CN116585978A - Triglycidyl isocyanurate melting granulation production system and production method - Google Patents

Triglycidyl isocyanurate melting granulation production system and production method Download PDF

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Publication number
CN116585978A
CN116585978A CN202310772473.2A CN202310772473A CN116585978A CN 116585978 A CN116585978 A CN 116585978A CN 202310772473 A CN202310772473 A CN 202310772473A CN 116585978 A CN116585978 A CN 116585978A
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triglycidyl isocyanurate
melt
granulation
crystallizer
pipeline
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Inventor
杨志萍
林光伟
项纯
何领
汪泽军
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HUANGSHAN HUAHUI TECHNOLOGY CO LTD
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HUANGSHAN HUAHUI TECHNOLOGY CO LTD
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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
    • B01J2/00—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic
    • B01J2/26—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic on endless conveyor belts
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D1/00—Evaporating
    • B01D1/22—Evaporating by bringing a thin layer of the liquid into contact with a heated surface
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/02—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping in boilers or stills
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D9/00—Crystallisation
    • B01D9/0004—Crystallisation cooling by heat exchange
    • B01D9/0013—Crystallisation cooling by heat exchange by indirect heat exchange
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D9/00—Crystallisation
    • B01D9/0059—General arrangements of crystallisation plant, e.g. flow sheets
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D9/00—Crystallisation
    • B01D9/0063—Control or regulation
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D9/00—Crystallisation
    • B01D9/02—Crystallisation from solutions
    • 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
    • B01J6/00—Heat treatments such as Calcining; Fusing ; Pyrolysis
    • B01J6/005—Fusing
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07D—HETEROCYCLIC COMPOUNDS
    • C07D405/00—Heterocyclic compounds containing both one or more hetero rings having oxygen atoms as the only ring hetero atoms, and one or more rings having nitrogen as the only ring hetero atom
    • C07D405/14—Heterocyclic compounds containing both one or more hetero rings having oxygen atoms as the only ring hetero atoms, and one or more rings having nitrogen as the only ring hetero atom containing three or more hetero rings
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/10—Process efficiency

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

The invention relates to a triglycidyl isocyanurate melting granulation production system and a production method, and belongs to the technical field of triglycidyl isocyanurate granulation. Solves the technical problems of high volatile matter residue, large dust amount, complicated process for preparing TGIC particles by using a melt granulation process, large process safety risk, immature technology, unstable product quality and the like in the preparation of TGIC particles by using an extrusion granulation process in the prior art. The production system comprises a melting kettle, a temporary storage kettle, a thin film evaporator, a crystallizer, a distributing device and a steel belt granulator. The invention also provides a method for producing triglycidyl isocyanurate particles by using the production system. The melting granulation production system and the production method have the advantages of high efficiency, good continuity and good safety, and the prepared TGIC particles are free of powder, stable and uniform in quality and high in reliability.

Description

Triglycidyl isocyanurate melting granulation production system and production method
Technical Field
The invention belongs to the technical field of triglycidyl isocyanurate granulation, and particularly relates to a triglycidyl isocyanurate (TGIC) melt granulation production system and a production method.
Background
Triglycidyl isocyanurate (TGIC), the academic name (1H, 3H, 5H) -tris (2, 3-epoxypropyl) -s-triazine-2, 4, 6-trione, is a curing agent with excellent performance. TGIC contains three epoxy groups and triazine ring structures, and is crosslinked and solidified with acid or anhydride to form a coating film, so that the coating film has excellent heat resistance, weather resistance, chemical resistance, high temperature resistance and the like, and is widely applied to the fields of powder coating, electronic ink, packaging and the like.
In the prior art, the production process of TGIC generally comprises: synthesizing, distilling, crystallizing, wet extrusion granulating, drying and the like. The wet powder extrusion granulation is a granulation mode by physical extrusion, which is easy to cause solvent residue, thus leading to long drying process time, and the produced TGIC particles have insufficient strength, serious powder falling phenomenon exists in transportation and use, and the problem of large dust amount is caused.
In order to reduce the dust of TGIC particles and the residual amount of solvent, in recent years, it has been proposed to produce TGIC particles by melt granulation. For example, chinese patent discloses a melting granulation process of triglycidyl isocyanurate and a production line thereof (publication No. 101773806A), the melting granulation process uses a distillation kettle to carry out normal pressure and reduced pressure distillation at different temperatures, and after all the organic solvent is distilled out, the materials in the distillation kettle are uniformly placed on a belt-type cooling conveyor, cooled and crushed. However, the process still cannot effectively reduce the residual solvent content in the product, and the product still needs to be crushed after passing through a belt cooler, the process is complex, fine powder still can be generated in the crushing process, and the particle size is uneven. As further disclosed in chinese patent publication No. 103896929a, the granulation production line comprises a vibration dryer, wherein the vibration dryer is provided with a material inlet, a material outlet and a gas outlet, the gas outlet of the vibration dryer is connected with the inlet of a condenser, and the outlet of the condenser is sequentially connected with a solvent recovery tank and a gas induced draft fan i; the material outlet of the vibration dryer is connected with the material inlet of the dry powder cyclone separator through a conveying pipeline, an emptying valve and a material discharging bottom valve are arranged on the conveying pipeline, a coarse material powder outlet and a fine material powder outlet are respectively arranged on the dry powder cyclone separator, the coarse material powder outlet is connected with one material inlet of the dry powder tank, the fine material powder outlet is connected with the cloth bag dust remover, one end of the cloth bag dust remover is connected with the induced draft fan II, the other end of the cloth bag dust remover is connected with the other material inlet of the dry powder tank, the material outlet of the dry powder tank is sequentially connected with the material extruder, the tablet press, the belt cooling conveyor, the pulverizer, the screening machine and the packaging machine, the water inlet and the water outlet of the condenser are connected with the cooling water pipeline, and the interlayer of the vibration dryer is connected with the steam pipeline. However, the TGIC wet material is used in the granulating production line to be dried into a dry powder raw material, the dust amount is large, the working environment is poor, the products of the same melting granulation need crushing and screening procedures, the problems of dust and uneven particle size are also caused, the procedures are complicated, and the energy consumption is high. Further, as disclosed in chinese patent, a TGIC production method (publication No. 108299403 a) of granulating molten steel strip, in which epichlorohydrin, cyanuric acid and tetramethylammonium chloride catalyst are added into a reaction vessel, heated and subjected to synthesis reaction under normal pressure to obtain an intermediate product, and then added with solid base to perform cyclization reaction; filtering, standing and layering the cyclization reaction product, and heating and distilling the lower organic phase under reduced pressure; crystallizing and centrifuging the distilled material to obtain TGIC crystals containing volatile organic compounds; placing the TGIC crystal containing the volatile organic compounds in a vacuum environment, and heating to obtain TGIC in a molten state; the TGIC is quickly cooled to form TGIC particles which are hard in texture and not easy to generate dust. However, the production method adopts TGIC materials containing methanol as main volatile substances to remove solvents in a heating and reduced pressure distillation mode, because TGIC is a heat-sensitive substance, a large amount of molten materials are easy to carbonize at high temperature for a long time, so that the safety risk is caused, TGIC crystals containing volatile organic substances are placed in a vacuum environment, the materials are thick in accumulation degree under the heating in a single melting kettle, only low-boiling-point volatile solvents can be removed, ECH residues in products are high, and the quality is not up to standard. And as disclosed in Chinese patent, an integrated processing method of efficient devolatilization and melt extrusion granulation of TGIC (publication No. 114130303A) is disclosed, the processing method melts TGIC wet powder in a double-screw extruder, the melted TGIC is conveyed to a discharge port of the double-screw extruder under the action of double screws, and the melt is uniformly formed into spherical liquid through a material distributing machine head and is dripped on a formed steel belt to form TGIC particles. Although the process can realize the preparation of the granular TGIC without dust, the process is subject to the defect that equipment is a vacuum system, the vacuum is unstable, the solvent residue is not removed stably, the process is incomplete, the product quality is unstable, in addition, TGIC powder seed crystal without epichlorohydrin and methanol is required to be input in the processing method, the product forming process time is long, the equipment investment is large, and the production efficiency is low.
In summary, the method for preparing TGIC particles by adopting the melt granulation method in the prior art has the technical problems of complex procedures, high process safety risk, immature technology, unstable product quality and the like.
Disclosure of Invention
In view of the above, the invention provides a triglycidyl isocyanurate melt granulation production system and a production method for solving the technical problems of high volatile matter residue, large dust amount, complicated process for preparing TGIC particles by using a melt granulation process, high process safety risk, immature technology, unstable product quality and the like in the prior art.
In order to achieve the above object, the present invention adopts the following technical scheme.
The invention provides a triglycidyl isocyanurate melting granulation production system, which comprises a melting kettle, a temporary storage kettle, a thin film evaporator, a crystallizer, a distributing device and a steel belt granulator, wherein the melting kettle is connected with the temporary storage kettle; the discharge port of the melting kettle is communicated with the feed port of the temporary storage kettle through a first pipeline, the discharge port of the temporary storage kettle is communicated with the feed port of the thin film evaporator through a second pipeline, the discharge port of the thin film evaporator is communicated with the feed port of the third melt pump through a third pipeline, the discharge port of the third melt pump is communicated with the feed port of the crystallizer through a fourth pipeline, the discharge port of the crystallizer is communicated with the feed port of the third melt pump through a fifth pipeline, the discharge port of the crystallizer is communicated with the feed port of the distributor through a sixth pipeline, and the steel belt granulator is arranged below the discharge port of the distributor.
Preferably, the first pipeline is provided with a first melt pump, the second pipeline is provided with a second melt pump, and the sixth pipeline is provided with a fourth melt pump.
Preferably, valves are arranged on the first pipeline, the second pipeline, the third pipeline and the sixth pipeline.
Preferably, the sixth pipeline is provided with a digital remote transmission pressure gauge.
Preferably, the production system further comprises a first condenser and a first collecting tank, one end of the first condenser is communicated with the melting kettle, the other end of the first condenser is communicated with the first collecting tank, and the first condenser can condense volatilized methanol in the melting kettle and store the volatilized methanol in the first collecting tank.
Preferably, the production system further comprises a second condenser and a second collecting tank, one end of the second condenser is communicated with the thin film evaporator, the other end of the second condenser is communicated with the second collecting tank, and the second condenser can condense volatilized epichlorohydrin in the thin film evaporator and store the volatilized epichlorohydrin in the second collecting tank.
The invention also provides a method for producing triglycidyl isocyanurate by melting and granulating, which comprises the following steps:
step one, adding wet triglycidyl isocyanurate powder containing methanol into a melting kettle;
step two, after the wet powder of triglycidyl isocyanurate containing methanol is kept at 65-90 ℃ for 60-90 min, the methanol is distilled off, and the obtained molten material is conveyed to a temporary storage kettle;
preheating a film evaporator to 105-130 ℃ and controlling the pressure to be minus 0.095-minus 0.1Mpa, continuously conveying the molten materials in the temporary storage kettle to the film evaporator, and removing epichlorohydrin under reduced pressure to obtain transparent molten materials;
step four, conveying the transparent melt material to a crystallizer through a third melt pump, preserving heat for 20-30 min at 95-105 ℃, simultaneously, pushing the transparent melt material in the crystallizer by the third melt pump to self-circulate, cooling to 80-95 ℃ at a cooling rate of 0.3-0.5 ℃/min, and controlling the light transmittance to 15-35%, thus obtaining the crystallized material;
step five, conveying the crystallized material to a distributing device, controlling the pressure of the crystallized material to be 0.15-0.45 MPa, uniformly dripping the crystallized material onto a steel belt granulator, and cooling and forming to obtain triglycidyl isocyanurate particles;
the temperature of the steel belt granulator is gradually reduced along the moving direction of the crystallized materials, and the temperature interval is 15-80 ℃.
Preferably, in the first step, the wet powder of triglycidyl isocyanurate containing methanol is obtained by: adding cyanuric acid, epoxy chloropropane and catalyst benzyl triethyl ammonium chloride into a reaction vessel according to the mass ratio of 1:10-15:0.02-0.06, heating to 100-110 ℃ under normal pressure to carry out synthesis reaction, adding caustic soda flakes according to the mass ratio of cyanuric acid to caustic soda flakes according to the mass ratio of 1:1-1.3, carrying out cyclization reaction at 15-25 ℃, filtering the obtained cyclization reaction product, layering, distilling a lower organic phase to recover epoxy chloropropane, crystallizing distilled materials with methanol, centrifuging, and adding the obtained methanol-containing triglycidyl isocyanurate wet powder into a melting kettle.
Preferably, in the second step, the temperature is kept at 70-80 ℃ for 60-90 min.
Preferably, in the second step, the distilled methanol is condensed by a first condenser to a first collecting tank for collection.
Preferably, the second step is performed under stirring at a stirring speed of 40 to 60rpm.
Preferably, in the third step, the preheating temperature is 110 to 120 ℃.
Preferably, in the third step, the epichlorohydrin removed under reduced pressure is condensed by a second condenser to a second collecting tank for collection.
Preferably, in the fourth step, the crystallizer is filled with circulating cooling water, and the filling amount of the cooling water is controlled by a valve.
Preferably, in the fourth step, the stirring speed of the crystallizer is 15 to 30rpm.
Preferably, in the fourth step, the temperature is kept between 95 ℃ and 100 ℃ and is reduced to 83 ℃ to 90 ℃.
Preferably, in the fourth step, the light transmittance is controlled to be 20 to 30%.
Preferably, in the fourth step, the speed of self-circulation of the transparent melt material in the third melt pump pushing crystallizer is 30-60L/min.
Preferably, in the fifth step, the crystallization material is conveyed to the distributor through a fourth melt pump, the rotation displacement of the fourth melt pump is 30-45L/min, and the crystallization material is uniformly dropped onto the steel belt granulator.
Preferably, in the fifth step, the cooling temperature of the first 0% -less than 20% of the length of the granulating section of the steel belt granulator is 50-80 ℃, the cooling temperature of the 20% -40% of the length is 40-50 ℃, the cooling temperature of the more than 40% -less than 65% of the length is 25-40 ℃, and the cooling temperature of the later 65% -100% of the length is 15-25 ℃ based on the dropping point of the crystalline material as a starting point.
The principle of the invention is as follows: according to the triglycidyl isocyanurate melting granulation production system and method, the low-volatility organic solvent (methanol) is distilled off through the melting kettle, after the low-volatility organic solvent is completely distilled off, the melted material in the melting kettle is transferred to the temporary storage kettle and is conveyed to the thin film evaporator through the pump, the effect of continuously removing the high-boiling point solvent (epichlorohydrin) under the short residence time is formed in the thin film evaporator, the solvent residue in particles is reduced, and the problem that a large amount of melted materials are easy to carbonize under the long-time high temperature, so that the safety risk is caused is avoided. And then conveying the obtained transparent melt material to a crystallizer, wherein the temperature of a jacket of the crystallizer is controlled through the pushing speed of a third melt pump and the cooling water inlet amount, so that the control of the cooling rate is realized, the cooling rate is too fast, the material is easy to solidify in the crystallizer quickly, the material is not easy to operate and control, the cooling rate is too slow, the seed crystal generating speed of the material is very slow, the product is easy to be sticky after long-time heat preservation, therefore, the optimal cooling rate is controlled, TGIC in the transparent melt is gradually generated with seed crystals and controlled at an optimal point, the seed crystals are uniformly distributed, and the rapid granulation can be realized subsequently. Through a large amount of test data, when the light transmittance of the material reaches 15-35%, the material is still in a molten state with good fluidity, and the product forming effect is optimal. At this time, the crystallization material passes through the distributing device again, controls crystallization material discharge pressure, forms even liquid, evenly drops on the steel band granulator to even granulation. In addition, in the process of granulating triglycidyl isocyanurate, the dripping crystalline material is cooled by adopting zonal gradient cooling for the first time, so that the solidification time is shortened, the adhesion between a product and a steel belt granulator is reduced, the production efficiency is improved, and the product quality is improved.
Compared with the prior art, the invention has the beneficial effects that:
the triglycidyl isocyanurate melt granulation production system and the production method have the advantages of high production efficiency, good continuity and good safety, and the prepared TGIC particles are free of powder, stable and uniform in quality and high in reliability.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are needed in the embodiments 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 other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a schematic diagram of the system for producing triglycidyl isocyanurate by melt granulation according to the present invention;
in the figure, 1, a melting kettle, 2, a first melt pump, 3, a temporary storage kettle, 4, a second melt pump, 5, a thin film evaporator, 6, a third melt pump, 7, a crystallizer, 8, a distributor, 9, a fourth melt pump, 10, a digital remote transmission pressure gauge, 11, a steel belt granulator, 12, a first condenser, 13, a first collecting tank, 14, a second condenser, 15 and a second collecting tank.
Detailed Description
For a further understanding of the present invention, preferred embodiments of the invention are described below, but it is to be understood that these descriptions are merely intended to illustrate further features and advantages of the invention, and are not limiting of the claims of the invention.
As shown in figure 1, the triglycidyl isocyanurate melting granulation production system comprises a melting kettle 1, a temporary storage kettle 3, a thin film evaporator 5, a crystallizer 7, a distributing device 8 and a steel belt granulator 11; wherein, the discharge gate of melting kettle 1 and the feed inlet of keeping in cauldron 3 pass through first pipeline intercommunication, the discharge gate of keeping in cauldron 3 and the feed inlet of thin film evaporator 5 pass through the second pipeline intercommunication, the discharge gate of thin film evaporator 5 and the feed inlet of third melt pump 6 pass through the third pipeline intercommunication, the discharge gate of third melt pump 6 and the feed inlet of crystallizer 7 pass through the fourth pipeline intercommunication, the discharge gate of crystallizer 7 and the feed inlet of third melt pump 6 pass through the fifth pipeline intercommunication, and the discharge gate of crystallizer 7 and the feed inlet of distributing device 8 pass through the sixth pipeline intercommunication, steel band granulator 11 sets up in the below of the discharge gate of distributing device 8.
In the above technical solution, it is preferable that the first pipe is provided with the first melt pump 2, the second pipe is provided with the second melt pump 4, and the sixth pipe is provided with the fourth melt pump 9.
In the above technical solution, valves are preferably disposed on the first pipeline, the second pipeline, the third pipeline and the sixth pipeline, and the valves are preferably electromagnetic valves.
In the above technical solution, the sixth pipeline is preferably provided with a digital remote pressure gauge 10.
In the above technical solution, the production system preferably further includes a first condenser 12 and a first collecting tank 13, one end of the first condenser 12 is communicated with the melting kettle 1, the other end is communicated with the first collecting tank 13, and the first condenser 12 can condense methanol volatilized in the melting kettle 1 and store the methanol in the first collecting tank 13. The communication is usually carried out through a pipeline, and a valve is preferably arranged on the pipeline.
In the above technical solution, the production system preferably further includes a second condenser 14 and a second collecting tank 15, one end of the second condenser 14 is communicated with the thin film evaporator 5, the other end is communicated with the second collecting tank 15, and the second condenser 14 can condense epichlorohydrin volatilized in the thin film evaporator 5 and store the epichlorohydrin in the second collecting tank 15. The communication is usually through a pipeline, preferably a valve, preferably a solenoid valve, is arranged on the pipeline.
The invention relates to a method for producing triglycidyl isocyanurate by melting granulation, which comprises the following steps:
step one, preparation of TGIC
Adding wet triglycidyl isocyanurate powder containing methanol into a melting kettle 1;
step two, melt distillation
After the wet powder of triglycidyl isocyanurate containing methanol is kept at 65-90 ℃ for 60-90 min (the common realization mode is that hot water is introduced into an interlayer of a melting kettle 1 for heating, such as water at 95-98 ℃ for 40-60 min), methanol is distilled off, and the obtained molten material is conveyed to a temporary storage kettle 3;
step three, reduced pressure distillation
Preheating a thin film evaporator 5 to 105-130 ℃ and controlling the pressure to be minus 0.095-minus 0.1Mpa, continuously conveying the molten materials in a temporary storage kettle 3 to the thin film evaporator 5, and removing epichlorohydrin under reduced pressure to obtain transparent melt materials;
step four, melting crystallization
Conveying the transparent melt material to a crystallizer 7 through a third melt pump 6, preserving heat for 20-30 min at 95-105 ℃, simultaneously, pushing the transparent melt material in the crystallizer 7 by the third melt pump 6 to self-circulate, cooling to 80-95 ℃ at a cooling rate of 0.3-0.5 ℃/min, and controlling the light transmittance to 15-35%, thus obtaining the crystalline material;
step five, granulating
And (3) conveying the crystallized material to a distributing device 8, controlling the pressure of the crystallized material to be 0.15-0.45 MPa, uniformly dripping the crystallized material onto a steel belt granulator 11, and cooling and forming to obtain triglycidyl isocyanurate particles.
In the first step, the wet powder of triglycidyl isocyanurate containing methanol is obtained by the following steps: adding cyanuric acid, epoxy chloropropane and catalyst benzyl triethyl ammonium chloride into a reaction vessel according to the mass ratio of 1:10-15:0.02-0.06, heating to 100-110 ℃ under normal pressure to carry out synthesis reaction, adding caustic soda flakes according to the mass ratio of cyanuric acid to caustic soda flakes according to the mass ratio of 1:1-1.3, carrying out cyclization reaction at 15-25 ℃, filtering the obtained cyclization reaction product, layering, distilling a lower organic phase to recover epoxy chloropropane, crystallizing distilled materials with methanol, centrifuging, and adding the obtained methanol-containing triglycidyl isocyanurate wet powder into a melting kettle 1.
In the second step, the temperature is kept for 60-90 min at 70-80 ℃. The distilled methanol is preferably condensed by the first condenser 12 to the first collection tank 13 for collection. Preferably, the second step is carried out under stirring at a speed of 40 to 60rpm. In the third step, the preheating temperature is preferably 110 to 120 ℃. In step three, the epichlorohydrin removed, preferably under reduced pressure, is condensed by a second condenser 14 to a second collection tank 15 for collection. According to the invention, the low-volatility organic solvent (methanol) is distilled off through the melting kettle 1, after the low-volatility organic solvent is completely distilled off, the molten material in the melting kettle 1 is transferred to the temporary storage kettle 3 and is conveyed to the thin film evaporator 5 through the second melt pump 4, so that the effect of continuously removing the high-boiling point solvent (epichlorohydrin) under the short residence time in the thin film evaporator 5 is formed, the solvent residue is reduced, and the safety risk caused by that a large amount of molten material is easy to carbonize under the high temperature and long time is avoided.
In the fourth step, the heating temperature is preferably 95-100 ℃, the cooling temperature is 83-90 ℃, and the light transmittance is controlled to be 20-30%. Preferably, the speed of the self-circulation of the transparent melt material in the third melt pump 6 pushing the crystallizer 7 is 30-60L/min. Preferably, the crystallizer 7 is supplied with circulating cooling water, and the supply amount of the cooling water is controlled by a valve, preferably an electromagnetic valve. In the fourth step, the transparent melt is conveyed to a crystallizer 7, in the crystallizer 7, the driving force generated by the continuous external circulation of a third melt pump 6 is combined with cooling water to control the cooling rate, so that TGIC in the transparent melt material gradually generates seed crystals and is controlled at an optimal point, the seed crystals are uniformly distributed, the rapid granulation can be realized subsequently, in addition, when the light transmittance of the material reaches 15-35%, the material is still in a molten state with good fluidity, at the moment, the crystallized material passes through a distributor 8 to form uniform liquid, and the uniform liquid is uniformly dropped onto a steel belt granulator 11 and is uniformly granulated. If the seed crystal material is produced too little, the light transmittance is low, the solidification time of the transparent melt material is long, the transparent melt material is sticky, the seed crystal production amount is too large, the fluidity of the transparent melt material is poor, the wall is easy to form, and the problems of blocking and safety are caused.
In the fifth step, the crystallized material is conveyed to the distributor 8 by the fourth melt pump 9, the rotation displacement of the fourth melt pump 9 is 30-45L/min, and the crystallized material is uniformly dropped onto the steel belt granulator 11 after passing through the distributor 8. The temperature of the steel belt granulator 11 is gradually reduced along the moving direction of the crystallized materials, and the temperature range is 15-50 ℃. Specifically, the cooling temperature of the front 0% -less than 20% of the length of the granulating section of the steel belt granulator is 50-80 ℃, the cooling temperature of the 20% -40% of the length is 40-50 ℃, the cooling temperature of the greater than 40% -less than 65% of the length is 25-40 ℃, and the cooling temperature of the rear 65% -100% of the length is 15-25 ℃ by taking the dropping point of the crystalline material as a starting point. Too high or too low a temperature in the front zone (front 20-40%) can result in long TGIC product particle formation times and stickiness of the product. The temperature of the rear area (rear 65% -100%) is too high, the product is sticky, the temperature is too low, and energy waste is caused.
The terms used in the present invention generally have meanings commonly understood by those of ordinary skill in the art unless otherwise indicated. In order to enable those skilled in the art to better understand the technical solutions of the present invention, the present invention will be described in further detail with reference to examples.
In the following examples, various processes and methods, which are not described in detail, are conventional methods well known in the art. Materials, reagents, devices, instruments, equipment and the like used in the examples described below are commercially available unless otherwise specified.
The invention is further illustrated below with reference to examples.
Example 1
Adding 100 parts of cyanuric acid, 1200 parts of epoxy chloropropane and 3 parts of benzyl triethyl ammonium chloride catalyst into a reaction vessel, heating to 100-110 ℃ under normal pressure for synthesis reaction, adding 105 parts of caustic soda flakes for cyclization reaction at 25 ℃, filtering the obtained cyclization reaction product, layering, distilling a lower organic phase to recover epoxy chloropropane, crystallizing the distilled material with methanol, centrifuging to obtain triglycidyl isocyanurate wet powder containing methanol, and adding the triglycidyl isocyanurate wet powder into a melting kettle 1;
step two, after the wet powder of triglycidyl isocyanurate containing methanol is kept at 80 ℃ for 60min, the methanol is distilled off and recovered to a first collecting tank 13, and the obtained molten material is conveyed to a temporary storage kettle 3;
preheating the thin film evaporator 5 to 110 ℃, controlling the pressure to be-0.095 Mpa, continuously conveying the molten materials in the temporary storage kettle 3 to the thin film evaporator 5, removing epichlorohydrin under reduced pressure, and recycling the epichlorohydrin to the second collecting tank 15 to obtain transparent melt materials;
step four, conveying the transparent melt material to a crystallizer 7 through a third melt pump 6, preserving heat for 20min at 98 ℃, simultaneously, pushing the transparent melt material in the crystallizer 7 by the third melt pump 6 to self-circulate, wherein the self-circulation speed is 30L/min, cooling to 85 ℃ at a cooling rate of 0.4 ℃/min, and controlling the light transmittance to be 25%, so as to obtain a crystallized material;
step five, conveying the crystallized materials to a distributing device 8, controlling the pressure of the crystallized materials to be 0.45MPa, controlling the rotation displacement of a fourth melt pump 9 to be 30L/min, uniformly dripping the crystallized materials onto a steel belt granulator 11, cooling and shaping, wherein the cooling temperature of the front 0-20% of the granulating interval is 75 ℃, the cooling temperature of the 20-40% of the granulating interval is 50 ℃, the cooling temperature of the length of the front 20-40% is 40 ℃, the cooling temperature of the length of the front 40-65% is 25 ℃, and the cooling temperature of the rear 65-100% is 25 ℃, so as to obtain triglycidyl isocyanurate particles (semicircular).
Example 2
Step one is the same as in example 1;
step two, after the wet powder of triglycidyl isocyanurate containing methanol is kept at 70 ℃ for 90min, the methanol is distilled off and recovered to a first collecting tank 13, and the obtained molten material is conveyed to a temporary storage kettle 3;
preheating the thin film evaporator 5 to 115 ℃ and controlling the pressure to be-0.1 Mpa, continuously conveying the molten materials in the temporary storage kettle 3 to the thin film evaporator 5, removing epoxy chloropropane under reduced pressure, and recycling the epoxy chloropropane to the second collecting tank 15 to obtain transparent molten materials;
step four, conveying the transparent melt material to a crystallizer 7 through a third melt pump 6, preserving heat for 30min at 95 ℃, simultaneously, pushing the transparent melt material in the crystallizer 7 by the third melt pump 6 to self-circulate, wherein the self-circulation speed is 40L/min, cooling to 83 ℃ at a cooling rate of 0.5 ℃/min, and controlling the light transmittance to be 20%, so as to obtain a crystalline material;
step five, conveying the crystallized materials to a distributing device 8, controlling the pressure of the crystallized materials to be 0.3MPa, controlling the rotation displacement of a fourth melt pump 9 to be 40L/min, uniformly dripping the crystallized materials onto a steel belt granulator 11, cooling and shaping, wherein the cooling temperature of the front 0% -20% of the granulating interval is 65 ℃, the cooling temperature of the 20% -40% of the granulating interval is 45 ℃, the cooling temperature of the length of the product is more than 40% -40% and less than 65% is 35 ℃, and the cooling temperature of the product is 20 ℃ of the product after 65% -100% of the product is semicircular, so that triglycidyl isocyanurate particles are obtained.
Example 3
Step one is the same as in example 1;
step two, after the wet powder of triglycidyl isocyanurate containing methanol is kept at 75 ℃ for 80min, the methanol is distilled off and recovered to a first collecting tank 13, and the obtained molten material is conveyed to a temporary storage kettle 3;
preheating the thin film evaporator 5 to 120 ℃ and controlling the pressure to be-0.1 Mpa, continuously conveying the molten materials in the temporary storage kettle 3 to the thin film evaporator 5, removing epoxy chloropropane under reduced pressure, and recycling the epoxy chloropropane to the second collecting tank 15 to obtain transparent molten materials;
step four, conveying the transparent melt material to a crystallizer 7 through a third melt pump 6, preserving heat for 30min at 100 ℃, simultaneously, pushing the transparent melt material in the crystallizer 7 by the third melt pump 6 to self-circulate, wherein the self-circulation speed is 50L/min, cooling to 90 ℃ at a cooling rate of 0.3 ℃/min, and controlling the light transmittance to be 30%, so as to obtain a crystalline material;
step five, conveying the crystallized materials to a distributing device 8, controlling the pressure of the crystallized materials to be 0.3MPa, controlling the rotation displacement of a fourth melt pump 9 to be 45L/min, uniformly dripping the crystallized materials onto a steel belt granulator 11, cooling and shaping, wherein the cooling temperature of the first 0% -20% of the granulating interval is 60 ℃, the cooling temperature of the second 20% -40% of the granulating interval is 40 ℃, the cooling temperature of the second 20% -40% of the granulating interval is 30 ℃, and the cooling temperature of the second 65% -100% of the granulating interval is 15 ℃, so that triglycidyl isocyanurate particles (semicircular) are obtained.
Comparative example 1
As in example 1, only the light transmittance was controlled at 50%.
Comparative example 2
As in example 1, the temperature of the cooling-only shaped steel strip was controlled at 20℃in each zone.
Comparative example 3
The same as in example 1, the cooling temperature of the cooling-only shaping steel belt was 75 ℃ for the first 0% to less than 20% of the length of the granulating section, 75 ℃ for the 20% to 40% of the length, 30 ℃ for the more than 40% to less than 65% of the length, and 20 ℃ for the later 65% to 100% of the length.
Comparative example 4
The same as in example 1, the cooling temperature of the cooling-only shaping steel belt was 75 ℃ for the first 0% to less than 20% of the length of the granulating section, 45 ℃ for the 20% to 40% of the length, 40 ℃ for the more than 40% to less than 65% of the length, and 40 ℃ for the later 65% to 100% of the length.
Comparative example 5
As in example 1, only the crystallizer was cooled to 85℃at a cooling rate of 0.1℃per minute.
Comparative example 6
Steps one to three are the same as in example 1;
and fourthly, uniformly mixing the transparent melt material with 2wt% of TGIC dry powder, conveying the mixture to a distributing device 8 to form uniform liquid, uniformly dripping the uniform liquid onto a steel belt granulator 11, and cooling to form, wherein the cooling temperature is 50 ℃ to obtain triglycidyl isocyanurate particles.
Comparative example 7
Step one is the same as in example 1;
and step two, stirring wet powder of triglycidyl isocyanurate containing methanol, keeping the temperature at 80 ℃ for 60min, continuously heating to 90 ℃, keeping the temperature for 120min, distilling and removing the organic solvent under normal pressure, recovering the organic solvent to a collecting tank, continuously removing the solvent under vacuum under the pressure of-0.07 Mpa, and finally uniformly placing the melted material on a belt type cooling conveyor, cooling and crushing to obtain triglycidyl isocyanurate particles. (refer to the specific embodiment of patent CN 101773806A)
Comparative example 8
Refer to example 2 of patent CN108299403 a.
Comparative example 9
Reference is made to comparative example 2 of patent CN114130303 a.
The TGIC particles obtained in examples 1 to 3 and comparative examples 1 to 9 were measured, and the process parameters in the production methods of examples 1 to 3 and comparative examples 1 to 9 were monitored, and the results are shown in table 1.
TABLE 1 Performance test and method monitoring results of TGIC particles obtained in examples 1 to 3 and comparative examples 1 to 9
As can be seen from Table 1, the TGIC melt granulation production method of examples 1-3 has the advantages of low epichlorohydrin content in the prepared TGIC particles, obviously better product storage stability than the products produced by the methods of comparative examples 1-9, high production efficiency and good operation environment.
It is apparent that the above embodiments are merely examples for clarity of illustration and are not limiting examples. Other variations or modifications of the above teachings will be apparent to those of ordinary skill in the art. It is not necessary here nor is it exhaustive of all embodiments. And obvious variations or modifications thereof are contemplated as falling within the scope of the present invention.

Claims (10)

1. The triglycidyl isocyanurate melting granulation production system is characterized by comprising a melting kettle (1), a temporary storage kettle (3), a thin film evaporator (5), a crystallizer (7), a distributing device (8) and a steel belt granulator (11);
the utility model provides a feed inlet of melting kettle (1) and temporary storage kettle (3) passes through first pipeline intercommunication, the feed inlet of temporary storage kettle (3) and thin film evaporator (5) passes through the second pipeline intercommunication, the feed inlet of thin film evaporator (5) and third melt pump (6) passes through the third pipeline intercommunication, the feed inlet of third melt pump (6) and crystallizer (7) passes through the fourth pipeline intercommunication, the feed inlet of crystallizer (7) and third melt pump (6) passes through the fifth pipeline intercommunication, and the feed inlet of crystallizer (7) and distributor (8) passes through the sixth pipeline intercommunication, steel band granulator (11) set up in the below of distributor (8) discharge gate.
2. The triglycidyl isocyanurate melting granulation production system as set forth in claim 1 wherein the first conduit is provided with a first melt pump (2), the second conduit is provided with a second melt pump (4), and the sixth conduit is provided with a fourth melt pump (9).
3. The triglycidyl isocyanurate melt granulation system as set forth in claim 1, wherein,
valves are arranged on the first pipeline, the second pipeline, the third pipeline and the sixth pipeline;
and a digital remote pressure gauge (10) is arranged on the sixth pipeline.
4. The triglycidyl isocyanurate melt granulation system as set forth in claim 1, wherein,
the production system further comprises a first condenser (12) and a first collecting tank (13), wherein one end of the first condenser (12) is communicated with the melting kettle (1), and the other end of the first condenser is communicated with the first collecting tank (13);
the production system further comprises a second condenser (14) and a second collecting tank (15), wherein one end of the second condenser (14) is communicated with the thin film evaporator (5), and the other end of the second condenser is communicated with the second collecting tank (15).
5. The production method of the triglycidyl isocyanurate by melting granulation is characterized by comprising the following steps of:
step one, adding wet triglycidyl isocyanurate powder containing methanol into a melting kettle (1);
step two, insulating the wet powder of triglycidyl isocyanurate containing methanol at 65-90 ℃ for 60-90 min, distilling to remove the methanol, and conveying the obtained molten material to a temporary storage kettle (3);
preheating a thin film evaporator (5) to 105-130 ℃ and controlling the pressure to be minus 0.095-minus 0.1Mpa, continuously conveying the molten materials in a temporary storage kettle (3) to the thin film evaporator (5), and removing epichlorohydrin under reduced pressure to obtain transparent melt materials;
step four, conveying the transparent melt material to a crystallizer (7) through a third melt pump (6), preserving heat for 20-30 min at 95-105 ℃, simultaneously pushing the transparent melt material in the crystallizer (7) by the third melt pump (6) to self-circulate, cooling to 80-95 ℃ at a cooling rate of 0.3-0.5 ℃/min, and controlling the light transmittance to 15-35%, so as to obtain a crystalline material;
step five, conveying the crystallized material to a distributing device (8), controlling the pressure of the crystallized material to be 0.15-0.45 MPa, uniformly dripping the crystallized material onto a steel belt granulator (11), and cooling and forming to obtain triglycidyl isocyanurate particles;
the temperature of the steel belt granulator (11) is gradually reduced along the moving direction of the crystallized materials, and the temperature interval is 15-80 ℃.
6. The method for producing triglycidyl isocyanurate by melt granulation as claimed in claim 5, wherein in the first step, the wet powder of triglycidyl isocyanurate containing methanol is obtained by: adding cyanuric acid, epoxy chloropropane and catalyst benzyl triethyl ammonium chloride into a reaction vessel according to the mass ratio of 1:10-15:0.02-0.06, heating to 100-110 ℃ under normal pressure to carry out synthesis reaction, adding caustic soda flakes according to the mass ratio of cyanuric acid to caustic soda flakes according to the mass ratio of 1:1-1.3, carrying out cyclization reaction at 15-25 ℃, filtering the obtained cyclization reaction product, layering, distilling a lower organic phase to recover epoxy chloropropane, crystallizing distilled materials with methanol, centrifuging, and adding the obtained methanol-containing triglycidyl isocyanurate wet powder into a melting kettle (1).
7. The method for producing triglycidyl isocyanurate by melt granulation as claimed in claim 5, wherein in the second step, methanol is distilled off and condensed by a first condenser (12) to a first collecting tank (13) for collection;
in the third step, the epoxy chloropropane removed under reduced pressure is condensed to a second collecting tank (15) through a second condenser (14) for collection.
8. The method for producing triglycidyl isocyanurate by melt granulation according to claim 5, wherein in the fourth step, the speed of self-circulation of the transparent melt material in the pushing crystallizer (7) of the third melt pump (6) is 30-60L/min;
circulating cooling water is introduced into the crystallizer (7), and the introduced amount of the cooling water is controlled through a valve;
the light transmittance is controlled to be 20-30%.
9. The method for producing triglycidyl isocyanurate by melt granulation according to claim 5, wherein in the fifth step, the crystallization material is conveyed to the distributor (8) by a fourth melt pump (9), the rotation displacement of the fourth melt pump (9) is 30-45L/min, and the crystallization material is uniformly dropped onto the steel belt granulator (11).
10. The method according to claim 5, wherein in the fifth step, the cooling temperature of the first 0% to less than 20% of the length of the granulating section of the steel belt granulator (11) is 50 to 80 ℃, the cooling temperature of the 20% to 40% of the length is 40 to 50 ℃, the cooling temperature of the more than 40% to less than 65% of the length is 25 to 40 ℃, and the cooling temperature of the last 65% to 100% of the length is 15 to 25 ℃ based on the dropping point of the crystalline material.
CN202310772473.2A 2023-06-28 2023-06-28 Triglycidyl isocyanurate melting granulation production system and production method Pending CN116585978A (en)

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