord length of the section of the arc-shaped groove 111 to the maximum height of the distance chord on the arc is less than 0.5.
When the reactor works, the arc-shaped groove 111 is formed in the side wall of the cylinder 11 along the axial direction, so that the contact area of the side wall of the cylinder 11 and oil is increased, the cooling speed of liquid in the reactor is increased, the cooling time is shortened, and the production efficiency of epoxy resin is improved; the ratio of the chord length of the section of the arc-shaped groove 111 to the maximum height of the distance chord on the arc is less than 0.5, so that the oil is completely contacted with the side wall of the cylinder body 11 when entering the closed cavity, the heat dissipation speed is further ensured, and the heat dissipation efficiency is improved.
When the rapid stirring and mixing device works, the alkali liquor is dripped into the reaction kettle, and in order to ensure that the alkali liquor is fully mixed in the liquid for reaction, the stirring component 3 is additionally arranged in the reaction kettle to accelerate the mixing and further improve the reaction rate, and the stirring component 3 is mostly arranged at the axial position of the reaction kettle, so that the liquid in the reaction kettle can generate tangential flow in the rapid stirring and mixing process, the liquid can rotate around the stirring shaft 30, the liquid can flow towards the kettle wall under the action of centrifugal force, the liquid level at the kettle wall is raised, the liquid at the stirring shaft 30 descends, and a large vortex is formed, the vortex can reduce the mutual flowing speed of the liquid, a poor mixing area of a solid rotating part can be formed seriously, the mixing effect is poor, and the reaction rate is low; therefore, after the liquid dissolved in the dissolving kettle is pumped into the reaction kettle, the coil 21 and the motor 2 are powered on, alternating current is introduced into the coil 21 to heat the cylinder 11, and then the solution is heated, so that the temperature of the liquid reaches the temperature required by the reaction, meanwhile, the motor 2 rotates to further drive the stirring shaft 30 to rotate, and further drive the first stirring seat 36 and the second stirring seat 37 to rotate, and further drive the first stirring rod 31 and the second stirring rod 32 to rotate, because the second stirring rod 32 is close to the side wall of the cylinder 11, and further the liquid absorbing the heat emitted from the side wall of the cylinder 11 leaves the side wall of the cylinder 11 under the action of the second stirring rod 32, so that the temperature of the liquid at the side wall is lower than that of the side wall of the cylinder 11, and further the temperature of the liquid is increased, and simultaneously the liquid flows and is mixed everywhere under the action of the stirring part 3, and further the temperature of the liquid in the reaction kettle is increased, because the first stirring rod 31 is close to the stirring shaft 30, the first stirring shaft 30 is positioned in the middle of the reaction kettle, and further in the process that the first stirring rod 31 rotates around the stirring shaft 30, the first gear 34 also rotates around the stirring shaft 30, because the first gear 34 is meshed with the first gear ring 33, the first stirring rod 31 rotates, the rotating direction is opposite to the rotating direction of the stirring shaft 30, the rotating first stirring rod 31 drives surrounding liquid to rotate along with the rotating first stirring rod, and further drives the liquid to flow in the opposite direction when the first stirring rod 31 and the second stirring rod 32 rotate around the stirring shaft 30, so that the flow velocity and the liquid flow direction of the liquid in the middle are increased, and the liquid in different flow directions collide with each other, thereby eliminating the poor mixing region of a solid rotating part formed in the middle, and further increasing the mutual mixing of the liquid in the middle, thereby improving the mixing degree of the alkali liquor and the liquid dripped into the reaction kettle and being beneficial to the production of the epoxy resin; stirring rod 31 rotation drives liquid flow and has reduced reation kettle middle part liquid around (mixing) shaft 30 pivoted speed, and then has reduced liquid tangential flow speed and to the centrifugal force of the 1 lateral wall of the cauldron body, and then has eliminated the swirl at middle part, and then has improved reation kettle's volume utilization ratio, has avoided the swirl to inhale the air and has formed the bubble in liquid simultaneously and cause (mixing) shaft 30 to receive the impact, has reduced stirring part 3's vibrations.
While the present invention has been described with reference to the embodiments shown in the drawings, the present invention is not limited to the embodiments, which are illustrative and not restrictive, and it will be apparent to those skilled in the art that various changes and modifications can be made therein without departing from the spirit and scope of the invention as defined in the appended claims.

Claims (9)

1. A production process of epoxy resin is characterized in that: the method comprises the following steps:
s1: putting a certain amount of bisphenol A into a dissolving kettle, then introducing epoxy chloropropane for dissolving, heating the dissolving kettle, controlling the dissolving temperature to be 72 +/-2 ℃, and controlling the dissolving time to be 30min;
s2: after the dissolution is finished, pressing the liquid in the dissolution kettle into a reaction kettle with a stirrer by a pump, stirring, dropwise adding alkali liquor, controlling the reaction temperature in the reaction kettle at 52 +/-2 ℃, preserving heat after the alkali liquor is added for the first time, preserving heat for a certain time, controlling the heat preservation temperature at 57 +/-2 ℃, then carrying out reduced pressure distillation to recover excessive epichlorohydrin for recycling, and stopping recovering and cooling after the distillate is clear and transparent;
s3: when the temperature is cooled to 52 +/-2 ℃, dropwise adding alkali liquor for the second time, preserving heat again after dropwise adding is finished, controlling the heat preservation temperature to 52 +/-2 ℃, adding benzene for dissolving after heat preservation is finished, heating to 74 +/-1 ℃, dissolving for 30min, then cooling to 50 ℃ and standing for 30min;
s4: after standing, pumping the upper resin benzene solution into a reflux debenzolization kettle, then discharging the lower layer brine, heating the reflux debenzolization kettle to remove the benzene-water azeotropic mixture until the effluent liquid is clear and transparent, stopping distillation and cooling;
s5: and (3) cooling to 52 +/-2 ℃, standing, filtering, storing the filtrate in a resin benzene solution storage tank for sedimentation, pumping the filtrate into a debenzolization kettle after the sedimentation is finished, heating for debenzolization until no distillate exists, and stopping debenzolization to obtain the epoxy resin finished product.
2. The process for producing an epoxy resin according to claim 1, wherein: the reaction kettle in the step S2 comprises a kettle body (1), a motor (2), a coil (21), a fixed seat (22), a supporting seat (23), a protective cover (24) and a stirring component (3); one end of the kettle body (1) is provided with the supporting seat (23); the other end of the kettle body (1) is provided with the fixed seat (22); the fixed seat (22) is fixedly connected with the motor (2); the kettle body (1) comprises a cylinder body (11), a kettle cover (12) and a kettle bottom (13); the kettle cover (12) is arranged on the end face, located at one end of the fixed seat (22), of the barrel (11); the kettle cover (12) is fixedly connected to the cylinder (11); the fixed seat (22) is fixedly connected to the kettle cover (12); the kettle cover (12) is provided with a feeding interface, a manhole and other utility interfaces; the kettle bottom (13) is arranged on the end face, located at one end of the supporting seat (23), of the barrel (11); the kettle bottom (13) is fixedly connected to the barrel (11); the kettle bottom (13) is provided with a discharging interface and other function interfaces; the supporting seat (23) is fixedly connected to the kettle bottom (13); the coil (21) is spirally wound outside the side wall of the barrel body (11); the coil (21) is sleeved with the protective cover (24); the protective cover (24) is connected to the kettle body (1);
the stirring component (3) comprises a stirring shaft (30), a first stirring rod (31), a second stirring rod (32), a first gear ring (33), a first gear (34), a fixed connecting seat (35), a first stirring seat (36) and a second stirring seat (37); the middle part of the kettle cover (12) is rotationally connected with the stirring shaft (30); one end of the stirring shaft (30) positioned at the side of the kettle cover (12) penetrates through the kettle cover (12) and is fixedly connected with a rotating shaft of the motor (2); a cylindrical boss (121) is arranged in the middle of the inner wall of the kettle cover (12); the free end of the cylindrical boss (121) is fixedly connected with the fixed connecting seat (35); the first gear ring (33) is fixedly connected to the fixed connecting seat (35); the first stirring seat (36) is arranged on one side, close to the kettle cover (12), of the stirring shaft (30); a second stirring seat (37) is arranged on one side, close to the kettle bottom (13), of the stirring shaft (30); the first stirring seat (36) and the second stirring seat (37) are fixedly connected to the stirring shaft (30); the first stirring rods (31) and the second stirring rods (32) are uniformly arranged between the first stirring seat (36) and the second stirring seat (37) at intervals around the circumferential direction of the stirring shaft (30); the first stirring rod (31) is close to the stirring shaft (30); the second stirring rod (32) is close to the inner wall of the cylinder body (11); two ends of the first stirring rod (31) are respectively and rotatably connected to the first stirring seat (36) and the second stirring seat (37); one end of the first stirring rod (31) positioned at the kettle cover (12) is fixedly connected with the first gear (34); the first gear (34) is in meshing transmission with the first gear ring (33); the two ends of the second stirring rod (32) are connected to the first stirring seat (36) and the second stirring seat (37).
3. The process for producing an epoxy resin according to claim 2, wherein: stirring protrusions (321) are uniformly arranged on the outer cylindrical surface of the second stirring rod (32) at intervals along the axis direction; two ends of the second stirring rod (32) are rotatably connected to the first stirring seat (36) and the second stirring seat (37); a second gear (38) is arranged at one end, located on the kettle cover (12), of the second stirring rod (32); the second gear (38) is fixedly connected to the second stirring rod (32); a second gear ring (39) is arranged on one side, located on the kettle cover (12), of the barrel (11); the second gear ring (39) is fixedly connected to the cylinder body (11); the second gear (38) is in meshed transmission with the second gear ring (39).
4. The epoxy resin production process according to claim 3, wherein: stirring scrapers (4) are uniformly arranged in the kettle body (1) at intervals along the circumferential direction of the stirring shaft (30); the stirring scraper (4) is obliquely arranged; one side of the stirring scraper (4) is fixedly connected to the second stirring seat (37); the other side of the stirring scraper (4) is in contact with the inner wall of the kettle bottom (13).
5. The epoxy resin production process according to claim 4, wherein: the stirring protrusion (321) spirally rises along the axis of the second stirring rod (32); the pitch of the stirring protrusion (321) is 1-5 times of the length of the second stirring rod (32).
6. The epoxy resin production process according to claim 5, wherein: two ends of the protective cover (24) are respectively and fixedly connected to the kettle bottom (13) and the barrel body (11); a closed cavity is formed among the cylinder (11), the kettle bottom (13) and the protective cover (24); one side of the closed cavity, which is close to the kettle cover (12), is sequentially communicated with a first electromagnetic valve (5) and a vacuum pump (51) through an air pipe; one side of the closed cavity close to the kettle bottom (13) is sequentially communicated with a second electromagnetic valve (52) and an oil storage tank (53) through oil pipes; the oil storage tank (53) is positioned below the kettle bottom (13); the oil storage tank (53) is fixedly connected to the supporting leg of the supporting seat (23); and an electro-optical liquid sensor is arranged in the closed cavity.
7. The epoxy resin production process according to claim 6, wherein: one end of the stirring shaft (30) positioned at the kettle bottom (13) penetrates through the kettle bottom (13) and then is rotatably connected to the oil storage tank (53); an annular boss (371) is arranged on one side, located at the kettle bottom (13), of the second stirring seat (37); the annular boss (371) penetrates through the kettle bottom (13); the annular boss (371) is rotationally connected to the kettle bottom (13); an oil inlet channel (301) is formed in the end face, located at one end of the oil storage tank (53), of the stirring shaft (30); a spiral impeller (6) is arranged in the oil inlet channel (301); an oil pipe (61) is arranged between the spiral impeller (6) and the oil inlet channel (301); one end of the oil pipe (61) is fixedly connected to the oil storage tank (53); an oil inlet hole (611) is formed in the side wall, located in the oil storage tank (53), of the oil pipe (61); one end of the spiral impeller (6) is fixedly connected to the bottom surface of the oil inlet channel (301); the other end of the spiral impeller (6) is rotationally connected to the oil pipe (61); the first stirring rod (31) is of a hollow structure; an oil through hole (361) is formed in the first stirring seat (36); the oil through hole (361) is communicated with the oil inlet channel (301) and a hollow structure of the first stirring rod (31); an oil return hole (372) is formed in the second stirring seat (37); the oil return hole (372) is communicated with the hollow structure of the first stirring rod (31); an oil return groove (373) is formed in the end face of the annular boss (371); the oil return groove (373) is communicated with the oil return hole (372); an oil return gathering piece (62) is arranged in the oil return groove (373); one end of the oil return gathering piece (62) is rotatably connected with the oil return groove (373); the other end of the return oil gathering piece (62) is fixedly connected to the kettle bottom (13); the return oil gathering piece (62) is communicated with an external oil supply loop through an oil pipe; the oil storage tank (53) is communicated with external oil supply equipment.
8. The epoxy resin production process according to claim 7, wherein: the first stirring rod (31) is of a snake-shaped structure.
9. The process for producing an epoxy resin according to claim 8, wherein: annular arc-shaped grooves (111) are uniformly arranged on the side wall of the cylinder body (11) at intervals along the axial direction; the ratio of the chord length of the section of the arc-shaped groove (111) to the maximum height of the distance chord on the arc is less than 0.5.
CN202210970390.XA 2022-08-12 2022-08-12 Epoxy resin production process Pending CN115282914A (en)

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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CN117463279B (en) * 2023-12-28 2024-03-19 沧州营旭防腐设备有限公司 Chemical production is with high-efficient reation kettle

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