CN114130303B - TGIC efficient devolatilization and melt extrusion granulation integrated processing method - Google Patents
TGIC efficient devolatilization and melt extrusion granulation integrated processing method Download PDFInfo
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- CN114130303B CN114130303B CN202111426681.4A CN202111426681A CN114130303B CN 114130303 B CN114130303 B CN 114130303B CN 202111426681 A CN202111426681 A CN 202111426681A CN 114130303 B CN114130303 B CN 114130303B
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- OUPZKGBUJRBPGC-UHFFFAOYSA-N 1,3,5-tris(oxiran-2-ylmethyl)-1,3,5-triazinane-2,4,6-trione Chemical compound O=C1N(CC2OC2)C(=O)N(CC2OC2)C(=O)N1CC1CO1 OUPZKGBUJRBPGC-UHFFFAOYSA-N 0.000 title claims abstract description 303
- 238000005469 granulation Methods 0.000 title claims abstract description 66
- 230000003179 granulation Effects 0.000 title claims abstract description 66
- 238000001125 extrusion Methods 0.000 title claims abstract description 55
- 238000003672 processing method Methods 0.000 title claims abstract description 40
- 239000000843 powder Substances 0.000 claims abstract description 107
- 229910000831 Steel Inorganic materials 0.000 claims abstract description 76
- 239000010959 steel Substances 0.000 claims abstract description 76
- 238000002425 crystallisation Methods 0.000 claims abstract description 42
- 230000008025 crystallization Effects 0.000 claims abstract description 42
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 33
- 239000007788 liquid Substances 0.000 claims abstract description 28
- 239000002245 particle Substances 0.000 claims abstract description 25
- 238000000034 method Methods 0.000 claims abstract description 19
- 230000009471 action Effects 0.000 claims abstract description 15
- 230000008569 process Effects 0.000 claims abstract description 13
- 238000002844 melting Methods 0.000 claims abstract description 12
- 230000008018 melting Effects 0.000 claims abstract description 12
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 11
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 11
- BRLQWZUYTZBJKN-UHFFFAOYSA-N Epichlorohydrin Chemical compound ClCC1CO1 BRLQWZUYTZBJKN-UHFFFAOYSA-N 0.000 claims description 30
- 239000000463 material Substances 0.000 claims description 28
- 238000009835 boiling Methods 0.000 claims description 17
- 150000001875 compounds Chemical class 0.000 claims description 17
- 238000013022 venting Methods 0.000 claims description 17
- 150000001298 alcohols Chemical class 0.000 claims description 15
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 14
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- 238000002347 injection Methods 0.000 claims description 12
- 239000007924 injection Substances 0.000 claims description 12
- 238000000465 moulding Methods 0.000 claims description 12
- 239000001569 carbon dioxide Substances 0.000 claims description 7
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 229910001868 water Inorganic materials 0.000 claims description 7
- JCXJVPUVTGWSNB-UHFFFAOYSA-N nitrogen dioxide Inorganic materials O=[N]=O JCXJVPUVTGWSNB-UHFFFAOYSA-N 0.000 claims description 2
- 239000000155 melt Substances 0.000 abstract description 46
- 238000004519 manufacturing process Methods 0.000 abstract description 17
- 238000005265 energy consumption Methods 0.000 abstract description 4
- 230000008901 benefit Effects 0.000 abstract description 3
- 238000010924 continuous production Methods 0.000 abstract 1
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 57
- 238000001816 cooling Methods 0.000 description 19
- 230000000052 comparative effect Effects 0.000 description 17
- 238000004821 distillation Methods 0.000 description 12
- 239000013078 crystal Substances 0.000 description 11
- 238000001035 drying Methods 0.000 description 9
- 239000007789 gas Substances 0.000 description 8
- 235000012054 meals Nutrition 0.000 description 8
- 238000002156 mixing Methods 0.000 description 8
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- 230000001276 controlling effect Effects 0.000 description 7
- 238000011084 recovery Methods 0.000 description 7
- 230000000694 effects Effects 0.000 description 6
- 238000010438 heat treatment Methods 0.000 description 5
- 230000007246 mechanism Effects 0.000 description 5
- 229910052757 nitrogen Inorganic materials 0.000 description 5
- 239000003960 organic solvent Substances 0.000 description 5
- 238000004806 packaging method and process Methods 0.000 description 5
- 230000005540 biological transmission Effects 0.000 description 4
- 238000012216 screening Methods 0.000 description 4
- 238000003860 storage Methods 0.000 description 4
- 238000007872 degassing Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 238000007599 discharging Methods 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 239000000428 dust Substances 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 238000006482 condensation reaction Methods 0.000 description 2
- 239000000498 cooling water Substances 0.000 description 2
- 238000004132 cross linking Methods 0.000 description 2
- 239000004744 fabric Substances 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 229920001225 polyester resin Polymers 0.000 description 2
- 239000004645 polyester resin Substances 0.000 description 2
- 238000009704 powder extrusion Methods 0.000 description 2
- 238000010298 pulverizing process Methods 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- 238000007493 shaping process Methods 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 238000009849 vacuum degassing Methods 0.000 description 2
- LRWZZZWJMFNZIK-UHFFFAOYSA-N 2-chloro-3-methyloxirane Chemical compound CC1OC1Cl LRWZZZWJMFNZIK-UHFFFAOYSA-N 0.000 description 1
- 239000004925 Acrylic resin Substances 0.000 description 1
- 229920000178 Acrylic resin Polymers 0.000 description 1
- 239000004593 Epoxy Substances 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 239000002826 coolant Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000006735 epoxidation reaction Methods 0.000 description 1
- 125000003700 epoxy group Chemical group 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- LNEPOXFFQSENCJ-UHFFFAOYSA-N haloperidol Chemical class C1CC(O)(C=2C=CC(Cl)=CC=2)CCN1CCCC(=O)C1=CC=C(F)C=C1 LNEPOXFFQSENCJ-UHFFFAOYSA-N 0.000 description 1
- 125000000623 heterocyclic group Chemical group 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 230000007794 irritation Effects 0.000 description 1
- ZFSLODLOARCGLH-UHFFFAOYSA-N isocyanuric acid Chemical compound OC1=NC(O)=NC(O)=N1 ZFSLODLOARCGLH-UHFFFAOYSA-N 0.000 description 1
- 238000010309 melting process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
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- 238000007873 sieving Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000011343 solid material Substances 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
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- 239000000126 substance Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 238000005292 vacuum distillation Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
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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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Extrusion Moulding Of Plastics Or The Like (AREA)
Abstract
The application discloses an integrated processing method for high-efficiency devolatilization and melt extrusion granulation of TGIC, which comprises the following steps: adding TGIC wet powder obtained after alcohol crystallization after synthesis into a double screw extruder; the TGIC is melted in a feeding melting section of the double-screw extruder; the melted TGIC is conveyed to a discharge port of the double-screw extruder under the action of the double-screw extruder, and devolatilization is carried out through vacuum ports on a plurality of exhaust areas on the double-screw extruder in the process; the melted TGIC after devolatilization is sent to a distributing machine head, the temperature of the distributing machine head is controlled between 80 ℃ and 100 ℃, the melt is evenly formed into spherical liquid through the distributing machine head, and the spherical liquid is dripped on a formed steel belt; the molded steel belt moves, and the TGIC is controlled to be solidified and molded on the molded steel belt through a temperature control system; the steel strip shaped TGIC particles were collected. The application has the advantages of high devolatilization efficiency, continuous production, high automation degree, safe and environment-friendly production process, low energy consumption, high productivity and the like.
Description
Technical Field
The application relates to the technical field of triglycidyl isocyanurate granulation, in particular to a TGIC efficient devolatilization and melt extrusion granulation integrated processing method.
Background
Triglycidyl isocyanurate (TGIC) is a crystalline heterocyclic epoxy compound, and three active epoxy groups can be subjected to crosslinking reaction with hydroxyl groups in polyester resin, so that the TGIC has excellent heat resistance, weather resistance, corrosion resistance, chemical resistance and mechanical properties, and can be widely applied to crosslinking curing agents of polyester resin or acrylic resin powder coatings, and can also be applied to the fields of structural materials, electrical insulating materials, printed circuit boards, modified epoxy resins, high-efficiency adhesives and the like.
The existing TGIC production process flow generally includes: (1) Condensation reaction of cyanuric acid and epoxy chloropropane under the action of a catalyst and a certain temperature; (2) Reducing the temperature, adding alkali, and performing epoxidation to produce triglycidyl isocyanurate; (3) washing and distilling under reduced pressure to recover excessive raw materials; and (4) adding alcohols, crystallizing and drying to obtain a finished product.
In the TGIC production process, in order to make the condensation reaction proceed smoothly, excessive epichlorohydrin is usually added, while the residual epichlorohydrin in TGIC product has a certain irritation to human skin and affects the curing efficiency of the product and the performance of the coating, so that after the reaction is finished, epichlorohydrin is removed and recovered by distillation, for example, JP-B-45-22751 uses a rotary evaporator to remove epichlorohydrin, US4395542 uses a multistage stripper to remove epichlorohydrin, CN102174040a uses reduced pressure distillation plus high vacuum thin film evaporator to remove epichlorohydrin. The traditional methods all adopt high vacuum and high temperature distillation processes to remove epichlorohydrin residues, the temperature in the distillation process is raised to 100-120 ℃, the distillation time is required to be 3-6 hours, a large amount of energy consumption is required, the production cost is increased, meanwhile, the product is easy to generate polymerization explosion danger under the high temperature condition, and the ideal effect is difficult to achieve. The control of the content of epichlorohydrin in the TGIC product below 100ppm, especially below 50ppm, is an urgent problem to be solved in the field of TGIC application for improving the safety and the usability of the TGIC product.
In addition, the TGIC solution is crystallized with alcohols such as methanol or ethanol to obtain powdered TGIC, which contains about 15-25% of methanol or ethanol, called wet powder. In the production flow, alcohols are removed by drying, and extrusion granulation is performed to facilitate packaging and transportation.
CN201420188579.4 and CN201410155719.2 disclose a triglycidyl isocyanurate dry powder extrusion granulation production line and production process, comprising a vibration dryer, a condenser connected with a gas outlet of the vibration dryer, a solvent recovery tank and a gas induced draft fan I connected with the condenser in sequence; a dry powder cyclone separator connected with a material outlet of the vibration dryer, a dry powder tank, a discharge hole of the dry powder tank, a material extruder, a tablet press, a belt cooling conveyor, a pulverizer, a screening machine and a packaging machine in sequence.
CN201110443507.0 heats TGIC by microwave heating to volatilize methanol in TGIC, and the whole oven is in negative pressure state during heating, and volatilized methanol gas enters into methanol recovery system. By utilizing the characteristic of selectively heating the product by microwaves, the TGIC can be uniformly heated in the drying process, the problems of material agglomeration, material melting and the like in the traditional process are solved, the volatilized methanol gas is cooled by a three-way condenser, and 95% of methanol is recycled.
CN201010108286.7 discloses a process for granulating triglycidyl isocyanurate by melting and its production line, using distillation still to make atmospheric distillation and vacuum distillation at different temp., after the organic solvent is completely distilled out, uniformly placing the material in the distillation still on a belt-type cooling conveyor, cooling, pulverizing and sieving. The production line comprises a distillation kettle, a condenser, an organic solvent recovery tank, a vacuum pump, a belt type cooling conveyor arranged below the distillation kettle, a pulverizer, a screening machine and a packing machine,
CN201310000785.8 discloses a novel drying and granulating device of TGIC, which comprises a feeding kettle and a feeding device arranged at the lower end of the feeding kettle, wherein the feeding device is connected with an extruder, a plurality of vacuum air outlets are arranged on the extruder, and the tail ends of the vacuum air outlets are connected with a melt pump and a die head. The drying device can improve the drying efficiency.
In the traditional TGIC wet powder extrusion granulation process, the drying equipment is complex, the drying process time is long, the physical extrusion granulation is carried out, the compactness of particles is uneven, the serious powder falling phenomenon still exists, and the packaging and the transportation of the TGIC are relatively more troublesome.
Disclosure of Invention
The application aims to solve the problems of low distillation efficiency, high residue, long alcohol drying process equipment, long time, falling of powder existing in physical extrusion granulation, low production efficiency and the like of epichlorohydrin in a TGIC product, and provides an integrated processing method for high-efficiency devolatilization and melt extrusion granulation of TGIC.
The application provides an integrated processing method for efficient devolatilization and melt extrusion granulation of TGIC, which adopts the following technical scheme:
an integrated processing method for high-efficiency devolatilization and melt extrusion granulation of TGIC comprises the following steps:
(1) Adding TGIC wet powder obtained after alcohol crystallization after synthesis into a double-screw extruder, wherein the screw rotating speed is 80-200rpm;
(2) The TGIC is melted in a feeding melting zone of the double-screw extruder;
(3) The melted TGIC is conveyed to a discharge port of the double-screw extruder under the action of the double-screw extruder, and devolatilization is carried out through vacuum ports on a plurality of exhaust areas on the double-screw extruder in the process;
(4) The melted TGIC after devolatilization in the step (3) is sent to a distributing machine head, the temperature of the distributing machine head is controlled between 80 ℃ and 100 ℃, the melt is evenly formed into spherical liquid through the distributing machine head, and the spherical liquid is dripped on a formed steel belt;
(5) The molded steel belt moves, and the TGIC is controlled to be solidified and molded on the molded steel belt through a temperature control system;
(6) The steel strip shaped TGIC particles were collected.
Through above-mentioned technical scheme, through carrying out the devolatilization with TGIC wet powder, send into the cloth aircraft nose in, the fuse-element evenly forms into globular liquid through the cloth aircraft nose to solidify the shaping through shaping steel band, it is efficient to have the devolatilization, and production serialization, degree of automation are high, production process safety environmental protection, low energy consumption, productivity advantage such as high.
Optionally, the specific step of performing the devolatilization in the step (3) is:
(31) Controlling the temperature of a first exhaust area on a cylinder of the double-screw extruder to be 100-120 ℃, and controlling the vacuum degree of a vacuum port of the area to be 200-1000Pa through a vacuum pump pipeline system;
(32) Setting the temperature of a second exhaust area 6 on the cylinder of the double-screw extruder between 95 ℃ and 120 ℃, and controlling the vacuum degree of a vacuum port of the area between 200Pa and 1000Pa through a vacuum pump pipeline system to realize the first devolatilization;
(33) Setting the temperature of a third exhaust area 7 on a barrel 2 of the double-screw extruder at 95-120 ℃ and controlling the vacuum degree of a vacuum port of the area to be 50-200Pa so as to realize the second devolatilization.
Through the technical scheme, the pressure of the vacuum ports of the first exhaust area and the second exhaust area is controlled to be between 200Pa and 1000Pa, so that methanol or ethanol with low boiling point can be removed, the pressure is lower than 200Pa, TGIC melt can be pumped into a pipeline, the pressure is higher than 1000Pa, and the alcohol removal is incomplete; a cooling medium can be led out of the vacuum pipeline, so that vaporized methanol or ethanol is condensed and discharged into the recovery tank, and the volatile components are recovered and recycled, so that the production is safe and environment-friendly; the pressure of the vacuum port of the third exhaust zone is maintained at 50-200Pa, and the epichlorohydrin with higher boiling point can be removed.
Optionally, the method further comprises the step of adding TGIC to the barrel of the twin screw extruder between the vacuum port of the first venting zone and the vacuum port of the second venting zone, the step being specifically: and feeding TGIC wet powder into the double-screw extruder barrel for a plurality of times in a first side feeding port between the vacuum port of the first air exhaust area and the vacuum port of the second air exhaust area, wherein the feeding quantity is 30-50% of the total yield.
According to the technical scheme, the TGIC wet powder is fed for multiple times from the first side feeding port, so that the yield can be further improved, and the problem of uneven melting plasticization caused by concentrated feeding is solved;
optionally, the screws at the inlet and the outlet of the first air exhaust area, the second air exhaust area and the third air exhaust area are provided with reverse thread sections.
By arranging the reverse thread sections on the screw rods at the inlet and the outlet of the exhaust area, melt sealing is realized, and relatively independent vacuum degassing chambers are formed, so that the devolatilization effect is improved.
Optionally, the method further comprises the step of injecting a low boiling point inert compound into the barrel of the double screw extruder, wherein the step is specifically as follows: and injecting low-boiling-point inert compounds into the cylinder of the double-screw extruder between the vacuum port of the second exhaust area and the vacuum port of the third exhaust area, wherein the low-boiling-point inert compounds are one or more of water, nitrogen and carbon dioxide, and the injection amount is 1-10wt% of the total feeding amount of TGIC wet powder.
Through the technical scheme, low-boiling-point inert compounds such as water, nitrogen, carbon dioxide and the like can be injected from the gas injection port, and the inert compounds have a carrying effect on micromolecular components to be removed from materials, so that the devolatilization effect of impurities in TGIC melt is improved.
Optionally, the injection amount of the low boiling point inert compound is 3-5wt% of the total feeding amount of the TGIC wet powder.
Through the technical scheme, the low-boiling-point inert compound with the dosage can ensure that small molecular components in the materials are carried and discharged, and simultaneously ensure that the low-boiling-point inert compound cannot be excessively remained in the materials.
Optionally, a step of adding TGIC dry powder is further included between feeding the devolatilized molten TGIC to the spreader head, specifically: the temperature of each section of the twin screw downstream of the last vacuum port is 80-95 ℃, TGIC dry powder with epichlorohydrin and alcohols removed is fed into the section, and the feeding amount of the TGIC dry powder is 0.5-5wt% of the feeding amount of TGIC wet powder.
According to the technical scheme, TGIC dry powder from which epichlorohydrin and alcohols have been removed is added into each section of the double screw downstream of the last vacuum port to serve as seed crystals for crystallization molding, so that the TGIC crystallization cooling time is accelerated, and the crystallization granulating efficiency is high.
Alternatively, when the devolatilized molten TGIC is fed to the spreader head, the molten TGIC is fed to the spreader head by a second-order extruder, and the TGIC dry powder is fed into the second-order extruder.
Through the technical scheme, the molten TGIC is sent to the material distributing machine head through the second-order extruder, and the TGIC dry powder is fed into the second-order extruder, so that the contact time of the TGIC dry powder and the molten TGIC can be increased, the TGIC dry powder and the molten TGIC are uniformly mixed under the action of the second-order extruder, and the crystallization granulating efficiency is further improved.
Optionally, the inlet pressure of the material distributing machine head is 0.1-2MPa.
Through the technical scheme, the inlet pressure of the distributing machine head is set to be 0.1-2MPa, so that TGIC melt can be ensured to be uniformly filled in the distributing machine head, granulation is ensured to be uniform and stable, and granulation is caused to be uneven due to too low or too high pressure.
Optionally, the temperature on the formed steel belt is controlled to be 40-60 ℃.
By the technical scheme, the temperature of the formed steel belt is controlled between 40 ℃ and 60 ℃, so that the crystallization rate of the TGIC molten drops can be obviously improved, and the TGIC molten drops are solidified and formed within 1-2 minutes.
In summary, the present application includes at least one of the following beneficial technical effects:
1. According to the TGIC efficient devolatilization and melt extrusion granulation integrated processing method, TGIC wet powder is devolatilized and then fed into a material distribution machine head, a melt is uniformly formed into spherical liquid through the material distribution machine head, and solidification forming is carried out through a formed steel belt, so that the TGIC efficient devolatilization and melt extrusion granulation integrated processing method has the advantages of high devolatilization efficiency, high production continuity, high automation degree, safe and environment-friendly production process, low energy consumption, high productivity and the like.
2. According to the application, through the plurality of exhaust areas and the vacuum ports on the extruder barrel, the pressure is regulated and controlled through the vacuum ports and the vacuum pump pipeline system, so that impurities in TGIC melt can be removed in batches, and the removal efficiency is high.
3. TGIC dry powder from which epichlorohydrin and alcohols have been removed is added into each section of the twin screw downstream of the last vacuum port to serve as seed crystal for crystallization molding, and the TGIC crystallization cooling time is accelerated, so that the efficiency of crystallization granulation is high.
Drawings
Fig. 1 is a schematic diagram of a device structure corresponding to embodiment 1 of the present application.
Fig. 2 is a schematic structural view of a screw according to example 1 of the present application.
Fig. 3 is a schematic view of a steel strip forming machine according to an embodiment of the present application.
Fig. 4 is a schematic diagram of a device structure corresponding to embodiment 2 of the present application.
Fig. 5 is a schematic diagram of a device structure corresponding to embodiment 3 of the present application.
Reference numerals illustrate:
1. a frame; 2. an extruder barrel; 3. a screw; 4. a charging melting zone; 5. a first exhaust zone; 6. a second exhaust zone; 7. a third exhaust zone; 8. a melt homogenizing delivery zone; 9. a main feeding port; 10. a discharge port; 11. a transmission mechanism; 12. an air injection port; 13. a vacuum pump piping system; 14. a first side feed port; 15. a second side feed port; 16. a melt pump; 17. a second-order extruder; 18. a material distributing machine head; 19. a steel belt forming machine; 20. a metering feeding system; 21. a side feeding system; 22. a second melt pump; 23. a rotary drip; 24. a scraper; 51. a first vacuum port; 61. a second vacuum port; 71. a third vacuum port; 1901. forming a steel belt; 1902. a temperature control system.
Detailed Description
The application is described in further detail below with reference to fig. 1-5.
Example 1:
the embodiment discloses a TGIC efficient devolatilization and melt extrusion granulation integrated processing method, which is realized based on a TGIC efficient devolatilization and melt extrusion granulation integrated machine.
Referring to fig. 1 and 2, the TGIC high-efficiency devolatilizing and melt extrusion granulating integrated machine disclosed in this embodiment comprises a frame 1, a barrel 2 of a double-screw extruder is arranged on the frame 1, a main feeding port 9 is arranged at one end of the barrel 2 of the double-screw extruder, and a discharging port 10 is arranged at the other end of the barrel 2 of the double-screw extruder, wherein the main feeding port 9 is connected with a metering feeding system 20 for feeding TGIC wet powder. A pair of screws 3 are arranged in a barrel 2 of the double-screw extruder, one end of each screw 3 is driven to rotate by a transmission mechanism 11, the screws 3 are driven to rotate in the barrel 2 of the double-screw extruder by the transmission mechanism 11, and in the embodiment, the transmission mechanism 11 drives the two screws 3 to rotate in the same direction or drives the two screws 3 to rotate in opposite directions.
Between the length-diameter ratio of 48D and 72D of the screw 3, 5 functional sections are arranged on the barrel 2 of the double-screw extruder between the main feeding port 9 and the discharging port 10, and are respectively as follows: a charging melting zone 4, a first exhaust zone 5, a second exhaust zone 6, a third exhaust zone 7, and a melt homogenizing delivery zone 8.
The length of the feeding melting zone 4 is 8-12D, the TGIC solid conveying and melting process is mainly completed, and a heating mechanism is arranged on the barrel 2 of the double-screw extruder at the feeding melting zone 4 and is used for heating and melting TGIC solid materials. The lengths of the first air exhaust area 5, the second air exhaust area 6 and the third air exhaust area 7 are respectively 4-6D, the double-screw extruder barrel 2 of each air exhaust area is provided with a vacuum port, namely, the first air exhaust area 5 is provided with a first vacuum port 51, the second air exhaust area 6 is provided with a second vacuum port 61, and the third air exhaust area 7 is provided with a third vacuum port 71. Each vacuum port is connected with a vacuum pump pipeline system 13, and the vacuum pump pipeline system 13 is connected with a cooling sleeve and a liquid recovery pipe to realize condensation recovery of volatile matters removal
In this embodiment, a pair of screws 3 disposed in the barrel 2 of the twin-screw extruder are in a meshed structure, and reverse thread sections are disposed at the inlet and outlet of the first air discharge area 5, the inlet and outlet of the second air discharge area 6, and the inlet and outlet of the third air discharge area 7 to realize melt sealing, thereby forming a relatively independent vacuum degassing chamber.
The barrel 2 of the double-screw extruder between the first exhaust area 5 and the second exhaust area 6 is provided with a first side feeding port 14, the first side feeding port 14 is connected with a metering feeding system 20, TGIC wet powder is fed into the first side feeding port 14 through the metering feeding system 20, multiple feeding of the TGIC wet powder is realized, and the problem of uneven melting plasticization caused by concentrated feeding is reduced.
The melt homogenizing and conveying area 8 is arranged between the discharge ports 10 of the third exhaust area 7, the length of the melt homogenizing and conveying area 8 is 18-24D, a second side feeding port 15 is arranged on the melt homogenizing and conveying area 8, and the second side feeding port 15 is connected with a side feeding system 21 for metering and feeding TGIC dry powder.
Referring to fig. 1 and 3, the discharge port 10 on the barrel 2 of the twin-screw extruder is connected with a distributing head 18 through a melt pump 16, the distributing head 18 is also connected with a rotary drip device 23, the distributing head 18 is used for uniformly forming TGIC melt into spherical liquid drops, the spherical liquid drops fall into one end of a formed steel belt 1901 on a steel belt forming machine 19 through the rotary drip device 23, a temperature control system 1902 is arranged on the steel belt forming machine 19, the temperature control of the formed steel belt 1901 can be realized, the temperature control of the formed steel belt 1901 is carried out through the temperature control system on the steel belt forming machine 19, and the TGIC of the spherical liquid drops is cooled and crystallized. Thus, granulation is achieved, and a scraper 24 is provided at the other end, i.e., the tail portion, of the shaped steel strip 1901, and the scraper 24 is abutted against the shaped steel strip 1901 for hanging down and collecting TGIC crystal grains shaped on the shaped steel strip 1901.
In this embodiment, the temperature control system 1902 cools the back surface of the shaped steel strip 1901 by passing cooling water.
In this embodiment, the motors of the twin screw extruder, the metering and feeding system 20, the melt pump 16 and the dispensing head 18 are all explosion-proof motors, so that the safety of the production process can be improved.
The TGIC high-efficiency devolatilization and melt extrusion granulation integrated processing method of the embodiment comprises the following steps:
(1) TGIC wet powder obtained after synthesis and alcohol crystallization is added into a double screw extruder through a metering and feeding system 20, and the rotating speed of a screw 3 is 80rpm.
(2) The TGIC wet meal was melted in the feed melt zone 4 of the twin screw extruder, the temperature of this zone being set to 100 ℃.
(3) The temperature of the first venting zone 5 on the barrel 2 of the twin-screw extruder was controlled to 100 c and the vacuum level of the first vacuum port 51 of this zone was controlled to 200Pa by the vacuum pump piping system 13.
(4) TGIC wet powder was metered in through the first side feed port 14 in an amount of 30% of the total yield.
(5) And the TGIC melt passes through a second exhaust area 6 on a cylinder 2 of the double-screw extruder to realize vacuum devolatilization, the temperature of the second exhaust area 6 is set at 95 ℃, the vacuum degree of a second vacuum port 61 of the area is controlled to be 200Pa, and low-boiling-point methanol or ethanol is removed.
(6) Vacuum devolatilization is realized in a third exhaust zone 7 of TGIC melt, the temperature of the third exhaust zone 7 is set at 95 ℃, the vacuum degree of a third vacuum port 71 of the zone is controlled at 50Pa, and in the process, the epichlorohydrin with a higher boiling point is removed.
(7) Reducing the temperature of a melt homogenizing and conveying area 8 between a third vacuum port 7 and a discharge port 10 to 80 ℃, adding TGIC dry powder from which epichlorohydrin and alcohols are removed through a second side feeding port 15 to serve as seed crystals for crystallization molding, accelerating TGIC crystallization cooling time, adding TGIC dry powder with the addition amount of 0.5 weight percent of the feeding amount of TGIC wet powder, uniformly mixing the TGIC dry powder and TGIC melt under the shearing action of a screw 3,
(8) The melt mixed with the TGIC dry powder is sent into a distributing machine head 18 through a melt pump 16 by a discharge hole 10, and the pressure of the melt pump 16 is controlled to be 0.1MPa, so that the inlet pressure of the distributing machine head is equal to 0.1MPa, the TGIC melt can be ensured to be uniformly filled in the distributing machine head, and granulation is ensured to be uniform and stable.
(9) The temperature of the distributing machine head 18 is controlled between 80 ℃, TGIC melt is uniformly formed into spherical liquid through the distributing machine head 18, and the spherical liquid is dripped on a formed steel belt 1901 of the steel belt forming machine 19;
(10) The formed steel strip 1901 moves at a certain speed, and the temperature of the part contacted with the TGIC is controlled to be 40 ℃ by a temperature control system 1902 of a steel strip forming machine 19, so that the crystallization rate of the TGIC molten drops is improved, and the TGIC molten drops are solidified and formed within 1-2 minutes.
(11) The steel strip shaped TGIC particles are collected by the tail scraper 24 of the shaped steel strip 1901 to obtain TGIC particles.
Example 2:
the TGIC high-efficiency devolatilization and melt extrusion granulation integrated processing method of this example was realized by using the same TGIC high-efficiency devolatilization and melt extrusion granulation integrated machine as in example 1.
The TGIC high-efficiency devolatilization and melt extrusion granulation integrated processing method of the embodiment comprises the following steps:
(1) TGIC wet powder obtained after synthesis and alcohol crystallization is added into a double screw extruder through a metering and feeding system 20, and the rotating speed of a screw 3 is 100rpm.
(2) The TGIC wet meal was melted in the feed melt zone 4 of the twin screw extruder, the temperature of this zone being set to 100 ℃.
(3) The temperature of the first venting zone 5 on the twin-screw extruder barrel 2 was controlled to 105 c and the vacuum level of the first vacuum port 51 of this zone was controlled to be between 500Pa by the vacuum pump piping system 13.
(4) TGIC wet powder was metered in through the first side feed port 14 in an amount of 35% of the total yield.
(5) The TGIC melt passes through a second exhaust zone 6 on a barrel 2 of the double-screw extruder to realize vacuum devolatilization, the temperature of the second exhaust zone 6 is set at 100 ℃, the vacuum degree of a second vacuum port 61 of the zone is controlled to be 500Pa, and low-boiling-point methanol or ethanol is removed.
(6) Vacuum devolatilization is realized in a third exhaust zone 7 of TGIC melt, the temperature of the third exhaust zone 7 is set at 100 ℃, the vacuum degree of a third vacuum port 71 of the zone is controlled at 80Pa, and in the process, the epichlorohydrin with a higher boiling point is removed.
(7) Reducing the temperature of a melt homogenizing and conveying area 8 between a third vacuum port 7 and a discharge port 10 to be 85 ℃, adding TGIC dry powder from which epichlorohydrin and alcohols are removed through a second side feeding port 15 to serve as seed crystals for crystallization molding, accelerating TGIC crystallization cooling time, adding TGIC dry powder with the addition amount of 1 weight percent of TGIC wet powder feeding amount, uniformly mixing the TGIC dry powder and TGIC melt under the shearing action of a screw 3,
(8) The melt mixed with the TGIC dry powder is sent into a distributing machine head 18 through a melt pump 16 by a discharge hole 10, and the pressure of the melt pump 16 is controlled to be 0.5MPa, so that the inlet pressure of the distributing machine head is equal to 0.5MPa, the TGIC melt can be ensured to be uniformly filled in the distributing machine head, and granulation is ensured to be uniform and stable.
(9) The temperature of the distributing machine head 18 is controlled at 90 ℃, TGIC melt is uniformly formed into spherical liquid through the distributing machine head 18, and the spherical liquid is dripped on a formed steel belt 1901 of the steel belt forming machine 19;
(10) The formed steel strip 1901 is moved at a certain speed, and the temperature of the part contacted with the TGIC is controlled between 45 ℃ by a temperature control system 1902 of a steel strip forming machine 19, so that the crystallization rate of the TGIC molten drops is improved, and the TGIC molten drops are solidified and formed within 1-2 minutes.
(11) The steel strip shaped TGIC particles are collected by the tail scraper 24 of the shaped steel strip 1901 to obtain TGIC particles.
Example 3:
referring to fig. 4, the TGIC high-efficiency devolatilization and melt extrusion granulation integrated processing method of the present embodiment is realized based on a TGIC high-efficiency devolatilization and melt extrusion granulation integrated machine. The TGIC-based efficient devolatilization and melt extrusion granulation all-in-one machine adopted in this embodiment is the same as the TGIC-based efficient devolatilization and melt extrusion granulation all-in-one machine adopted in embodiment 1 and embodiment 2, except that in this embodiment, an air injection port 12 is further provided on the barrel 2 of the twin-screw extruder, the air injection port 12 is provided between the second air exhaust area 6 and the third air exhaust area 7, and low boiling point inert compounds such as water, nitrogen, carbon dioxide and the like are injected from the air injection port 12, and then the inert compounds are volatilized again through the third vacuum port 71, so that the small molecular components to be removed in the materials have a carrying effect.
The TGIC high-efficiency devolatilization and melt extrusion granulation integrated processing method of the embodiment comprises the following steps:
(1) TGIC wet powder obtained after synthesis and alcohol crystallization is added into a double screw extruder through a metering and feeding system 20, and the rotating speed of a screw 3 is 120rpm.
(2) The TGIC wet meal was melted in the feed melt zone 4 of the twin screw extruder, the temperature of this zone being set at 105 ℃.
(3) The temperature of the first venting zone 5 on the barrel 2 of the twin-screw extruder was controlled to 110 c and the vacuum level of the first vacuum port 51 of this zone was controlled to 700Pa by the vacuum pump piping system 13.
(4) TGIC wet powder was metered in through the first side feed port 14 in an amount of 40% of the total yield.
(5) And the TGIC melt passes through a second exhaust area 6 on a cylinder 2 of the double-screw extruder to realize vacuum devolatilization, the temperature of the second exhaust area 6 is set at 110 ℃, the vacuum degree of a second vacuum port 61 of the area is controlled to be 700Pa, and low-boiling-point methanol or ethanol is removed.
(6) Inert compounds with low boiling point, such as water, nitrogen, carbon dioxide, etc., are injected through the gas injection port 12 between the second vacuum port 6 and the third vacuum port 7 in an amount of 3wt% of the total feeding amount of TGIC wet powder.
(7) Vacuum devolatilization is realized in a third exhaust zone 7 of TGIC melt, the temperature of the third exhaust zone 7 is set at 105 ℃, the vacuum degree of a third vacuum port 71 of the zone is controlled to be 150Pa, and in the process, the epichlorohydrin with a higher boiling point is removed.
(8) Reducing the temperature of a melt homogenizing and conveying area 8 between a third vacuum port 7 and a discharge port 10 to 90 ℃, adding TGIC dry powder from which epichlorohydrin and alcohols are removed through a second side feeding port 15 to serve as seed crystals for crystallization molding, accelerating TGIC crystallization cooling time, adding TGIC dry powder with the addition amount of 2 weight percent of TGIC wet powder feeding amount, uniformly mixing the TGIC dry powder and TGIC melt under the shearing action of a screw 3,
(9) The melt mixed with the TGIC dry powder is sent into a distributing machine head 18 through a melt pump 16 by a discharge hole 10, and the pressure of the melt pump 16 is controlled to be 1.5MPa, so that the inlet pressure of the distributing machine head is equal to 1.5MPa, the TGIC melt can be ensured to be uniformly filled in the distributing machine head, and granulation is ensured to be uniform and stable.
(10) The temperature of the distributing machine head 18 is controlled at 90 ℃, TGIC melt is uniformly formed into spherical liquid through the distributing machine head 18, and the spherical liquid is dripped on a formed steel belt 1901 of the steel belt forming machine 19;
(11) The formed steel strip 1901 moves at a certain speed, and the temperature of the part contacted with the TGIC is controlled to be 55 ℃ by a temperature control system 1902 of a steel strip forming machine 19, so that the crystallization rate of the TGIC molten drops is improved, and the TGIC molten drops are solidified and formed within 1-2 minutes.
(12) The steel strip shaped TGIC particles are collected by the tail scraper 24 of the shaped steel strip 1901 to obtain TGIC particles.
Example 4:
the TGIC high-efficiency devolatilization and melt extrusion granulation integrated processing method of this example was realized by using the same TGIC high-efficiency devolatilization and melt extrusion granulation integrated machine as in example 3.
The TGIC high-efficiency devolatilization and melt extrusion granulation integrated processing method of the embodiment comprises the following steps:
(1) TGIC wet powder obtained after synthesis and alcohol crystallization is added into a double screw extruder through a metering and feeding system 20, and the rotating speed of a screw 3 is 150rpm.
(2) The TGIC wet meal was melted in the feed melt zone 4 of the twin screw extruder, the temperature of this zone being set to 115 ℃.
(3) The temperature of the first degassing zone 5 on the barrel 2 of the twin-screw extruder was controlled to 115℃and the degree of vacuum of the first vacuum port 51 of this zone was controlled to 800Pa by the vacuum pump piping system 13.
(4) TGIC wet powder was metered in through the first side feed port 14 in an amount of 45% of the total yield.
(5) The TGIC melt passes through a second exhaust zone 6 on a barrel 2 of the double-screw extruder to realize vacuum devolatilization, the temperature of the second exhaust zone 6 is set at 115 ℃, the vacuum degree of a second vacuum port 61 of the zone is controlled to be 800Pa, and low-boiling-point methanol or ethanol is removed.
(6) Inert compounds with low boiling point, such as water, nitrogen, carbon dioxide, etc., are injected through the gas injection port 12 between the second vacuum port 6 and the third vacuum port 7 in an amount of 4.5wt% of the total feeding amount of TGIC wet powder.
(7) Vacuum devolatilization is realized in a third exhaust zone 7 of TGIC melt, the temperature of the third exhaust zone 7 is set at 105 ℃, the vacuum degree of a third vacuum port 71 of the zone is controlled at 180Pa, and in the process, the epichlorohydrin with a higher boiling point is removed.
(8) Reducing the temperature of a melt homogenizing and conveying area 8 between a third vacuum port 7 and a discharge port 10 to 90 ℃, adding TGIC dry powder from which epichlorohydrin and alcohols are removed through a second side feeding port 15 to serve as seed crystals for crystallization molding, accelerating TGIC crystallization cooling time, adding TGIC dry powder with the addition amount of 3 weight percent of TGIC wet powder feeding amount, uniformly mixing the TGIC dry powder and TGIC melt under the shearing action of a screw 3,
(9) The melt mixed with the TGIC dry powder is sent into a distributing machine head 18 through a melt pump 16 by a discharge hole 10, and the pressure of the melt pump 16 is controlled to be 1.8MPa, so that the inlet pressure of the distributing machine head is equal to 1.8MPa, the TGIC melt can be ensured to be uniformly filled in the distributing machine head, and granulation is ensured to be uniform and stable.
(10) Uniformly forming TGIC melt into spherical liquid through the material distributing machine head 18 by controlling the temperature of the material distributing machine head 18 to be 95 ℃, and dripping the spherical liquid on a formed steel belt 1901 of the steel belt forming machine 19;
(11) The formed steel strip 1901 moves at a certain speed, and the temperature of the part contacted with the TGIC is controlled to be 55 ℃ by a temperature control system 1902 of a steel strip forming machine 19, so that the crystallization rate of the TGIC molten drops is improved, and the TGIC molten drops are solidified and formed within 1-2 minutes.
(12) The steel strip shaped TGIC particles are collected by the tail scraper 24 of the shaped steel strip 1901 to obtain TGIC particles.
Example 5:
referring to fig. 5, the TGIC high-efficiency devolatilization and melt extrusion granulation integrated processing method of the present embodiment is realized based on a TGIC high-efficiency devolatilization and melt extrusion granulation integrated machine. The TGIC-based efficient devolatilization and melt extrusion granulation all-in-one machine adopted in this embodiment is the same as the TGIC-based efficient devolatilization and melt extrusion granulation all-in-one machine of embodiment 3 and embodiment 4, except that in this embodiment, the length-diameter ratio of the screws of the twin-screw extruder is 36-52D, the discharge port 10 on the barrel 2 of the twin-screw extruder is connected to a second-order extruder 17 through a melt pump 16, the inlet of the melt pump 16 is connected to the discharge port 10 of the twin-screw extruder, and the outlet of the melt pump 16 is connected to the inlet of the second-order extruder 17.
The second-order extruder 17 may be a single screw extruder or a twin screw extruder, and the second-order extruder 17 in this embodiment is a co-rotating twin screw extruder. In this embodiment, the second side feeding port 15 is not arranged between the discharge ports 10 of the third exhaust area 7, the second side feeding port 15 is arranged on the second-order extruder 17, and the second side feeding port 15 is connected with the side feeding system 21; the outlet of the second-order extruder 17 is connected to a distribution head 18 via a second melt pump 22.
The TGIC high-efficiency devolatilization and melt extrusion granulation integrated processing method of the embodiment comprises the following steps:
(1) TGIC wet powder obtained after synthesis and alcohol crystallization is added into a double screw extruder through a metering and feeding system 20, and the rotating speed of a screw 3 is 200rpm.
(2) The TGIC wet meal was melted in the feed melt zone 4 of the twin screw extruder, the temperature of this zone being set to 120 ℃.
(3) The temperature of the first venting zone 5 on the barrel 2 of the twin-screw extruder was controlled to 120 c and the vacuum level of the first vacuum port 51 of this zone was controlled to 1000Pa by the vacuum pump piping system 13.
(4) TGIC wet powder was metered in through the first side feed port 14 in an amount of 50% of the total yield.
(5) The TGIC melt passes through a second exhaust area 6 on a cylinder 2 of the double-screw extruder to realize vacuum devolatilization, the temperature of the second exhaust area 6 is set at 120 ℃, the vacuum degree of a second vacuum port 61 of the area is controlled to be 1000Pa, and the methanol or ethanol with low boiling point is removed.
(6) Inert compounds with low boiling point, such as water, nitrogen, carbon dioxide, etc., are injected through the gas injection port 12 between the second vacuum port 6 and the third vacuum port 7 in an amount of 5wt% of the total feeding amount of TGIC wet powder.
(7) The third venting zone 7 of TGIC melt realizes vacuum devolatilization, the temperature of the third venting zone 7 is set between 110 ℃, the vacuum degree of the third vacuum port 71 of the zone is controlled between 200Pa, and in the process, the epichlorohydrin with higher boiling point is removed.
(8) The temperature of the melt homogenizing delivery zone 8 between the third vacuum port 7 and the discharge port 10 was reduced to between 95 c and the molten TGIC in the discharge port 10 was fed by melt pump 16 to a second order extruder 17.
(9) Adding TGIC dry powder from which epichlorohydrin and alcohols have been removed through a second side feeding port 15 on a second-order extruder 17, as seed crystals for crystallization molding, accelerating the crystallization cooling time of TGIC, wherein the addition amount of the TGIC dry powder is 3wt% of the feeding amount of TGIC wet powder, and uniformly mixing the TGIC dry powder and TGIC melt under the double screw shearing action of the second-order extruder 17;
(10) Then the melt mixed with TGIC dry powder is pumped into the distributing machine head 18 through a second melt pump 22, and the pressure is controlled at 2MPa after the second melt pump 22;
(11) The temperature of the distributing machine head 18 is controlled at 100 ℃, the melt is uniformly formed into spherical liquid by the distributing machine head 18 and is dripped on a formed steel belt 1901 of the steel belt forming machine 19;
(10) The strip 1901 is moved at a constant speed and the temperature of the portion in contact with the TGIC is controlled to 60 ℃ by the strip former 19 temperature control system 1902.
(11) The steel strip shaped TGIC particles are collected by the tail scraper 24 of the shaped steel strip 1901 to obtain TGIC particles.
Comparative example 1:
the TGIC high-efficiency devolatilization and melt extrusion granulation integrated processing method of this comparative example was realized by using the same TGIC high-efficiency devolatilization and melt extrusion granulation integrated machine as in example 1.
The TGIC high-efficiency devolatilization and melt extrusion granulation integrated processing method of the comparative example comprises the following steps:
(1) TGIC wet powder obtained after synthesis and alcohol crystallization is added into a double screw extruder through a metering and feeding system 20, and the rotating speed of a screw 3 is 80rpm.
(2) The TGIC wet meal was melted in the feed melt zone 4 of the twin screw extruder, the temperature of this zone being set to 100 ℃.
(3) The temperature of the first venting zone 5 on the barrel 2 of the twin-screw extruder was controlled to 90 c and the vacuum level of the first vacuum port 51 of this zone was controlled to 180Pa by the vacuum pump piping system 13.
(4) TGIC wet powder was metered in through the first side feed port 14 in an amount of 30% of the total yield.
(5) The TGIC melt passes through a second exhaust zone 6 on the barrel 2 of the double-screw extruder to realize vacuum devolatilization, the temperature of the second exhaust zone 6 is set at 90 ℃, and the vacuum degree of a second vacuum port 61 of the zone is controlled to be 180Pa.
(6) The vacuum devolatilization was achieved in the third venting zone 7 of the TGIC melt, the temperature of the third venting zone 7 was set at 90℃and the vacuum level of the third vacuum port 71 of this zone was controlled at 40Pa.
(7) Reducing the temperature of a melt homogenizing and conveying area 8 between a third vacuum port 7 and a discharge port 10 to 80 ℃, adding TGIC dry powder from which epichlorohydrin and alcohols are removed through a second side feeding port 15 to serve as seed crystals for crystallization molding, accelerating TGIC crystallization cooling time, adding TGIC dry powder with the addition amount of 0.5 weight percent of the feeding amount of TGIC wet powder, uniformly mixing the TGIC dry powder and TGIC melt under the shearing action of a screw 3,
(8) The melt mixed with the TGIC dry powder is sent into a distributing machine head 18 through a melt pump 16 by a discharge hole 10, and the pressure of the melt pump 16 is controlled to be 0.1MPa, so that the inlet pressure of the distributing machine head is equal to 0.1MPa, the TGIC melt can be ensured to be uniformly filled in the distributing machine head, and granulation is ensured to be uniform and stable.
(9) The temperature of the distributing machine head 18 is controlled between 80 ℃, TGIC melt is uniformly formed into spherical liquid through the distributing machine head 18, and the spherical liquid is dripped on a formed steel belt 1901 of the steel belt forming machine 19;
(10) The formed steel strip 1901 moves at a certain speed, and the temperature of the part contacted with the TGIC is controlled to be 40 ℃ by a temperature control system 1902 of a steel strip forming machine 19, so that the crystallization rate of the TGIC molten drops is improved, and the TGIC molten drops are solidified and formed within 1-2 minutes.
(11) The steel strip shaped TGIC particles are collected by the tail scraper 24 of the shaped steel strip 1901 to obtain TGIC particles.
Comparative example 2:
the TGIC high-efficiency devolatilization and melt extrusion granulation integrated processing method of this comparative example was realized by using the same TGIC high-efficiency devolatilization and melt extrusion granulation integrated machine as in example 1.
The TGIC high-efficiency devolatilization and melt extrusion granulation integrated processing method of the comparative example comprises the following steps:
(1) TGIC wet powder obtained after synthesis and alcohol crystallization is added into a double screw extruder through a metering and feeding system 20, and the rotating speed of a screw 3 is 80rpm.
(2) The TGIC wet meal was melted in the feed melt zone 4 of the twin screw extruder, the temperature of this zone being set to 100 ℃.
(3) The temperature of the first venting zone 5 on the barrel 2 of the twin-screw extruder was controlled at 125℃and the degree of vacuum of the first vacuum port 51 of this zone was controlled to 1100Pa by the vacuum pump piping system 13.
(4) TGIC wet powder was metered in through the first side feed port 14 in an amount of 30% of the total yield.
(5) The TGIC melt was subjected to vacuum devolatilization by passing through a second degassing zone 6 on the barrel 2 of the twin-screw extruder, the temperature of the second degassing zone 6 was set at 125℃and the degree of vacuum of the second vacuum port 61 of this zone was controlled at 1100Pa.
(6) The third venting zone 7 of the TGIC melt was subjected to vacuum devolatilization, the temperature of the third venting zone 7 was set at 120℃and the vacuum level of the third vacuum port 71 of this zone was controlled at 220Pa.
(7) Reducing the temperature of a melt homogenizing and conveying area 8 between a third vacuum port 7 and a discharge port 10 to 80 ℃, adding TGIC dry powder from which epichlorohydrin and alcohols are removed through a second side feeding port 15 to serve as seed crystals for crystallization molding, accelerating TGIC crystallization cooling time, adding TGIC dry powder with the addition amount of 0.5 weight percent of the feeding amount of TGIC wet powder, uniformly mixing the TGIC dry powder and TGIC melt under the shearing action of a screw 3,
(8) The melt mixed with the TGIC dry powder is sent into a distributing machine head 18 through a melt pump 16 by a discharge hole 10, and the pressure of the melt pump 16 is controlled to be 0.1MPa, so that the inlet pressure of the distributing machine head is equal to 0.1MPa, the TGIC melt can be ensured to be uniformly filled in the distributing machine head, and granulation is ensured to be uniform and stable.
(9) The temperature of the distributing machine head 18 is controlled between 80 ℃, TGIC melt is uniformly formed into spherical liquid through the distributing machine head 18, and the spherical liquid is dripped on a formed steel belt 1901 of the steel belt forming machine 19;
(10) The formed steel strip 1901 moves at a certain speed, and the temperature of the part contacted with the TGIC is controlled to be 40 ℃ by a temperature control system 1902 of a steel strip forming machine 19, so that the crystallization rate of the TGIC molten drops is improved, and the TGIC molten drops are solidified and formed within 1-2 minutes.
(11) The steel strip shaped TGIC particles are collected by the tail scraper 24 of the shaped steel strip 1901 to obtain TGIC particles.
Comparative example 3:
the TGIC high-efficiency devolatilization and melt extrusion granulation integrated processing method of this comparative example was realized by using the same TGIC high-efficiency devolatilization and melt extrusion granulation integrated machine as in example 1.
The TGIC high-efficiency devolatilization and melt extrusion granulation integrated processing method of the embodiment comprises the following steps:
(1) TGIC wet powder obtained after synthesis and alcohol crystallization is added into a double screw extruder through a metering and feeding system 20, and the rotating speed of a screw 3 is 80rpm.
(2) The TGIC wet meal was melted in the feed melt zone 4 of the twin screw extruder, the temperature of this zone being set to 100 ℃.
(3) The temperature of the first venting zone 5 on the barrel 2 of the twin-screw extruder was controlled to 100 c and the vacuum level of the first vacuum port 51 of this zone was controlled to 200Pa by the vacuum pump piping system 13.
(4) And the TGIC melt passes through a second exhaust area 6 on a cylinder 2 of the double-screw extruder to realize vacuum devolatilization, the temperature of the second exhaust area 6 is set at 95 ℃, the vacuum degree of a second vacuum port 61 of the area is controlled to be 200Pa, and low-boiling-point methanol or ethanol is removed.
(5) Vacuum devolatilization is realized in a third exhaust zone 7 of TGIC melt, the temperature of the third exhaust zone 7 is set at 95 ℃, the vacuum degree of a third vacuum port 71 of the zone is controlled at 50Pa, and in the process, the epichlorohydrin with a higher boiling point is removed.
(6) Reducing the temperature of a melt homogenizing and conveying area 8 between a third vacuum port 7 and a discharge port 10 to 80 ℃, adding TGIC dry powder from which epichlorohydrin and alcohols are removed through a second side feeding port 15 to serve as seed crystals for crystallization molding, accelerating TGIC crystallization cooling time, adding TGIC dry powder with the addition amount of 0.5 weight percent of the feeding amount of TGIC wet powder, uniformly mixing the TGIC dry powder and TGIC melt under the shearing action of a screw 3,
(7) The melt mixed with the TGIC dry powder is sent into a distributing machine head 18 through a melt pump 16 by a discharge hole 10, and the pressure of the melt pump 16 is controlled to be 0.1MPa, so that the inlet pressure of the distributing machine head is equal to 0.1MPa, the TGIC melt can be ensured to be uniformly filled in the distributing machine head, and granulation is ensured to be uniform and stable.
(8) The temperature of the distributing machine head 18 is controlled between 80 ℃, TGIC melt is uniformly formed into spherical liquid through the distributing machine head 18, and the spherical liquid is dripped on a formed steel belt 1901 of the steel belt forming machine 19;
(9) The formed steel strip 1901 moves at a certain speed, and the temperature of the part contacted with the TGIC is controlled to be 40 ℃ by a temperature control system 1902 of a steel strip forming machine 19, so that the crystallization rate of the TGIC molten drops is improved, and the TGIC molten drops are solidified and formed within 1-2 minutes.
(10) The steel strip shaped TGIC particles are collected by the tail scraper 24 of the shaped steel strip 1901 to obtain TGIC particles.
Comparative example 1:
CN201410155719.2 adopted in this comparative example discloses a process for producing triglycidyl isocyanurate dry powder by extrusion granulation, which comprises the following specific steps:
(1) Adding triglycidyl isocyanurate containing 25-30% of an organic solvent into the vibration dryer through a material inlet of the vibration dryer, starting the vibration dryer, introducing steam into a jacket of the vibration dryer, and introducing cooling water into a condenser;
(2) When the vibration dryer heats triglycidyl isocyanurate containing 25-30% of organic solvent to 70 ℃, a condensing vacuum pump is started, reduced pressure distillation is carried out under the vacuum degree of 0.1MPa, the materials are kept for 2 hours, so that the materials become dry powder materials with the moisture content less than 0.5%, and the volatile organic solvent in the vibration dryer is changed into liquid through the condenser and is recovered into a solvent recovery tank;
(3) Opening an emptying valve and a discharging bottom valve of the vibration dryer, simultaneously starting a draught fan, enabling coarse dry powder materials of triglycidyl isocyanurate with the particle size of more than 80 microns to fall into a dry powder storage tank through a coarse powder outlet of the cyclone separator under the action of gravity, enabling fine dry powder materials of triglycidyl isocyanurate with the particle size of less than 80 microns to be fed into a dust remover through a fine powder outlet of the cyclone separator under the action of the draught fan, and feeding into the dry powder storage tank after dust removal through a bag-type dust remover;
(4) Feeding triglycidyl isocyanurate dry powder materials in the dry powder storage tank in the step (3) into a double-screw extruder at a constant speed, controlling the extrusion temperature to be 85 ℃, carrying out melt extrusion through the double-screw extruder at a feeding speed of 20m/s, feeding the materials into a belt type cooling conveyor after tabletting by a tablet press, conveying the flaky materials on the belt type cooling conveyor while cooling, feeding the flaky materials into a pulverizer for pulverizing when cooling to room temperature, screening by a screening machine, feeding qualified products with the particle size of more than 2mm into a packaging machine for packaging and warehousing, and returning the products with the particle size of less than 2mm to the dry powder storage tank for re-melt extrusion granulation.
The TGIC particles obtained in the above examples, comparative examples and comparative examples were measured, while the production per unit time of TGIC prepared in the above examples, comparative examples and comparative examples was measured.
The volatile (methanol) and epichlorohydrin residual content in TGIC was tested by GB/T27807-2011 method.
TABLE 1
As can be seen from Table 1, the TGIC high-efficiency devolatilization and melt extrusion granulation integrated processing method of the present application is characterized by high devolatilization efficiency and high efficiency, and the content of epichlorohydrin and methanol of the processed product is significantly lower than that of the product produced by the method of the comparative example in combination with the detection results of examples 1-5 and comparative example 1.
As can be seen from the results of the test in examples 1-5 and comparative example 2, the TGIC processing method of the present application with high devolatilization efficiency and integrated melt extrusion granulation has the highest methanol removal rate by controlling the pressure of the vacuum ports of the first exhaust area and the second exhaust area between 200 Pa and 1000Pa, and the residual amount of methanol in the obtained product is the lowest.
The technical means disclosed by the scheme of the application is not limited to the technical means disclosed by the technical means, and also comprises the technical scheme formed by any combination of the technical features. It should be noted that modifications and adaptations to the application may occur to one skilled in the art without departing from the principles of the present application and are intended to be within the scope of the present application.
Claims (8)
1. The integrated processing method for high-efficiency devolatilization and melt extrusion granulation of TGIC is characterized by comprising the following steps:
(1) Adding TGIC wet powder obtained after alcohol crystallization after synthesis into a double-screw extruder, wherein the screw rotating speed is 80-200rpm;
(2) The TGIC is melted in a feeding melting zone (4) of the double-screw extruder;
(3) The melted TGIC is conveyed to a discharge port (10) of the double-screw extruder under the action of the double-screw extruder, and devolatilization is carried out in the process through vacuum ports on a plurality of exhaust areas on the double-screw extruder;
(4) The melted TGIC after devolatilization in the step (3) is sent to a distributing machine head (18), the temperature of the distributing machine head (18) is controlled between 80 ℃ and 100 ℃, the TGIC melt is uniformly formed into spherical liquid through the distributing machine head (18), and the spherical liquid is dripped on a formed steel belt (1901);
(5) Moving the molding steel belt (1901), and controlling the TGIC to be solidified and molded on the molding steel belt (1901) through a temperature control system (1902);
(6) Collecting TGIC particles formed by the steel belt;
the specific steps of devolatilization in the step (3) are as follows:
(31) Controlling the temperature of a first exhaust area (5) on a machine barrel (2) of the double-screw extruder to be 100-120 ℃, and controlling the vacuum degree of a vacuum port of the first exhaust area (5) to be 200-1000Pa through a vacuum pump pipeline system (13);
(32) Setting the temperature of a second exhaust area (6) on a machine barrel (2) of the double-screw extruder between 95 ℃ and 120 ℃, and controlling the vacuum degree of a vacuum port of the second exhaust area (6) between 200Pa and 1000Pa through a vacuum pump pipeline system (13) to realize the first devolatilization;
(33) Setting the temperature of a third exhaust area (7) on a machine barrel (2) of the double-screw extruder at 95-120 ℃, and controlling the vacuum degree of a vacuum port of the third exhaust area (7) to be 50-200Pa so as to realize the second devolatilization;
The step of adding TGIC dry powder is also included between the feeding of the devolatilized molten TGIC to the spreader head (18), and specifically comprises: the temperature of each section of the twin screw downstream of the last vacuum port is 80-95 ℃, TGIC dry powder with epichlorohydrin and alcohols removed is fed into the section, and the feeding amount of the TGIC dry powder is 0.5-5wt% of the feeding amount of TGIC wet powder.
2. The integrated processing method for high-efficiency devolatilization and melt extrusion granulation of TGIC according to claim 1, wherein the integrated processing method is characterized in that: the method further comprises the step of adding TGIC into the barrel (2) of the double-screw extruder between the vacuum port of the first exhaust zone (5) and the vacuum port of the second exhaust zone (6), wherein the step is specifically as follows: the twin screw extruder barrel (2) was fed multiple times of TGIC wet powder in a first side feed port (14) between the vacuum port of the first venting zone (5) and the vacuum port of the second venting zone (6), with a feed rate of 30% -50% of the total throughput.
3. The integrated processing method for high-efficiency devolatilization and melt extrusion granulation of TGIC according to claim 1, wherein the integrated processing method is characterized in that: the screw rods (3) at the inlet and the outlet of the first air exhaust area (5), the second air exhaust area (6) and the third air exhaust area (7) are provided with reverse thread sections.
4. The integrated processing method for high-efficiency devolatilization and melt extrusion granulation of TGIC according to claim 1, wherein the integrated processing method is characterized in that: further comprising the step of injecting into the barrel (2) of the twin-screw extruder a low boiling point inert compound, in particular: and injecting a low-boiling-point inert compound which is one or more of water, nitrogen and carbon dioxide into the barrel (2) of the double-screw extruder between the vacuum port of the second exhaust area (6) and the vacuum port of the third exhaust area (7), wherein the injection amount is 1-10wt% of the total feeding amount of the TGIC wet powder.
5. The integrated processing method for high-efficiency devolatilization and melt extrusion granulation of TGIC according to claim 4, wherein the integrated processing method is characterized in that: the injection amount of the low boiling point inert compound is 3-5wt% of the total feeding amount of the TGIC wet powder.
6. The integrated processing method for high-efficiency devolatilization and melt extrusion granulation of TGIC according to claim 1, wherein the integrated processing method is characterized in that: when the devolatilized molten TGIC is fed to the spreader head (18), the molten TGIC is fed to the spreader head (18) through a second-order extruder (17), and the dry TGIC powder is fed into the second-order extruder (17).
7. The integrated processing method of TGIC high-efficiency devolatilization and melt extrusion granulation according to any one of claims 1-6, characterized in that: the inlet pressure of the material distributing machine head (18) is 0.1-2MPa.
8. The integrated processing method of TGIC high-efficiency devolatilization and melt extrusion granulation according to any one of claims 1-6, characterized in that: the temperature of the formed steel belt (1901) is controlled between 40 ℃ and 60 ℃.
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