CN112062893A - Method and equipment for macroporous weak-acid cation exchange resin - Google Patents
Method and equipment for macroporous weak-acid cation exchange resin Download PDFInfo
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- CN112062893A CN112062893A CN202010972483.7A CN202010972483A CN112062893A CN 112062893 A CN112062893 A CN 112062893A CN 202010972483 A CN202010972483 A CN 202010972483A CN 112062893 A CN112062893 A CN 112062893A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/04—Acids; Metal salts or ammonium salts thereof
- C08F220/06—Acrylic acid; Methacrylic acid; Metal salts or ammonium salts thereof
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D33/00—Filters with filtering elements which move during the filtering operation
- B01D33/01—Filters with filtering elements which move during the filtering operation with translationally moving filtering elements, e.g. pistons
- B01D33/03—Filters with filtering elements which move during the filtering operation with translationally moving filtering elements, e.g. pistons with vibrating filter elements
- B01D33/0346—Filters with filtering elements which move during the filtering operation with translationally moving filtering elements, e.g. pistons with vibrating filter elements with flat filtering elements
- B01D33/0353—Filters with filtering elements which move during the filtering operation with translationally moving filtering elements, e.g. pistons with vibrating filter elements with flat filtering elements self-supporting
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D33/00—Filters with filtering elements which move during the filtering operation
- B01D33/04—Filters with filtering elements which move during the filtering operation with filtering bands or the like supported on cylinders which are impervious for filtering
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D33/00—Filters with filtering elements which move during the filtering operation
- B01D33/35—Filters with filtering elements which move during the filtering operation with multiple filtering elements characterised by their mutual disposition
- B01D33/41—Filters with filtering elements which move during the filtering operation with multiple filtering elements characterised by their mutual disposition in series connection
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D33/00—Filters with filtering elements which move during the filtering operation
- B01D33/44—Regenerating the filter material in the filter
- B01D33/46—Regenerating the filter material in the filter by scrapers, brushes nozzles or the like acting on the cake-side of the filtering element
- B01D33/461—Regenerating the filter material in the filter by scrapers, brushes nozzles or the like acting on the cake-side of the filtering element brushes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0053—Details of the reactor
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0053—Details of the reactor
- B01J19/0066—Stirrers
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/18—Stationary reactors having moving elements inside
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J39/00—Cation exchange; Use of material as cation exchangers; Treatment of material for improving the cation exchange properties
- B01J39/08—Use of material as cation exchangers; Treatment of material for improving the cation exchange properties
- B01J39/16—Organic material
- B01J39/18—Macromolecular compounds
- B01J39/20—Macromolecular compounds obtained by reactions only involving unsaturated carbon-to-carbon bonds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/12—Esters of monohydric alcohols or phenols
- C08F220/16—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
- C08F220/18—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
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- Chemical Kinetics & Catalysis (AREA)
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Abstract
The invention relates to a method for preparing macroporous weakly acidic cation exchange resin and equipment thereof, which are characterized in that the final product is pure white through reasonable process structure arrangement, the defect of yellow product color in the prior process taking acrylonitrile as a raw material is directly improved, meanwhile, the process is simple, the aqueous phase calcium chloride solution can be recycled, the cost is low, the environmental pollution is small, the production efficiency is high, and the production cost of enterprises can be saved.
Description
Technical Field
The invention relates to a method and equipment for macroporous weak-acid cation exchange resin.
Background
The macroporous weak-acid acrylic cationic resin is mainly applied to water treatment, has a large market share, and has two main production processes adopted by various resin enterprises at present, wherein one process adopts primary or secondary polymerized polymethyl acrylate as white balls, and the macroporous weak-acid resin is obtained by hydrolysis; the other process is to prepare macroporous white balls by using acrylonitrile as a monomer and obtain macroporous weak acid resin by hydrolysis. If the production process using methyl acrylate as a raw material is adopted, the defect is that the weak acid exchange capacity of the finally obtained weak acid resin cannot reach 11mmol/g, and the requirement of a client cannot be met; if acrylonitrile is used as a polymerization monomer, the weak acid exchange capacity of a final product can reach the standard, but the product is creamy yellow or yellow bead in appearance, so that the aim of pure white resin cannot be fulfilled, and the product is not easily accepted by customers. The reaction kettle, the curing kettle and the filter are needed to be used in the production process, the heating device of the existing reaction kettle is generally only arranged at one position, so when the chemical raw material is heated, the heat quantity received by different positions of the chemical raw material is different, the imbalance of the heat quantity is difficult to compensate in a short time, potential safety hazards are brought, the threat is brought to the life and property of people, oil stains can be remained on the inner wall of the reaction kettle in the production process, along with the increase of the using time, the remained oil stains can be more and more, the reaction kettle can be insufficiently heated due to the attachment of the oil stains on the inner wall of the reaction kettle, the reaction time is too long, the production efficiency is influenced, the inner wall of the reaction kettle is manually cleaned at present, the cleaning mode is very labor-consuming, the cleaning efficiency is low, the cleaning device needs to be put into the reaction kettle and taken out after the cleaning is finished, the reaction kettle can be communicated with, the external impurity can get into and cause secondary pollution in the reation kettle, influence the quality of next reaction, adopt the filter screen to filter in the filter, the smaller its filter effect of general filter screen mesh is just better, but the filter screen of little mesh is very easy to be blockked up, need regularly clean the filter screen, influence production efficiency, the curing reaction of resin is a heat release process, in the curing process, the temperature in the curing kettle can constantly rise, consequently, need release heat to the curing kettle, but present industrial curing kettle all directly discharges steam to the external world, a large amount of steam has been wasted like this, be very big loss to the enterprise, from this it is necessary to make the improvement.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a method and equipment for preparing macroporous weak-acid cation exchange resin, which can obtain pure white resin, has high production efficiency and can save the production cost of enterprises.
The technical scheme of the invention is realized as follows: a method for preparing macroporous weakly acidic cation exchange resin comprises a reaction kettle, a curing kettle and a circulating filter, wherein a stirrer is arranged in the reaction kettle, and the method is characterized in that: comprises the following steps:
s1, taking 1-3 parts of styrene, 60-80 parts of a mixture of acrylic acid and acrylic ester and 5-10 parts of divinylbenzene and triallyl isocyanurate as monomers according to the weight ratio; taking toluene and gasoline or carbon alcohol which are 5-30 percent of the total weight of the monomers as mixed pore-foaming agents, taking benzoyl peroxide which is 0.1-2 percent of the total weight of the monomers and azobisisobutyronitrile which is 0.1-2 percent of the total weight of the monomers as initiators, and mixing to obtain an oil phase;
s2, dissolving 0.2-1 part of cellulose and 250-400 parts of anhydrous calcium chloride in 500 parts of deionized water according to the weight ratio to prepare a calcium chloride aqueous solution with the concentration of 35-40%;
s3, introducing a calcium chloride aqueous solution into a reaction kettle, putting an oil phase into the reaction kettle to mix with the calcium chloride aqueous solution, starting a stirrer at a rotating speed of 40-120 r/min until the particle size of oil droplets is 0.4-1.2mm, starting to heat to 65-75 ℃, carrying out constant-temperature reaction, continuing to carry out heat preservation reaction at the temperature for 5 hours, then slowly heating to 75-85 ℃, and carrying out constant-temperature reaction for 2-4 hours; then raising the temperature to 85-95 ℃ at the same heating rate, carrying out constant temperature reaction for 2-4 hours, finally raising the temperature to 97 ℃, keeping the temperature for 8 hours, introducing the mixture into a curing kettle for curing reaction, and filtering the mixture through a circulating filter after the curing reaction is finished to obtain beads;
s4, washing the bead balls with deionized water at the temperature of 75-90 ℃ until the washing liquid is clear; then extracting with acetone, and leaching with ethanol until the washing liquid is clear; obtaining a macroporous cation resin semi-finished product;
s5, taking 150ml of the macroporous cation resin semi-finished product, adding 200ml of 15-25% liquid alkali, and reacting at the constant temperature of 70-90 ℃ for 5-10 h; after the reaction is finished, filling the column, washing the column with deionized water with the same volume, then passing 1N hydrochloric acid with 2 times of volume through the column for 1h-2h, and then washing the column with deionized water until the column is neutral to obtain the macroporous weakly acidic cation exchange resin.
By adopting the technical scheme, the production method of the macroporous weakly-acidic cation exchange resin has reasonable process design and high quality of the obtained product, compared with the prior art, the polyacrylic resin can be directly obtained by polymerizing acrylic acid, alcohol groups are not removed by hydrolysis, the price of the acrylic acid is low, and the utilization rate of raw materials can be improved in any aspect.
The invention also discloses a device suitable for the macroporous weak acid cation exchange resin method, which comprises the following steps: the method is characterized in that: the device comprises a processing production line, wherein the processing production line comprises a reaction kettle, a curing kettle and a circulating filter which are sequentially connected, the reaction kettle comprises a kettle body, a feed port is arranged at the top of the kettle body, a reaction discharge pipe is arranged at the bottom of the kettle body, a reaction discharge valve is arranged on the reaction discharge pipe, a stirrer comprises a driving motor, a stirring shaft and stirring blades, the stirring shaft is hollow, one end of the stirring shaft is in transmission connection with the driving motor through a shaft coupling, a heating pipe is arranged on the outer wall of the kettle body, a heating seat is arranged at the bottom of the kettle body, a heating rod is arranged at the top of the heating seat, the upper end of the heating rod penetrates through the bottom of the kettle body and then extends into the stirring shaft, a plurality of heat transfer holes are arranged on the stirring shaft, a first temperature sensor is arranged on the inner wall of the kettle, the solidification feed pipe is communicated with the reaction discharge pipe, and the solidification discharge pipe is connected with the circulating filter.
By adopting the technical scheme, the reaction discharging pipe of the reaction kettle is communicated with the curing feeding pipe of the curing kettle, the curing discharging pipe of the curing kettle is connected with the circulating filter, so that the reaction kettle, the curing kettle and the circulating filter are sequentially connected into a processing production line, the production efficiency is improved, calcium chloride aqueous solution and oil phase are sequentially fed into the kettle body through the feeding port, the driving motor is started, the coupling is connected with the output shaft of the driving motor and the stirring shaft, the stirring shaft rotates and simultaneously drives the stirring blades to stir the mixed solution under the connection of the coupling, the mixed solution is accelerated to react, the heating pipe is opened to heat the outer wall of the kettle body, heat is transferred into the kettle body through the outer wall of the kettle body, the heating seat is started to heat the heating rod on the heating pipe while the heating pipe is heated, the upper end of the heating rod extends into the stirring shaft, so that the, like this internal and external concurrent heating of cauldron, can reach the temperature of needs sooner, production efficiency has been improved, first temperature sensor can the internal portion's of real-time supervision cauldron temperature, when the internal portion's of cauldron temperature reaches the value of needs, heating pipe and heating rod stop heating, heating pipe or heating rod heat the cauldron body after the fixed time of isothermal reaction, in order to satisfy the production demand, the reaction bleeder valve is closed during the reaction, the reaction bleeder valve is opened after the reaction is accomplished, the reaction liquid carries out solidification reaction through reaction discharging pipe and the leading-in solidification cauldron of solidification inlet pipe, after reation kettle uses, utilize the cleaning assembly can in time clear up remaining greasy dirt on the internal wall of cauldron, avoid the greasy dirt to pile up too much influence reation kettle work, manual cleaning is labour saving and time saving relatively.
The invention is further configured to: the circulating filter comprises a shell, a partition plate is vertically arranged in the middle of the shell and divides the inner wall of the shell into a primary filtering bin and a secondary filtering bin, the primary filtering bin is communicated with the top of the secondary filtering bin, a feed inlet is arranged at the top of the shell, the upper end of the feed inlet is communicated with a solidifying discharge pipe, the lower end of the feed inlet is communicated with the top of the primary filtering bin, a driving roller is arranged at the top of the secondary filtering bin, a driven roller is arranged at the top of the primary filtering bin, the same primary filtering net is sleeved on the driving roller and the driven roller, a primary flow guide plate is obliquely arranged at the bottom of the primary filtering bin, a primary flow discharge pipe is arranged at the lower part of the primary flow guide plate and extends out of the shell, a cleaning roller is arranged at one side of the driving roller far, the secondary filter storehouse bottom slope is equipped with the second grade guide plate, second grade guide plate lower part is equipped with the second grade fluid-discharge tube, the second grade fluid-discharge tube extends to the casing outside, second grade guide plate top is equipped with the second grade filter screen, the slope of second grade filter screen sets up, second grade filter screen lower part is equipped with the granule export, second grade filter screen bottom is equipped with vibrating motor.
By adopting the technical scheme, the feed inlet is communicated with the solidification discharge pipe, solidified products are guided into the first-stage filter bin through the solidification discharge pipe and the feed inlet after solidification reaction, the solidified products fall on the first-stage filter screen from the feed inlet to be filtered, unqualified products and liquid pass through the first-stage filter screen to fall on the first-stage guide plate and are discharged downwards along the first-stage guide plate through the first-stage liquid discharge pipe, qualified products are left on the first-stage filter screen, the driving roller rotates while the first-stage filter screen filters, the first-stage filter screen transports qualified products to the second-stage filter bin under the coordination of the driven roller, the cleaning roller also rotates while the driving roller rotates, the cleaning roller drives the cleaning brush to rotate, the cleaning brush cleans the first-stage filter screen and pushes the qualified products on the first-stage filter screen downwards to avoid the meshes of the first-stage filter screen, the qualified products fall on the second-stage filter screen downwards under the, the slope of second grade filter screen sets up, the mesh of second grade filter screen is greater than the mesh of one-level filter screen, the product of doping part granule undersize in the qualified result of one-level filter screen screening, these products will pass the second grade filter screen and fall on the second grade guide plate, and discharge through the second grade fluid-discharge tube downwards along the second grade guide plate, the equal qualified result of screening through twice then rolls downwards along the second grade filter screen to the granule export and collects, when the second grade filter screen is filterable, vibrating motor starts to drive the second grade filter screen and vibrates from top to bottom, the efficiency of the filterable efficiency of second grade filter screen and the efficiency that the final qualified result.
The invention is further configured to: the cleaning component comprises a lifting motor, a threaded rod, a lifting block and a brush, the lifting motor is fixed at the upper end inside the stirring shaft, the threaded rod is in transmission connection with a lifting motor, the lifting block is provided with a thread groove, the lifting block is sleeved on the outer wall of the threaded rod through the thread fit of the thread groove and the threaded rod, a limit groove is arranged on the inner wall of the stirring shaft along the vertical direction, one side of the lifting block extends into the limit groove and can slide along the length direction of the limit groove, a rotating frame is arranged on the outer wall of the stirring shaft and below the limiting groove, one end of the rotating frame is hinged with the outer wall of the stirring shaft, the brush is fixed at one end of the rotating frame far away from the stirring shaft, the middle part of the rotating frame is hinged with a supporting rod, one end of the support rod, which is far away from the rotating frame, is hinged with the side wall of the lifting block, and the lifting block is provided with a detection assembly for detecting the upper limit position and the lower limit position.
By adopting the technical scheme, in the reaction process of the mixed solution, the lifting block is positioned at the upper part of the threaded rod, the rotating frame is in a vertical state, the supporting rod fixes the rotating frame, after the reaction kettle is used, the lifting motor is started to drive the threaded rod to rotate, the threaded rod provides a rotating thrust force for the lifting block, under the limiting action of the limiting groove, the lifting block moves downwards on the outer wall of the threaded rod, the lifting block moves downwards and simultaneously drives one end of the supporting rod, which is hinged with the lifting block, to move downwards, one end of the supporting rod, which is far away from the lifting block, opens towards one side far away from the lifting block, one end of the supporting rod, which is far away from the lifting block, is hinged with the middle part of the rotating frame, the rotating frame turns downwards with a hinged point between the rotating frame and the stirring shaft as a fulcrum when the supporting rod opens, the bracing piece stops moving downwards, the rotating turret is the horizontality this moment, the brush that the rotating turret kept away from (mixing) shaft one end offsets with cauldron internal wall, the bracing piece is fixed the rotating turret, driving motor starts to drive the (mixing) shaft and rotates this moment, the (mixing) shaft rotates and washes on cauldron internal wall through the rotating turret area brush, wash remaining greasy dirt on the cauldron internal wall, driving motor closes after the washing is accomplished, the (mixing) shaft stops rotating, the brush stops washing, lifting motor starts to drive the threaded rod reverse rotation this moment, the threaded rod drives the elevator block upward movement, the elevator block drives bracing piece one end upward movement, the bracing piece drives the rotating turret upwards upset, when detecting component detects the upper limit position, lifting motor closes, the threaded rod stops rotating, the elevator block stops upward movement, the bracing piece stops upward movement, the rotating turret is vertical state this moment, wait for the going, compared with the prior art, this structure can drive the brush through the (mixing) shaft and rotate and wash the internal wall of cauldron, has saved the trouble of manual cleaning, and the cleaning efficiency is high, washs and can pack up the back brush of accomplishing, can not influence going on of reaction.
The invention is further configured to: the detection assembly comprises an upper travel switch and a lower travel switch, the upper travel switch is fixed on the upper surface of the lifting block and located on one side of the limiting groove, the contact of the upper travel switch faces upwards, the lower travel switch is fixed on the lower surface of the lifting block and located on one side of the limiting groove, and the contact of the lower travel switch faces downwards.
Through adopting above-mentioned technical scheme, in the elevator downstream process, the real-time ready of low travel switch, when the contact of lower travel switch and the lower lateral wall contact trigger low travel switch of spacing groove, elevator motor closes, the elevator stops the downstream, in the elevator upward motion process, go up travel switch and wait in real time, when the contact of last travel switch and the contact of spacing groove upper wall contact trigger upward travel switch, elevator motor closes, the elevator stops the upward movement, setting through last travel switch and low travel switch, make the lift of elevator more accurate, it is safer to use.
The invention is further configured to: cauldron body upper portion is equipped with the sealed kettle cover of detachable, be equipped with electric telescopic handle between rotating turret and the brush, the one end fixed connection of (mixing) shaft is kept away from to electric telescopic handle one end and rotating turret, the electric telescopic handle other end and brush fixed connection, be equipped with height adjuster between last travel switch and the elevator upper surface, be equipped with down height adjuster between lower travel switch and the elevator lower surface.
Through adopting above-mentioned technical scheme, sealed kettle cover and the cauldron body can be dismantled and be connected, can come (mixing) shaft and the epaxial part of stirring to move out outside the cauldron body through dismantling sealed kettle cover, the internal portion of different reation kettle cauldron is different in size, distance between brush and the rotating turret can be adjusted to electric telescopic handle between rotating turret and the brush, make it with different reation kettle adaptations, when different (mixing) shafts of different cauldron body depths different needs to be changed, the spacing groove on the (mixing) shaft is different, go up height adjuster can adjust the distance between stroke switch and the elevator, distance between lower stroke switch and the elevator can be adjusted to lower height adjuster, the upper and lower extreme position that makes the elevator and the position of rotating turret can reach the best most suitable state, interchangeability is good, can practice thrift use cost.
The invention is further configured to: the width of rotating turret is greater than the width of spacing groove, be equipped with the baffle between threaded rod and the heating rod, the baffle lateral wall offsets with the (mixing) shaft inner wall.
Through adopting above-mentioned technical scheme, the baffle is the heat insulating board, and the baffle lateral wall offsets with the (mixing) shaft inner wall, can prevent that the heat directly rises to around the threaded rod, can reduce the heat that the heating rod produced to threaded rod and elevator motor's influence, and the width of rotating turret is greater than the width of spacing groove, and when being in the reaction process, the rotating turret is vertical state, and the rotating turret can block the spacing groove, avoids reaction liquid to splash and gets into the inside elevator motor that influences of (mixing) shaft through the spacing groove.
The invention is further configured to: the curing kettle is characterized in that a recovery tank is arranged on one side of the curing kettle, a heat preservation layer is arranged on the inner wall of the recovery tank, a gas pipe is arranged on the side wall of the curing kettle, an electromagnetic valve is arranged at one end, close to the curing kettle, of the gas pipe, one end, far away from the curing kettle, of the gas pipe is communicated with the recovery tank, a negative pressure pump is arranged on the gas pipe, and a second temperature sensor is arranged on the inner wall of the curing.
Through adopting above-mentioned technical scheme, the solidification cauldron produces the heat in the solidification reaction process, second temperature sensor can the inside temperature of real-time supervision solidification cauldron, when the temperature risees to a definite value, the solenoid valve is opened, the negative pressure pump starts and forms the atmospheric pressure difference, steam in the solidification cauldron gets into through the gas-supply pipe under the effect of negative pressure pump and collects in the recovery jar, the heat that the heat preservation on the recovery jar inner wall can avoid in the recovery jar scatters and disappears, compare with prior art, this structure can be retrieved the heat that the solidification reaction produced, avoid the heat to be lost by the useless.
The invention is further configured to: the negative pressure pump is provided with a screen, the screen is positioned between the negative pressure pump and the gas pipe, and the bottom of the recovery tank is provided with a heat transmission pipe.
Through adopting above-mentioned technical scheme, the screen cloth is fixed on the negative pressure pump, and steam is in the intraductal transportation process of gas transmission, and the screen cloth can filter the impurity in the steam, makes the steam of retrieving purer, and the heat transmission pipe of recovery tank bottom can be used for providing heat energy for other equipment with other equipment intercommunications, has practiced thrift the use cost of enterprise.
The invention is further configured to: the screen mesh is detachably connected with the negative pressure pump.
Through adopting above-mentioned technical scheme, can dismantle the screen cloth and wash after production is accomplished, install the negative pressure pump again after the washing is accomplished, can recycle and can not influence the function of screen cloth, practiced thrift use cost.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without creative efforts.
FIG. 1 is a schematic view of a processing line structure according to an embodiment of the present invention.
FIG. 2 is a schematic structural diagram of a cleaning state of a reaction vessel in the embodiment of the present invention.
FIG. 3 is a schematic diagram of the reaction state structure of the reaction vessel in the embodiment of the present invention.
Fig. 4 is a schematic view of a part a of the enlarged structure in fig. 3.
FIG. 5 is a schematic view of a circulation filter according to an embodiment of the present invention.
FIG. 6 is a schematic view of a connection structure of a curing kettle and a recovery tank in an embodiment of the present invention.
The labels in the figures are:
1-reaction kettle, 2-solidification kettle, 3-circulating filter, 101-kettle body, 102-feed opening, 103-reaction discharge pipe, 104-reaction discharge valve, 105-driving motor, 106-stirring shaft, 107-stirring blade, 108-coupler, 109-heating pipe, 1010-heating seat, 1011-heating rod, 1012-heat transfer hole, 1013-first temperature sensor, 201-solidification feed pipe, 202-solidification discharge pipe, 301-shell, 302-partition plate, 303-first-stage filtering bin, 304-second-stage filtering bin, 305-feed opening, 306-driving roller, 307-driven roller, 308-first-stage filter screen, 309-first-stage guide plate, 3010-first-stage liquid discharge pipe, 3011-cleaning roller, 3012-cleaning brush, 3013-second level guide plate, 3014-second level liquid discharge pipe, 3015-second level filter screen, 3016-particle outlet, 3017-vibration motor, 401-lifting motor, 402-threaded rod, 403-lifting block, 404-brush, 405-threaded groove, 406-limit groove, 407-rotating frame, 408-supporting rod, 409-upper travel switch, 4010-lower travel switch, 4011-upper height regulator, 4012-lower height regulator, 4013-sealing kettle cover, 4014-electric telescopic rod, 4015-baffle, 501-recovery tank, 502-heat insulation layer, 503-gas pipe, 504-solenoid valve, 505-negative pressure pump, 506-second temperature sensor, 507-screen mesh and 508-heat transmission pipe.
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.
As shown in fig. 1-fig. 6, the invention discloses a method for preparing macroporous weakly acidic cation exchange resin, comprising a reaction kettle 1, a curing kettle 2 and a circulating filter 3, wherein a stirrer is arranged in the reaction kettle 1, in the specific embodiment of the invention: comprises the following steps:
s1, taking 1-3 parts of styrene, 60-80 parts of a mixture of acrylic acid and acrylic ester and 5-10 parts of divinylbenzene and triallyl isocyanurate as monomers according to the weight ratio; taking toluene and gasoline or carbon alcohol which are 5-30 percent of the total weight of the monomers as mixed pore-foaming agents, taking benzoyl peroxide which is 0.1-2 percent of the total weight of the monomers and azobisisobutyronitrile which is 0.1-2 percent of the total weight of the monomers as initiators, and mixing to obtain an oil phase;
s2, dissolving 0.2-1 part of cellulose and 250-400 parts of anhydrous calcium chloride in 500 parts of deionized water according to the weight ratio to prepare a calcium chloride aqueous solution with the concentration of 35-40%;
s3, introducing a calcium chloride aqueous solution into a reaction kettle 1, putting an oil phase into the reaction kettle 1 to mix with the calcium chloride aqueous solution, starting a stirrer, rotating at a speed of 40-120 r/min until the particle size of oil droplets is 0.4-1.2mm, starting heating to 65-75 ℃, carrying out constant-temperature reaction, continuing carrying out heat preservation reaction at the temperature for 5 hours, then slowly heating to 75-85 ℃, and carrying out constant-temperature reaction for 2-4 hours; then raising the temperature to 85-95 ℃ at the same heating rate, carrying out constant temperature reaction for 2-4 hours, finally raising the temperature to 97 ℃, keeping the temperature for 8 hours, introducing the mixture into a curing kettle 2 for curing reaction, and filtering the mixture through a circulating filter 3 after the curing reaction is finished to obtain beads;
s4, washing the bead balls with deionized water at the temperature of 75-90 ℃ until the washing liquid is clear; then extracting with acetone, and leaching with ethanol until the washing liquid is clear; obtaining a macroporous cation resin semi-finished product;
s5, taking 150ml of the macroporous cation resin semi-finished product, adding 200ml of 15-25% liquid alkali, and reacting at the constant temperature of 70-90 ℃ for 5-10 h; after the reaction is finished, filling the column, washing the column with deionized water with the same volume, then passing 1N hydrochloric acid with 2 times of volume through the column for 1h-2h, and then washing the column with deionized water until the column is neutral to obtain the macroporous weakly acidic cation exchange resin.
By adopting the technical scheme, the production method of the macroporous weakly-acidic cation exchange resin has reasonable process design and high quality of the obtained product, compared with the prior art, the polyacrylic resin can be directly obtained by polymerizing acrylic acid, alcohol groups are not removed by hydrolysis, the price of the acrylic acid is low, and the utilization rate of raw materials can be improved in any aspect.
The invention also discloses a device suitable for the macroporous weak acid cation exchange resin method, which comprises the following steps: in a specific embodiment of the invention: the production line comprises a reaction kettle 1, a curing kettle 2 and a circulating filter 3 which are sequentially connected, wherein the reaction kettle 1 comprises a kettle body 101, a feeding port 102 is arranged at the top of the kettle body 101, a reaction discharging pipe 103 is arranged at the bottom of the kettle body 101, a reaction discharging valve 104 is arranged on the reaction discharging pipe 103, the stirrer comprises a driving motor 105, a stirring shaft 106 and a stirring blade 107, the stirring shaft 106 is hollow, one end of the stirring shaft 106 is in transmission connection with the driving motor 105 through a shaft coupling 108, a heating pipe 109 is arranged on the outer wall of the kettle body 101, a heating seat 1010 is arranged at the bottom of the kettle body 101, a heating rod 1011 is arranged at the top of the heating seat 1010, the upper end of the heating rod 1011 extends into the stirring shaft 106 after penetrating through the bottom of the kettle body 101, a plurality of heat transfer holes 1012 are arranged on the stirring shaft 106, a first temperature sensor 1013 is arranged on the inner wall of the kettle, and a curing feed pipe 201 and a curing discharge pipe 202 are arranged on the curing kettle 2, the curing feed pipe 201 is communicated with the reaction discharge pipe 103, and the curing discharge pipe 202 is connected with the circulating filter 3.
By adopting the technical scheme, the reaction discharge pipe 103 of the reaction kettle 1 is communicated with the curing feed pipe 201 of the curing kettle 2, the curing discharge pipe 202 of the curing kettle 2 is connected with the circulating filter 3, so that the reaction kettle 1, the curing kettle 2 and the circulating filter 3 are sequentially connected into a processing production line, the production efficiency is improved, calcium chloride aqueous solution and oil phase are sequentially fed into the kettle body 101 through the feed inlet 102, the driving motor 105 is started, the coupler 108 is connected with the output shaft of the driving motor 105 and the stirring shaft 106, the stirring shaft 106 rotates and simultaneously drives the stirring blades 107 to stir the mixed solution under the connection of the coupler 108, the mixed solution is accelerated to react, the heating pipe 109 is started to heat the outer wall of the kettle body 101, heat is transferred into the kettle body 101 through the outer wall of the kettle body 101, the heating seat 1010 is started to heat the heating rod 1011 on the heating pipe 109 while the heating pipe 109 is heated, so that the heating rod 1011 heats the inside of the stirring shaft 106, and heat is transferred out through the heat transfer hole 1012 on the stirring shaft 106, so that the inside and the outside of the kettle body 101 are heated simultaneously, and the required temperature can be reached more quickly, thereby improving the production efficiency, the temperature inside the kettle body 101 can be monitored in real time by the first temperature sensor 1013, when the temperature inside the kettle body 101 reaches the required value, the heating pipe 109 and the heating rod 1011 stop heating, after the constant temperature reaction is fixed, one of the heating pipe 109 or the heating rod 1011 heats the kettle body 101 to meet the production requirement, the reaction discharge valve 104 is closed during the reaction, the reaction discharge valve 104 is opened after the reaction is completed, the reaction liquid is guided into the curing kettle 2 through the reaction discharge pipe 103 and the curing kettle 201 to carry out the curing reaction, after the reaction kettle 1 is used, the oil stain remained on the inner wall of the kettle body 101 can be cleaned in time by the cleaning assembly, thereby avoiding the phenomenon that the, the cleaning is time-saving and labor-saving relatively to manual cleaning.
In a specific embodiment of the invention: the circulating filter 3 comprises a shell 301, a partition plate 302 is vertically arranged in the middle of the shell 301, the partition plate 302 separates the inner wall of the shell 301 into a primary filtering bin 303 and a secondary filtering bin 304, the primary filtering bin 303 is communicated with the top of the secondary filtering bin 304, a feed inlet 305 is arranged at the top of the shell 301, the upper end of the feed inlet 305 is communicated with a curing discharge pipe 202, the lower end of the feed inlet 305 is communicated with the top of the primary filtering bin 303, a driving roller 306 is arranged at the top of the secondary filtering bin 304, a driven roller 307 is arranged at the top of the primary filtering bin 303, the same primary filter screen 308 is sleeved on the driving roller 306 and the driven roller 307, a primary guide plate 309 is obliquely arranged at the bottom of the primary filtering bin 303, a primary discharge pipe 3010 is arranged at the lower part of the primary guide plate 309, the primary discharge pipe 3010 extends to the outside, cleaning roller 3011 outside cover is equipped with cleaning brush 3012, cleaning brush 3012 can wash one-level filter screen 308, the slope of second grade filter storehouse 304 bottom is equipped with second grade guide plate 3013, second grade guide plate 3013 lower part is equipped with second grade fluid-discharge tube 3014, second grade fluid-discharge tube 3014 extends to the casing 301 outside, second grade guide plate 3013 top is equipped with second grade filter screen 3015, second grade filter screen 3015 slope sets up, second grade filter screen 3015 lower part is equipped with granule export 3016, second grade filter screen 3015 bottom is equipped with vibrating motor 3017.
By adopting the technical scheme, the feed inlet 305 is communicated with the solidification discharge pipe 202, after solidification reaction, a solidified product is guided into the primary filter bin 303 through the solidification discharge pipe 202 and the feed inlet 305, the solidified product falls on the primary filter screen 308 from the feed inlet 305 for filtering, unqualified products and liquid pass through the primary filter screen 308 and fall down on the primary guide plate 309 and are discharged through the primary liquid discharge pipe 3010 along the primary guide plate 309, qualified products are left on the primary filter screen 308, the driving roller 306 rotates while the primary filter screen 308 filters, the primary filter screen 308 transports the qualified products to the secondary filter bin 304 under the coordination of the driven roller 307, the cleaning roller 3011 also rotates while the driving roller 306 rotates, the cleaning roller 3011 rotates to drive the cleaning brush 3012 to rotate, the cleaning brush 3012 cleans the primary filter screen 308 and pushes down the qualified products on the primary filter screen 308, the problem that meshes of the primary filter screen 308 are blocked is avoided, qualified products fall downwards on the secondary filter screen 3015 under the pushing of the cleaning brush 3012, the secondary filter screen 3015 is arranged in a tilted mode, the meshes of the secondary filter screen 3015 are larger than the meshes of the primary filter screen 308, the qualified products are screened through the primary filter screen 308, the products with undersize particles are mixed in the qualified products, the products penetrate through the secondary filter screen 3015 and fall on the secondary guide plate 3013 and are discharged downwards along the secondary guide plate 3013 through the secondary liquid discharge pipe 3014, the qualified products after being screened for two times roll downwards along the secondary filter screen 3015 to the particle outlet 3016 for collection, when the secondary filter screen 3015 is used for filtering, the vibrating motor 3017 is started to drive the secondary filter screen 3015 to vibrate upwards and downwards, and the filtering efficiency of the secondary filter screen 3015 and the collection efficiency of.
In a specific embodiment of the invention: the cleaning component comprises a lifting motor 401, a threaded rod 402, a lifting block 403 and a brush 404, the lifting motor 401 is fixed at the upper end inside the stirring shaft 106, the threaded rod 402 is in transmission connection with the lifting motor 401, a threaded groove 405 is arranged on the lifting block 403, the lifting block 403 is sleeved on the outer wall of the threaded rod 402 through the threaded groove 405 and the threaded rod 402 in a threaded fit manner, a limit groove 406 is arranged on the inner wall of the stirring shaft 106 along the vertical direction, one side of the lifting block 403 extends into the limit groove 406 and can slide along the length direction of the limit groove 406, a rotating frame 407 is arranged on the outer wall of the stirring shaft 106 and below the limit groove 406, one end of the rotating frame 407 is hinged with the outer wall of the stirring shaft 106, the brush 404 is fixed at one end of the rotating frame 407 far away from the stirring shaft 106, a support rod 408 is hinged at the middle part of, and a detection assembly for detecting the upper limit position and the lower limit position is arranged on the lifting block 403.
By adopting the technical scheme, in the reaction process of the mixed solution, the lifting block 403 is positioned at the upper part of the threaded rod 402, the rotating frame 407 is in a vertical state, the supporting rod 408 fixes the rotating frame 407, after the reaction kettle 1 is used, the lifting motor 401 is started to drive the threaded rod 402 to rotate, the threaded rod 402 provides a rotating thrust for the lifting block 403, under the limiting action of the limiting groove 406, the lifting block 403 moves downwards on the outer wall of the threaded rod 402, the lifting block 403 moves downwards while driving the end, hinged to the lifting block 403, of the supporting rod 408 to move downwards, the end, far away from the lifting block 403, of the supporting rod 408 starts to open towards the side far away from the lifting block 403, the end, far away from the lifting block 403, of the supporting rod 408 is hinged to the middle part of the rotating frame 407, and downwards turns over with the hinged point between the rotating frame 407 and the stirring shaft 106 as the supporting, the lifting motor 401 is turned off, the threaded rod 402 stops rotating, the lifting block 403 stops moving downwards, the support rod 408 stops moving downwards, the rotating frame 407 is in a horizontal state at the moment, the brush 404 at the end, away from the stirring shaft 106, of the rotating frame 407 abuts against the inner wall of the kettle body 101, the support rod 408 fixes the rotating frame 407, the driving motor 105 is started to drive the stirring shaft 106 to rotate at the moment, the stirring shaft 106 rotates to drive the brush 404 to wash the inner wall of the kettle body 101 through the rotating frame 407, oil stains remained on the inner wall of the kettle body 101 are washed, the driving motor 105 is turned off after the washing is finished, the stirring shaft 106 stops rotating, the brush 404 stops washing, the lifting motor 401 is started to drive the threaded rod 402 to rotate reversely at the moment, the threaded rod 402 drives the lifting block 403 to move upwards, the lifting block 403 drives one end of the support rod 408 to move, elevator motor 401 closes, threaded rod 402 stall, elevator 403 stops the upward movement, bracing piece 408 stops the rebound, rotating turret 407 is vertical state this moment, wait for going on of next reaction, compare with prior art, this structure can drive brush 404 through (mixing) shaft 106 and rotate and wash the cauldron body 101 inner wall, saved manual cleaning's trouble, the cleaning efficiency is high, brush 404 can pack up after the washing is accomplished, can not influence going on of reaction.
In a specific embodiment of the invention: the detection assembly comprises an upper travel switch 409 and a lower travel switch 4010, the upper travel switch 409 is fixed on the upper surface of the lifting block 403 and located on one side of the limiting groove 406, a contact of the upper travel switch 409 faces upwards, the lower travel switch 4010 is fixed on the lower surface of the lifting block 403 and located on one side of the limiting groove 406, and a contact of the lower travel switch 4010 faces downwards.
Through adopting above-mentioned technical scheme, in the lift piece 403 downward movement in-process, lower travel switch 4010 stands by in real time, when lower travel switch 4010's contact triggered lower travel switch 4010 with the lower lateral wall contact of spacing groove 406, lift motor 401 closes, lift piece 403 stops the downstream, in the lift piece 403 upward movement in-process, go up travel switch 409 and stand by in real time, when the contact of going up travel switch 409 and the lateral wall contact trigger upward travel switch 409 on spacing groove 406, lift motor 401 closes, lift piece 403 stops the upward movement, through the setting of last travel switch 409 and lower travel switch 4010, make the lift of lift piece more accurate, it is safer to use.
In a specific embodiment of the invention: cauldron body 101 upper portion is equipped with detachable sealed kettle cover 4013, be equipped with electric telescopic handle 4014 between rotating turret 407 and the brush 404, the one end fixed connection of (mixing) shaft 106 is kept away from to electric telescopic handle 4014 one end and rotating turret 407, the electric telescopic handle 4014 other end and brush 404 fixed connection, be equipped with height adjuster 4011 between last travel switch 409 and the elevator 403 upper surface, be equipped with down height adjuster 4012 between lower travel switch 4010 and the elevator 403 lower surface.
By adopting the technical scheme, the sealing kettle cover 4013 is detachably connected with the kettle body 101, the stirring shaft 106 and the components on the stirring shaft 106 can be moved out of the kettle body 101 by detaching the sealed kettle cover 4013, the inner parts of the kettle bodies 101 of different reaction kettles 1 have different sizes, the distance between the brush 404 and the rotating rack 407 can be adjusted by the electric telescopic rod 4014 between the rotating rack 407 and the brush 404, so that the electric telescopic rod can be adapted to different reaction kettles 1, when different stirring shafts 106 need to be replaced due to different depths of different kettle bodies 101, the spacing grooves 406 on the stirring shaft 106 are different, the upper height adjuster 4011 can adjust the distance between the upper travel switch 409 and the lifting block 403, and the lower height adjuster 4012 can adjust the distance between the lower travel switch 4010 and the lifting block 403, so that the upper limit position and the lower limit position of the lifting block 403 and the position of the rotating frame 407 can reach the optimal and most suitable state, the interchangeability is good, and the use cost can be saved.
In a specific embodiment of the invention: the width of the rotating frame 407 is greater than that of the limit groove 406, a baffle 4015 is arranged between the threaded rod 402 and the heating rod 1011, and the side wall of the baffle 4015 abuts against the inner wall of the stirring shaft 106.
Through adopting above-mentioned technical scheme, baffle 4015 is the heat insulating board, baffle 4015 lateral wall offsets with (mixing) shaft 106 inner wall, can prevent that the heat directly rises to threaded rod 402 around, can reduce the heat that heating rod 1011 produced to threaded rod 402 and elevator motor 401's influence, the width of rotating turret 407 is greater than the width of spacing groove 406, when being in the reaction process, rotating turret 407 is vertical state, rotating turret 407 can block spacing groove 406, avoid reaction liquid to splash and get into the inside elevator motor 401 that influences of (mixing) shaft 106 through spacing groove 406.
In a specific embodiment of the invention: 2 one side of curing kettle is equipped with retrieves jar 501, it is equipped with heat preservation 502 on the jar 501 inner wall to retrieve, be equipped with gas-supply pipe 503 on the 2 lateral walls of curing kettle, the one end that gas-supply pipe 503 is close to curing kettle 2 is equipped with solenoid valve 504, curing kettle 2's one end and recovery jar 501 intercommunication are kept away from to gas-supply pipe 503, be equipped with negative pressure pump 505 on the gas-supply pipe 503, be equipped with second temperature sensor 506 on the 2 inner walls of curing kettle.
Through adopting above-mentioned technical scheme, curing kettle 2 produces the heat in the curing reaction in-process, second temperature sensor 506 can the inside temperature of real-time supervision curing kettle 2, when the temperature risees to a definite value, solenoid valve 504 is opened, negative pressure pump 505 starts and forms the atmospheric pressure difference, steam in curing kettle 2 gets into through gas-supply pipe 503 under negative pressure pump 505 and collects in retrieving jar 501, the heat dissipation in retrieving jar 501 can be avoided to the heat preservation 502 on retrieving jar 501 inner wall, compared with the prior art, this structure can be retrieved the heat that curing reaction produced, avoid the heat to be wasted by vain.
In a specific embodiment of the invention: a screen 507 is arranged on the negative pressure pump 505, the screen 507 is positioned between the negative pressure pump 505 and the gas transmission pipe 503, and the bottom of the recovery tank 501 is provided with a heat transmission pipe 508.
Through adopting above-mentioned technical scheme, screen cloth 507 is fixed on negative pressure pump 505, and hot gas is in the air-supply pipe 503 in transportation process, and screen cloth 507 can filter the impurity in the hot gas, makes the hot gas of retrieving purer, and the heat transmission pipe 508 of retrieving jar 501 bottom can be used for providing heat energy for other equipment with other equipment intercommunications, has practiced thrift the use cost of enterprise.
In a specific embodiment of the invention: the screen 507 is detachably connected to the negative pressure pump 505.
Through adopting above-mentioned technical scheme, can dismantle the screen cloth 507 after production is accomplished and wash, install negative pressure pump 505 again after the washing is accomplished on, can recycle and can not influence the function of screen cloth 507, practiced thrift use cost.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (10)
1. A method for preparing macroporous weakly acidic cation exchange resin comprises a reaction kettle, a curing kettle and a circulating filter, wherein a stirrer is arranged in the reaction kettle, and the method is characterized in that: comprises the following steps:
s1, taking 1-3 parts of styrene, 60-80 parts of a mixture of acrylic acid and acrylic ester and 5-10 parts of divinylbenzene and triallyl isocyanurate as monomers according to the weight ratio; taking toluene and gasoline or carbon alcohol which are 5-30 percent of the total weight of the monomers as mixed pore-foaming agents, taking benzoyl peroxide which is 0.1-2 percent of the total weight of the monomers and azobisisobutyronitrile which is 0.1-2 percent of the total weight of the monomers as initiators, and mixing to obtain an oil phase;
s2, dissolving 0.2-1 part of cellulose and 250-400 parts of anhydrous calcium chloride in 500 parts of deionized water according to the weight ratio to prepare a calcium chloride aqueous solution with the concentration of 35-40%;
s3, introducing a calcium chloride aqueous solution into a reaction kettle, putting an oil phase into the reaction kettle to mix with the calcium chloride aqueous solution, starting a stirrer at a rotating speed of 40-120 r/min until the particle size of oil droplets is 0.4-1.2mm, starting to heat to 65-75 ℃, carrying out constant-temperature reaction, continuing to carry out heat preservation reaction at the temperature for 5 hours, then slowly heating to 75-85 ℃, and carrying out constant-temperature reaction for 2-4 hours; then raising the temperature to 85-95 ℃ at the same heating rate, carrying out constant temperature reaction for 2-4 hours, finally raising the temperature to 97 ℃, keeping the temperature for 8 hours, introducing the mixture into a curing kettle for curing reaction, and filtering the mixture through a circulating filter after the curing reaction is finished to obtain beads;
s4, washing the bead balls with deionized water at the temperature of 75-90 ℃ until the washing liquid is clear; then extracting with acetone, and leaching with ethanol until the washing liquid is clear; obtaining a macroporous cation resin semi-finished product;
s5, taking 150ml of the macroporous cation resin semi-finished product, adding 200ml of 15-25% liquid alkali, and reacting at the constant temperature of 70-90 ℃ for 5-10 h; after the reaction is finished, filling the column, washing the column with deionized water with the same volume, then passing 1N hydrochloric acid with 2 times of volume through the column for 1h-2h, and then washing the column with deionized water until the column is neutral to obtain the macroporous weakly acidic cation exchange resin.
2. An apparatus adapted for the method of macroporous weakly acidic cation exchange resin of claim 1, characterized in that: the device comprises a processing production line, wherein the processing production line comprises a reaction kettle, a curing kettle and a circulating filter which are sequentially connected, the reaction kettle comprises a kettle body, a feed port is arranged at the top of the kettle body, a reaction discharge pipe is arranged at the bottom of the kettle body, a reaction discharge valve is arranged on the reaction discharge pipe, a stirrer comprises a driving motor, a stirring shaft and stirring blades, the stirring shaft is hollow, one end of the stirring shaft is in transmission connection with the driving motor through a shaft coupling, a heating pipe is arranged on the outer wall of the kettle body, a heating seat is arranged at the bottom of the kettle body, a heating rod is arranged at the top of the heating seat, the upper end of the heating rod penetrates through the bottom of the kettle body and then extends into the stirring shaft, a plurality of heat transfer holes are arranged on the stirring shaft, a first temperature sensor is arranged on the inner wall of the kettle, the solidification feed pipe is communicated with the reaction discharge pipe, and the solidification discharge pipe is connected with the circulating filter.
3. The apparatus of claim 2, wherein the apparatus comprises: the circulating filter comprises a shell, a partition plate is vertically arranged in the middle of the shell and divides the inner wall of the shell into a primary filtering bin and a secondary filtering bin, the primary filtering bin is communicated with the top of the secondary filtering bin, a feed inlet is arranged at the top of the shell, the upper end of the feed inlet is communicated with a solidifying discharge pipe, the lower end of the feed inlet is communicated with the top of the primary filtering bin, a driving roller is arranged at the top of the secondary filtering bin, a driven roller is arranged at the top of the primary filtering bin, the same primary filtering net is sleeved on the driving roller and the driven roller, a primary flow guide plate is obliquely arranged at the bottom of the primary filtering bin, a primary flow discharge pipe is arranged at the lower part of the primary flow guide plate and extends out of the shell, a cleaning roller is arranged at one side of the driving roller far, the secondary filter storehouse bottom slope is equipped with the second grade guide plate, second grade guide plate lower part is equipped with the second grade fluid-discharge tube, the second grade fluid-discharge tube extends to the casing outside, second grade guide plate top is equipped with the second grade filter screen, the slope of second grade filter screen sets up, second grade filter screen lower part is equipped with the granule export, second grade filter screen bottom is equipped with vibrating motor.
4. The apparatus of claim 3 for a method of macroporous weakly acidic cation exchange resin, wherein: the cleaning component comprises a lifting motor, a threaded rod, a lifting block and a brush, the lifting motor is fixed at the upper end inside the stirring shaft, the threaded rod is in transmission connection with a lifting motor, the lifting block is provided with a thread groove, the lifting block is sleeved on the outer wall of the threaded rod through the thread fit of the thread groove and the threaded rod, a limit groove is arranged on the inner wall of the stirring shaft along the vertical direction, one side of the lifting block extends into the limit groove and can slide along the length direction of the limit groove, a rotating frame is arranged on the outer wall of the stirring shaft and below the limiting groove, one end of the rotating frame is hinged with the outer wall of the stirring shaft, the brush is fixed at one end of the rotating frame far away from the stirring shaft, the middle part of the rotating frame is hinged with a supporting rod, one end of the support rod, which is far away from the rotating frame, is hinged with the side wall of the lifting block, and the lifting block is provided with a detection assembly for detecting the upper limit position and the lower limit position.
5. The apparatus of claim 4 for a method of macroporous weakly acidic cation exchange resin, wherein: the detection assembly comprises an upper travel switch and a lower travel switch, the upper travel switch is fixed on the upper surface of the lifting block and located on one side of the limiting groove, the contact of the upper travel switch faces upwards, the lower travel switch is fixed on the lower surface of the lifting block and located on one side of the limiting groove, and the contact of the lower travel switch faces downwards.
6. The apparatus of claim 5 for a method of macroporous weakly acidic cation exchange resin, wherein: cauldron body upper portion is equipped with the sealed kettle cover of detachable, be equipped with electric telescopic handle between rotating turret and the brush, the one end fixed connection of (mixing) shaft is kept away from to electric telescopic handle one end and rotating turret, the electric telescopic handle other end and brush fixed connection, be equipped with height adjuster between last travel switch and the elevator upper surface, be equipped with down height adjuster between lower travel switch and the elevator lower surface.
7. The apparatus of claim 6 for a method of macroporous weakly acidic cation exchange resin, wherein: the width of rotating turret is greater than the width of spacing groove, be equipped with the baffle between threaded rod and the heating rod, the baffle lateral wall offsets with the (mixing) shaft inner wall.
8. The apparatus of claim 7 for a method of macroporous weakly acidic cation exchange resin, wherein: the curing kettle is characterized in that a recovery tank is arranged on one side of the curing kettle, a heat preservation layer is arranged on the inner wall of the recovery tank, a gas pipe is arranged on the side wall of the curing kettle, an electromagnetic valve is arranged at one end, close to the curing kettle, of the gas pipe, one end, far away from the curing kettle, of the gas pipe is communicated with the recovery tank, a negative pressure pump is arranged on the gas pipe, and a second temperature sensor is arranged on the inner wall of the curing.
9. The apparatus of claim 8 for a method of macroporous weakly acidic cation exchange resin, wherein: the negative pressure pump is provided with a screen, the screen is positioned between the negative pressure pump and the gas pipe, and the bottom of the recovery tank is provided with a heat transmission pipe.
10. The apparatus of claim 9 for a method of macroporous weakly acidic cation exchange resin, wherein: the screen mesh is detachably connected with the negative pressure pump.
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Effective date of registration: 20230822 Address after: 324000 No. 19 Development Avenue, Zhejiang Longyou Economic Development Zone, Donghua Street, Longyou County, Quzhou City, Zhejiang Province Patentee after: Zhejiang Tianqi Biochemical Co.,Ltd. Address before: No.5, Huishang Road, Longyou Industrial Park, Longyou County, Quzhou City, Zhejiang Province 324400 Patentee before: ZHEJIANG TIANSHUN BIOTECHNOLOGY CO.,LTD. |