WO2022121480A1 - Ensemble de refroidissement entièrement dégradable, son procédé de préparation et son utilisation - Google Patents

Ensemble de refroidissement entièrement dégradable, son procédé de préparation et son utilisation Download PDF

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Publication number
WO2022121480A1
WO2022121480A1 PCT/CN2021/122583 CN2021122583W WO2022121480A1 WO 2022121480 A1 WO2022121480 A1 WO 2022121480A1 CN 2021122583 W CN2021122583 W CN 2021122583W WO 2022121480 A1 WO2022121480 A1 WO 2022121480A1
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WO
WIPO (PCT)
Prior art keywords
cooling
fully degradable
temperature
melt
filter rod
Prior art date
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PCT/CN2021/122583
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English (en)
Chinese (zh)
Inventor
杨俊鹏
杨光远
彭三文
邓少鹏
李世建
王昊
Original Assignee
湖北中烟工业有限责任公司
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Publication of WO2022121480A1 publication Critical patent/WO2022121480A1/fr

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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J3/00—Processes of treating or compounding macromolecular substances
    • C08J3/20—Compounding polymers with additives, e.g. colouring
    • C08J3/22—Compounding polymers with additives, e.g. colouring using masterbatch techniques
    • C08J3/226—Compounding polymers with additives, e.g. colouring using masterbatch techniques using a polymer as a carrier
    • A—HUMAN NECESSITIES
    • A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24D—CIGARS; CIGARETTES; TOBACCO SMOKE FILTERS; MOUTHPIECES FOR CIGARS OR CIGARETTES; MANUFACTURE OF TOBACCO SMOKE FILTERS OR MOUTHPIECES
    • A24D3/00—Tobacco smoke filters, e.g. filter-tips, filtering inserts; Filters specially adapted for simulated smoking devices; Mouthpieces for cigars or cigarettes
    • A24D3/02—Manufacture of tobacco smoke filters
    • A24D3/0229—Filter rod forming processes
    • A24D3/0237—Filter rod forming processes by extrusion
    • A—HUMAN NECESSITIES
    • A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24D—CIGARS; CIGARETTES; TOBACCO SMOKE FILTERS; MOUTHPIECES FOR CIGARS OR CIGARETTES; MANUFACTURE OF TOBACCO SMOKE FILTERS OR MOUTHPIECES
    • A24D3/00—Tobacco smoke filters, e.g. filter-tips, filtering inserts; Filters specially adapted for simulated smoking devices; Mouthpieces for cigars or cigarettes
    • A24D3/02—Manufacture of tobacco smoke filters
    • A24D3/0275—Manufacture of tobacco smoke filters for filters with special features
    • A24D3/0279—Manufacture of tobacco smoke filters for filters with special features with tubes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B9/00—Making granules
    • B29B9/02—Making granules by dividing preformed material
    • B29B9/06—Making granules by dividing preformed material in the form of filamentary material, e.g. combined with extrusion
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2423/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
    • C08J2423/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
    • C08J2423/04—Homopolymers or copolymers of ethene
    • C08J2423/06—Polyethene
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2423/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
    • C08J2423/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
    • C08J2423/10—Homopolymers or copolymers of propene
    • C08J2423/12—Polypropene
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2467/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2467/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
    • C08J2467/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2467/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
    • C08J2467/04—Polyesters derived from hydroxy carboxylic acids, e.g. lactones

Definitions

  • the invention belongs to the technical field of tobacco, and in particular relates to a fully degradable cooling firmware and a preparation method and application thereof.
  • the smoke in the filter rod is in an aerosol state (aerosol particles in the state of tiny droplets). Since the size and composition of aerosol particles are directly affected by the temperature of the smoke, the harmful components of the smoke and the sensory quality of the HNB cigarettes will also be affected by the temperature of the smoke. After the tobacco components in the heat-not-burn cigarette are heated by a heating device at about 250-350°C (degrees Celsius), nicotine and some aromatic substances will be fully released.
  • the purpose of the present invention is to aim at the deficiencies of the prior art, to provide a fully degradable cooling firmware and a preparation method and application thereof, which can reduce the temperature of the smoke at the inlet end of the heat-not-burn cigarette without affecting the suction resistance of the cooling filter rod. and filtration efficiency.
  • a fully degradable cooling firmware including a fully degradable cooling master batch for reducing the temperature of flue gas; the cooling master batch is made of a variety of fully degradable materials and solubilizers. .
  • the plurality of fully degradable materials include polylactic acid, polycaprolactone, thermoplastic polyester elastomer, copolymers of butylene adipate and butylene terephthalate, poly Various substances in butylene succinate, polypropylene, and polyethylene.
  • the polypropylene: the polybutylene succinate: the polycaprolactone 3:3:6.
  • the solubilizer includes one or more of PR023-7, ADR, 115C, isopropanol, maleic anhydride, epoxy compatibilizer, polyethylene glycol and polycaprolactone .
  • the mass fraction of the solubilizer in the cooling master batch is 0.3-1.5%.
  • the fully degradable cooling firmware includes a fully degradable cooling pipe for reducing flue gas; the interior of the cooling pipe is provided with an air flow that passes through both ends of the axial direction and is used for the flue gas to pass through. channel; the cooling pipe is made of the cooling master batch.
  • the airflow channel includes a full-through hollow cavity, a spoked hollow cavity or a non-through hollow cavity.
  • the preparation method of fully degradable cooling firmware includes the following steps: obtaining the multiple fully degradable materials and mixing, and adding the solubilizer during the mixing process to obtain raw materials for granulation; extruding and granulating In the process, the raw materials are extruded and pelletized to obtain the fully degradable cooling masterbatch.
  • the multiple fully degradable materials are dried; the drying temperature is 60-80 degrees Celsius; and the drying time is 2-4 hours.
  • the raw material is extruded and pelletized by an extrusion and pelletizing process
  • the process of obtaining the cooling masterbatch includes: determining an extruder, a first shaping device, a first cooling/ an air-drying device and a first shearing device; placing the raw material in the extruder, so that the raw material is melted, plasticized and extruded to form the cooling master batch parison;
  • the blank is placed in the first setting device for structure, shape and size setting;
  • the first cooling/air-drying device is used to cool and/or air-dry and solidify the shaped cooling masterbatch parison;
  • the first shearing device cuts the solidified cooling master batch parison to obtain the cooling master batch.
  • the first setting device includes a first vacuum cooling setting sleeve for setting the structure, shape and size of the cooling masterbatch parison;
  • the first cooling/air-drying device includes a an air-cooled conveyor belt for transferring the cooling masterbatch parison and cooling and solidifying it;
  • the first shearing device includes a pelletizer for dicing the cooling masterbatch parison.
  • a first pressure sensor is provided on the screw of the extruder and/or the extrusion die, and the first pressure sensor is connected to a first servo motor.
  • the raw material is extruded and granulated by an extrusion and granulation process
  • the process of obtaining the cooling masterbatch further includes: determining a first feeding device for quantitatively feeding the raw material placed in the extruder.
  • the cooling masterbatch is prepared into the cooling tube by an extrusion process.
  • the process of using the extrusion molding process to prepare the cooling masterbatch into the cooling pipe includes: determining an extruder, a second shaping device, a second cooling/air-drying device, a dislocation traction device and The second shearing device; placing the cooling masterbatch in the extruder, so that the cooling masterbatch is melted, plasticized and extruded to form the cooling tube parison; the cooling tube parison is Place in the second shaping device for structure, shape and size shaping; use the second cooling/air-drying device to cool and/or air-dry the shaped cooling tube parison; use the dislocation traction
  • the device displaces, twists and pulls the solidified cooling tube parison to form a cooling section product; uses the second shearing device to cut the cooling section product to obtain the cooling tube.
  • the inside of the extruder is provided with a material conveying part, a material melting part, a melt conveying part, a homogenizing conveying part, a heating and heat preservation part and an extrusion die head; It is used to transport the cooling master batch to the inside of the extruder; the material melting part is used to make the cooling master batch reach the melting temperature and gradually melt into a melt; the melt conveying part is used to The melt is stirred and mixed along the screw of the extruder and conveyed to the homogenizing conveying part; the homogenizing conveying part is used to continuously melt and stabilize the melt and convey it to the heating and heat preservation part; The heating and heat preservation part is used to stabilize the temperature of the melt; the extrusion die part is used to extrude the melt and form a tubular strand.
  • the material conveying part is provided with a first temperature control part for controlling the conveying temperature of the cooling masterbatch; the material melting part is provided with a second temperature control part for controlling the melting temperature of the cooling masterbatch a control part; the melt conveying part is provided with a third temperature control part for controlling the temperature of the melt being stirred, mixed and conveyed along the screw of the extruder; the homogenization conveying part is provided with a third temperature control part for controlling the temperature The melt continues to melt and stabilize and conveys the temperature of the fourth temperature control part; the heating and heat preservation part is provided with a fifth temperature control part for stabilizing the melt temperature; the extrusion die head is provided with a The melt is extruded and forms a sixth temperature control portion of the temperature of the tubular strand.
  • the first temperature control part is used to keep the conveying temperature of the cooling masterbatch at 110-140 degrees Celsius; the second temperature control part is used to make the cooling masterbatch melt at a temperature of 110-140 degrees Celsius. maintained at 140-180 degrees Celsius; the third temperature control part is used to keep the temperature at which the melt is stirred, mixed and transported along the screw of the extruder at 150-180 degrees Celsius; the fourth temperature control part The fifth temperature control part is used to keep the stable temperature of the melt at 150-180 degrees Celsius; the fifth temperature control part is used to keep the stable temperature of the melt at 140-165 degrees Celsius; the sixth The temperature control part is used to keep the temperature at which the melt is extruded and formed into the tubular strand at 130-150 degrees Celsius.
  • the second setting device includes a second vacuum cooling setting sleeve for setting the structure, shape and size of the cooling tube parison;
  • the second cooling/air-drying device includes a setting sleeve for holding a cooling tank for cooling the liquid and cooling and solidifying the cooling tube parison;
  • the dislocation traction device includes a dislocation twisting part for dislocation and twisting the solidified cooling tube parison and a dislocation twisting part for dislocation and twisting the The pulling part of the cloth tape reel of the filter rod forming machine for pulling the parison of the cooling tube;
  • the second shearing device includes the flying scissor head for cutting the product in the cooling section.
  • the cooling/air-drying device further includes a suction tape for further cooling and solidifying the cooling tube parison.
  • a second pressure sensor is provided on the screw of the extruder and/or the extrusion die head, and the second pressure sensor is connected to a second servo motor.
  • the process of using the extrusion molding process to prepare the cooling masterbatch into the cooling pipe further includes: determining a second feeding device for quantitatively placing the cooling masterbatch on the cooling pipe. inside the extruder.
  • Use of fully degradable cooling firmware in cooling filter rods for heat-not-burn cigarettes include: the use of the cooling masterbatch in the cooling filter rod; and/or the use of a cooling tube in the cooling filter rod use.
  • the cooling filter rod includes a plurality of first solid filter rods, and particle segments are arranged between adjacent first solid filter rod segments; the particle segments include a hollow tube body and a the cooling masterbatch in the hollow tube body; the first solid filter rod is used to block the cooling masterbatch; the first solid filter rod adopts the first polymer fiber and plasticizer or glue
  • the first polymer fiber comprises polylactic acid tow, polypropylene tow and/or cellulose diacetate tow.
  • the cooling filter rod comprises a hollow filter rod and/or a second solid filter rod, and is connected to one end and/or both ends of the second solid filter rod and/or the hollow filter rod the cooling tube;
  • the second solid filter rod is made of the second polymer fiber and plasticizer or adhesive;
  • the second polymer fiber includes polylactic acid tow, polypropylene tow and/or Cellulose diacetate tow;
  • the hollow filter rod is made of a third polymer fiber and a plasticizer or adhesive;
  • the third polymer fiber includes polylactic acid tow, polypropylene tow and/or two Cellulose acetate tow;
  • the hollow filter rod is provided with a hollow cavity body, and the hollow cavity body includes an axial through-type hollow cavity or an axial non-through type hollow cavity;
  • the hardness is more than 60% of the hardness of the solid filter rod of the same material and outer diameter.
  • the fully degradable cooling firmware of the present invention can effectively improve the heat absorption efficiency of the flue gas in the cooling section of the cooling filter rod, and the cooling effect is good, and simultaneously does not affect the suction resistance and the filtration efficiency of the cooling filter rod.
  • the fully degradable cooling firmware of the present invention has good thermal stability, good safety and good environmental protection.
  • the fully degradable cooling firmware of the present invention has low material consumption and good economy.
  • the fully degradable cooling firmware of the present invention includes a cooling master batch and/or a cooling tube, and has a simple structure and convenient use.
  • the cooling pipe of the present invention can increase the contact area between the flue gas and the airflow channel, and prolong the circulation and residence time of the flue gas in the airflow channel; thus, the contact collision effect between the flue gas and the material can be improved, and the cooling effect is remarkable.
  • the present invention is provided with a cooling tank and a suction ribbon, which can effectively cool and solidify the cooling tube parison, so that the spokes inside the cooling tube parison have a better cooling and shaping effect; at the same time, the cold air of the suction ribbon can also remove the cooling tube. The moisture on the blank is ready for the cutting of the cooling tube parison.
  • the present invention is provided with a dislocation traction device.
  • the dislocation traction device includes a dislocation twisted part and a filter rod forming machine tape reel traction part.
  • the dislocation twisted part can increase the contact area between the flue gas and the airflow channel, and improve the contact between the flue gas and the raw material.
  • the collision effect can further improve the cooling effect of the flue gas, and the traction part of the cloth tape reel of the filter rod forming machine can increase the stability of the traction.
  • the present invention is provided with a first vacuum cooling setting sleeve and a second vacuum cooling setting sleeve, which can quickly complete the structure, shape and size setting of the cooling master batch parison and the cooling tube parison.
  • the present invention is provided with a first pressure sensor and a second pressure sensor, which can ensure that the pressure of the raw material and the cooling masterbatch is controllable and adjustable during the melting process.
  • the present invention is provided with a flying scissor head. Since the flying scissors head and the product in the cooling section are in a synchronous operation state, the cut end face of the product in the cooling section can be kept flush, and the shearing effect is good.
  • Fig. 1 shows the structural representation of a specific embodiment of the cooling filter rod of the present invention
  • Figure 2 shows a schematic cross-sectional view of a specific embodiment of the cooling pipe of the present invention
  • Figure 3 shows a schematic cross-sectional view of a specific embodiment of the hollow filter rod of the present invention
  • FIG. 4 shows a schematic cross-sectional view of a specific embodiment of the second solid filter rod of the present invention
  • Fig. 5 shows the structural schematic diagram of the extruder, the second cooling/air drying device and the second shearing device of the present invention
  • Fig. 6 shows the thermogravimetric curve schematic diagram of PLA/PBAT blending series samples of the present invention
  • Figure 7 shows a schematic diagram of the tensile properties of the PLA/PBAT blend series of samples of the present invention
  • Figure 8 shows a DSC (differential scanning calorimetry) analysis chart of the PLA/PBAT blend series of samples of the present invention when scanned at 40 degrees Celsius/min.
  • 1-cooling pipe 11-air flow channel; 2-cooling filter rod; 3-extruder; 4-second cooling/air drying device; 5-second shearing device; 6-hollow filter rod; 7-th Two solid filter rods
  • the fully degradable cooling firmware of the present invention includes: a fully degradable cooling master batch for reducing the temperature of flue gas; the cooling master batch is made of various fully degradable materials and solubilizers.
  • the cooling masterbatch can be completely degraded and has good environmental protection; and can realize the cooling of the flue gas at the inlet end of the heat-not-burn cigarette without affecting the suction resistance and filtration efficiency of the cooling filter rod, and has good cooling effect and good stability.
  • the various fully degradable materials include PLA (polylactic acid), PCL (polycaprolactone), TPEE (thermoplastic polyester elastomer), PBAT (butylene adipate and terephthalate) Copolymers of butylene formate), PBS (polybutylene succinate), PP (polypropylene), and various substances in PE (polyethylene).
  • PLA polylactic acid
  • PCL polycaprolactone
  • TPEE thermoplastic polyester elastomer
  • PBAT butylene adipate and terephthalate
  • PBS polybutylene succinate
  • PP polypropylene
  • PE polypropylene
  • the solubilizer includes one or more of PR023-7, ADR, 115C, isopropanol, maleic anhydride, epoxy compatibilizer, polyethylene glycol and polycaprolactone;
  • the solubilizer can effectively improve the mixing effect of various fully degradable materials, and is convenient for obtaining raw materials for granulation.
  • the mass fraction of the solubilizer in the cooling masterbatch is 0.3-1.5%.
  • the fully degradable cooling firmware further includes a fully degradable cooling pipe 1 for reducing flue gas.
  • the inside of the cooling pipe 1 is provided with an airflow channel 11 penetrating both ends in the axial direction and used for the passage of flue gas.
  • the cooling tube 1 is made of cooling masterbatch.
  • the cooling pipe 1 can be completely degraded, and has good environmental protection; and can realize the cooling of the smoke at the inlet end of the heat-not-burn cigarette without affecting the suction resistance and filtration efficiency of the cooling filter rod 2, and has good cooling effect and stability. it is good.
  • the airflow channel 11 includes a full-through hollow cavity, a spoked hollow cavity or a non-through hollow cavity.
  • the air flow channel 11 is a spoke-type hollow cavity, which can increase the contact area between the flue gas and the air flow channel, prolong the circulation and residence time of the flue gas in the air flow channel, and thus can improve the efficiency of the flue gas and the flow rate. Contact collision effect of a fully degradable material.
  • the spoke-type hollow cavity includes a spiral spoke-type structure, which can not only improve the contact and collision effect between the smoke and various fully degradable materials, but also has good aesthetics.
  • the preparation method of the fully degradable cooling firmware of the present invention comprises the following steps:
  • Extrusion and granulation are used to extrude and granulate the raw materials used for granulation to obtain fully degradable cooling masterbatches.
  • drying a variety of fully degradable materials can effectively remove moisture and prevent hydrolysis and cracking of raw materials during subsequent heating and melting.
  • the drying temperature is 60-80 degrees Celsius.
  • the drying time is 2 to 4 hours.
  • using hot air to dry a variety of fully degradable materials is simple and efficient, and has a good drying effect.
  • the raw material is extruded and granulated by extrusion and granulation process, and the process of obtaining the cooling master batch includes:
  • the raw material is placed in the extruder, so that the raw material is melted, plasticized and extruded to form a cooling masterbatch parison;
  • the solidified cooling masterbatch parison is cut into pellets by using the first shearing device to obtain the cooling masterbatch.
  • the first setting device includes a first vacuum cooling setting sleeve for setting the structure, shape and size of the cooling masterbatch parison, which can quickly complete the structure and shape of the cooling masterbatch parison and sizing.
  • the temperature in the first vacuum cooling and shaping sleeve is 30-60 degrees Celsius, which can ensure the cooling and shaping effect of the cooling masterbatch parison, and avoid quenching shrinkage of the cooling masterbatch parison.
  • the first cooling/air-drying device includes an air-cooled conveyor belt for transferring the cooling masterbatch parison and cooling and solidifying it, which can effectively cool and solidify the cooling masterbatch parison, and has a simple structure and convenient use.
  • the cooled master batch parison is transported to the first shearing device through an air-cooled conveyor belt for dicing.
  • the air-cooled conveyor belt includes a conveyor belt for conveying the cooling master batch parison, and an air cooling part for cooling and solidifying the cooling master batch parison is provided on the conveyor belt.
  • the temperature of the air cooling part is 20 to 30 degrees Celsius.
  • the first shearing device includes a pelletizer for dicing the cooled masterbatch parison, which can stably cut the cooled masterbatch parison with good uniformity.
  • the cooling masterbatch is packaged by a first packaging machine.
  • the screw of the extruder and/or the extrusion die is provided with a first pressure sensor, and the first pressure sensor is connected to the first servo motor, which can ensure that the pressure of the raw material is controllable during the melting process Adjustable.
  • the raw materials are extruded and granulated using extrusion and granulation processes
  • the process of obtaining the cooling masterbatch includes further comprising: determining a first feeding device for quantitatively placing the raw materials in the extrusion In the machine, it can improve the stability of the extruded material.
  • an extrusion process is used to prepare the cooling masterbatch into a cooling tube 1 (as shown in Figures 1 and 2).
  • the process of preparing the cooling masterbatch into the cooling pipe 1 (as shown in Figure 1 and Figure 2 ) by an extrusion molding process includes:
  • the cooling masterbatch is placed in the extruder 3, so that the cooling masterbatch is melted, plasticized and extruded to form a cooling tube parison;
  • the cured cooling tube parison is dislocated, twisted and pulled by a dislocation traction device to form a cooling section product
  • the inside of the extruder 3 is provided with a material conveying part, a material melting part, a melt conveying part, a homogenizing conveying part, a heating and heat preservation part and an extrusion die head;
  • the material conveying part is used to convey the cooling masterbatch to the inside of the extruder 3;
  • the material melting part is used to make the cooling masterbatch reach the melting temperature and gradually melt into a melt
  • the melt conveying part is used for stirring and mixing the melt along the screw of the extruder 3 and conveying it to the homogenizing conveying part; wherein, the temperature of the melt conveying part is required to be close to the melting point of the raw material, which can ensure sufficient melting and plasticizing of the raw material. effect.
  • the homogenizing conveying part is used to continuously melt and stabilize the melt and convey it to the heating and heat preservation part;
  • the heating and heat preservation part is used to stabilize the temperature of the melt
  • the extrusion die head is used to extrude the melt and form a tubular strand.
  • the material conveying part is provided with a first temperature control part for controlling the conveying temperature of the cooling masterbatch, which can stably control the conveying temperature of the cooling masterbatch and has good reliability.
  • the material melting part is provided with a second temperature control part for controlling the melting temperature of the cooling masterbatch, which can stably control the melting temperature of the cooling masterbatch and has good reliability.
  • the melt conveying part is provided with a third temperature control part for controlling the mixing and conveying temperature of the melt along the screw of the extruder 3, which can stably control the mixing and conveying of the melt along the screw of the extruder 3 temperature and good reliability.
  • the homogenizing and conveying part is provided with a fourth temperature control part for controlling the continuous melting and stable temperature of the melt and the conveying temperature, which can stably control the temperature at which the melt continues to melt, stabilize and convey, and has good reliability.
  • the heating and heat preservation part is provided with a fifth temperature control part for stabilizing the temperature of the melt, so that the temperature of the melt can be stably controlled.
  • the extrusion die head is provided with a sixth temperature control part for controlling the temperature of extruding the melt and forming the tubular strand, which can stably control the temperature of extruding the melt and forming the tubular strand, and has good reliability.
  • the first temperature control part is used to keep the conveying temperature of the cooling masterbatch at 110-140 degrees Celsius.
  • the second temperature control part is used to keep the melting temperature of the cooling masterbatch at 140-180 degrees Celsius.
  • the third temperature control part is used to keep the temperature at which the melt is stirred, mixed and conveyed along the screw of the extruder 3 at 150-180 degrees Celsius.
  • the fourth temperature control part is used to keep the temperature at which the melt continues to be melted stably and transported at 150-180 degrees Celsius.
  • the fifth temperature control part is used to keep the stable temperature of the melt at 140-165 degrees Celsius.
  • the sixth temperature control part is used to keep the temperature at which the melt is extruded and formed into a tubular strand at 130-150 degrees Celsius, and can be adjusted according to the extrusion state of the material.
  • the second setting device includes a second vacuum cooling setting sleeve for setting the structure, shape and size of the cooling tube parison, which can quickly complete the structure, shape and size setting of the cooling tube parison.
  • the temperature of the second vacuum cooling and shaping sleeve is 30-60 degrees Celsius, which can ensure the cooling and shaping effect of the cooling tube parison, and avoid the rapid cooling and shrinkage of the cooling tube parison.
  • the length of the second vacuum cooling setting sleeve is 0.1 cm to 1 meter, which can prolong the setting time of the cooling tube parison, and the setting effect will be better, so that the structure, shape and size of the cooling firmware parison It is more stable, and at the same time, the substantial extension of the second vacuum cooling setting sleeve can effectively improve the production efficiency.
  • the second cooling/air-drying device 4 includes a cooling tank 41 for containing the cooling liquid and cooling and solidifying the cooling tube parison, which can achieve dimensional stability of the cooling tube parison.
  • the cooling liquid includes a first cooling liquid and a second cooling liquid.
  • the temperature of the first cooling liquid is 10-20 degrees Celsius, and the temperature of the second cooling liquid is 20-30 degrees Celsius.
  • the second cooling/air-drying device 4 further includes a suction tape for further cooling and solidifying the cooling tube parison, and the cooling tube parison can be further cooled and solidified by using the suction tape type cold air cooling method, The cooling and shaping effect of the spokes inside the cooling tube parison is better.
  • the cold air of the suction ribbon can also remove the moisture on the parison of the cooling tube, so as to prepare for the cutting of the parison of the cooling tube.
  • the dislocation pulling device includes a dislocation twisting part for dislocating and twisting the cured cooling tube parison and a filter rod forming machine cloth belt for pulling the dislocation and twisting cooling tube parison
  • the disc traction part can obtain the cooling section products that meet the requirements.
  • the dislocation and twisted part can increase the contact area between the flue gas and the airflow channel, and improve the contact and collision effect between the flue gas and the raw material, thereby improving the cooling effect of the flue gas.
  • the pulling part of the cloth tape reel of the filter rod forming machine can increase the stability of the pulling.
  • the second shearing device 5 includes a flying scissor head for cutting the product in the cooling section. Since the flying scissors head and the product in the cooling section are in a synchronous operation state, the cutting end surface of the product in the cooling section can be kept flush. , the cutting effect is good.
  • a second pressure sensor is provided on the screw and/or the extrusion die head of the extruder 3, and the second pressure sensor is connected to the second servo motor, which can ensure that the cooling masterbatch is melted in a zoned process.
  • the medium pressure is controllable and adjustable.
  • the process of preparing the cooling masterbatch into the cooling tube 1 by the extrusion molding process further includes: determining a second feeding device for quantitatively placing the cooling masterbatch in the extruder 3, which can improve the Stability of extruded material.
  • the cooling tube 1 is packaged by a second packaging machine.
  • the present invention provides the use of the fully degradable cooling firmware according to the present invention and the fully degraded cooling firmware prepared by the above-mentioned method of the present invention in a cooling filter rod 2 for heat-not-burn cigarettes (as shown in Figure 1 ); the uses include: Application of cooling masterbatch in cooling filter rod; and/or application of cooling tube 1 in cooling filter rod 2 (as shown in Figure 1 and Figure 2).
  • the cooling filter rod 2 includes a plurality of first solid filter rods, and particle segments are arranged between adjacent first solid filter rod segments.
  • the particle section includes a hollow tube body and a cooling masterbatch placed in the hollow tube body.
  • the first solid filter rod is used to block the cooling masterbatch.
  • the first solid filter rod is made of the first polymer fiber and plasticizer or adhesive, which can effectively block the cooling masterbatch and prevent the cooling masterbatch from flowing out of the particle section.
  • the first polymer fibers comprise polylactic acid tow, polypropylene tow, and/or cellulose diacetate tow.
  • the cooling filter rod 2 includes a hollow filter rod 6 and/or a second solid filter rod 7 , and the second solid filter rod 7 and/or the hollow filter rod 6 One end and/or both ends of the cooling pipe 1 are connected.
  • the cooling filter rod 2 includes a hollow filter rod 6 and a second solid filter rod 7 , and a cooling pipe disposed between the hollow filter rod 6 and the second solid filter rod 7 1.
  • the second solid filter rod 7 is made of a second polymer fiber and a plasticizer or adhesive.
  • the second polymer fibers comprise polylactic acid tow, polypropylene tow, and/or cellulose diacetate tow.
  • the hollow filter rod 6 is made of a third polymer fiber and a plasticizer or adhesive.
  • the third polymer fibers comprise polylactic acid tow, polypropylene tow, and/or cellulose diacetate tow.
  • a hollow cavity portion 61 is provided inside the hollow filter rod 6 .
  • the hollow cavity portion 61 includes an axial through-type hollow cavity or an axial non-through-type hollow cavity.
  • the hardness of the hollow filter rod is more than 60% of the hardness of the solid filter rod of the same material and outer diameter.
  • a filter rod ternary composite equipment (for the composite cooling tube 1 , the hollow filter rod 6 and the second solid filter rod 7 ) is used to prepare the cooling filter rod 2 for heating non-burning cigarettes.
  • Embodiment 1 the preparation of cooling master batch
  • the raw material is placed inside a twin-screw extruder for melt plasticization and extrusion to form a cooling masterbatch parison.
  • a twin-screw extruder for melt plasticization and extrusion to form a cooling masterbatch parison.
  • the cooled masterbatch parison is transported to a pelletizer for pelletizing.
  • drying temperature is 60-80 degrees Celsius.
  • polylactic acid, polycaprolactone, thermoplastic polyester elastomer, copolymer of butylene adipate and butylene terephthalate, polybutylene succinate were 2 to 4 substances in polypropylene and polyethylene and the solubilizer are mixed at high speed, and the mixing speed is 3000 to 7000 rpm.
  • the first feeding device is used to quantitatively place the raw materials inside the twin-screw extruder for melt plasticization and extrusion.
  • the melting temperature is 170 to 210°C.
  • the air-cooled conveyor belt includes a conveyor belt for conveying the cooling master batch parison, and an air cooling portion for cooling and solidifying the cooling master batch parison is provided on the conveyor belt.
  • the pelletizer is provided with a pelletizing cutter head for pelletizing, which can stably pelletize the cooled masterbatch parison.
  • the particle size of the cooling master batch is 0.1-0.4 mm.
  • cooling masterbatch is packaged by the first packaging machine.
  • the basic characteristics of polylactic acid E-1300 are shown in Table 1.
  • the cooling pipe includes the following steps: purchasing vacuum-packed biodegradable plastics that can be used directly after unpacking, If the package is not used up after opening, it should be sealed and stored again.
  • the biodegradable plastic is prepared into a cooling masterbatch, and the cooling masterbatch is placed in the extruder 3 for melting, plasticizing and extrusion to form a cooling tube parison.
  • the temperature of the material conveying part in the extruder 3 is kept at 140 degrees Celsius
  • the temperature of the material melting part in the extruder 3 is kept at 150 degrees Celsius
  • the temperature of the melt conveying part in the extruder 3 is kept at 160 degrees Celsius
  • the extrusion molding The temperature of the homogenization and conveying part in the extruder 3 is kept at 165 degrees Celsius
  • the temperature of the heating and heat preservation part in the extruder 3 is kept at 165 degrees Celsius
  • the temperature of the extrusion die head in the extruder 3 is kept at 150 degrees Celsius
  • the extrusion die is kept at 150 degrees Celsius.
  • the temperature of the head can be appropriately adjusted according to the extrusion of the cooling tube parison.
  • the rotational speed and pulling speed of the screw of the extruder 3 can be appropriately adjusted according to the wall thickness and inner diameter of the cooling pipe.
  • Shape the cooling tube parison The shaped cooling tube parison is cooled and solidified by the cooling liquid in the cooling tank 41 . Among them, the temperature of the cooling liquid is less than or equal to 25 degrees Celsius. If it is difficult to cure and form, the temperature of the cooling liquid should be further reduced. The cured cooling tube parison is dislocated, twisted and pulled by a dislocation traction device to form a cooling section product. Cut off the product in the cooling section to obtain the cooling pipe 1.
  • the cooling pipe 1 obtained in the second embodiment has the following advantages:
  • the weight of the cooling tube 1 is only about 80% of the wrinkle form (film wrinkle), the material consumption is low, and the economy is good.
  • the cooling area of the cooling tube 1 is 2.7 times that of the round tube with film (paper tube with polylactic acid film). Considering that the porosity is only 86% of that of the round tube with film, The actual cooling efficiency of the cooling tube 1 is 2.3 times that of the round tube with film.
  • the PLA/PBAT copolymer was placed in a vacuum drying oven and dried at 50 degrees Celsius for 4 hours; then PLA/PBAT was added to an internal mixer (SU-70L, Jiangsu Suyuan Rubber and Plastic Technology Co., Ltd.) in different proportions and dried at 180 °C.
  • Different PLA/PBAT blend series samples were prepared by mixing for 3 minutes under the processing conditions of degrees Celsius/120 rpm (revolutions per minute). The code and composition of the prepared blend series samples are shown in Table 3.
  • FIG. 6 is the thermogravimetric curve of the PLA/PBAT blend series samples.
  • curve 1 represents the thermal weight loss curve of pure PBAT. The temperature reaches about 400 degrees Celsius, and its mass retention rate is basically 100%, indicating that the thermal stability of PBAT is very high.
  • the thermal decomposition temperature of the PLA/PBAT blend series samples was determined, as shown in Table 4.
  • PLA/PBAT material mechanical properties of PLA/PBAT were determined. Specifically, the PLA/ PBAT blending series samples were prepared and tested in accordance with ASTM D-638 Type IV standard samples; all samples were hot-pressed under the conditions of 190 degrees Celsius and 10 MPa for 3 minutes, cooled and formed, and then cut with standard cutters The standard samples were taken out, and then the tensile properties were tested with a HT-9112 universal material testing machine from Hongda Instrument Company at a tensile speed of 50 mm/min at 25 degrees Celsius. The values of all mechanical properties under each composition are the average value of the test data of 5 splines, as shown in Table 5.
  • FIG. 7 is a schematic diagram of the tensile properties of PLA/PBAT blend series samples.
  • the tensile strength ( ⁇ f) of pure PLA is as high as 48.3 MPa, while the elongation at break ( ⁇ f) is only 3.7 %; in the PLAxPBATy blend series samples, with the increase of PLA content, the fracture of the PLAxPBATy blend series samples The elongation values increased significantly.
  • the material thermal properties of PLA/PBAT were determined. Specifically, the prepared PLA and PLAxPBATy series samples were analyzed by TA company Q100 differential scanning calorimetry analyzer (differential scanning calorimetry). Scanning calorimeter, DSC) to analyze its melting point, crystallinity and other thermal properties. Within the detection temperature range, adjust the reference line so that its fluctuation range is less than 0.04mW (milliwatts), so that the maximum deviation of the heat of fusion is within ⁇ 3J/g (joule per gram), that is, for crystallinity, about only 1% error. The instrument is calibrated with pure indium (indium) fusion heat of 28.4 joules per gram.
  • Figure 8 shows (a) PLA, (b) PLA 90 PBAT 10 , (c) PLA 80 PBAT 20 , (d) PLA 70 PBAT 30 , (e) PLA 60 PBAT 40 , (f) PLA 50 PBAT 50 and (g) PLA 50 PBAT 50 ) DSC analysis of a PBAT sample scanned at 40°C/min. From Figure 8(a), it can be observed that the glass transition temperature of PLA is 60 degrees Celsius, and the melting endothermic peak temperature of PLA is 171.8 degrees Celsius. A broad endothermic peak corresponding to PBAT can be seen from Fig. 8(g), with a peak around 55°C.
  • the crystallinity, melting temperature and recrystallization onset temperature of PLAxPBATy samples decreased gradually with the increase of PBAT content.
  • the glass transition temperature values of the PLAxPBATy samples increased gradually with the increase of PBAT content.
  • the glass transition temperature values of PLA in the PLAxPBATy blend samples increased from 62.8 degrees Celsius to 63 degrees Celsius and 63.6 degrees Celsius.

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Extrusion Moulding Of Plastics Or The Like (AREA)
  • Processing And Handling Of Plastics And Other Materials For Molding In General (AREA)

Abstract

Sont divulgués un ensemble de refroidissement entièrement dégradable, son procédé de préparation et son utilisation. L'ensemble de refroidissement entièrement dégradable comprend un mélange maître de refroidissement entièrement dégradable pour réduire la température de la fumée. Le mélange maître de refroidissement est constitué d'une pluralité de matériaux entièrement dégradables et d'un agent de solubilisation. Le procédé de préparation de l'ensemble de refroidissement entièrement dégradable comprend les étapes suivantes consistant : à obtenir la pluralité de matériaux entièrement dégradables et à les mélanger, et à ajouter l'agent de solubilisation durant le mélange pour obtenir une matière première permettant la granulation ; et à extruder et à réaliser la granulation de la matière première au moyen d'un procédé d'extrusion et de granulation, afin d'obtenir le mélange maître de refroidissement entièrement dégradable. L'ensemble de refroidissement dégradable est destiné à être utilisé une barre de filtre de refroidissement pour des cigarettes sans combustion. L'utilisation comprend l'utilisation du mélange maître de refroidissement dans la barre de filtre de refroidissement ; et/ou l'utilisation de tubes de refroidissement dans la barre de filtre de refroidissement. La présente invention peut efficacement réduire la température de la fumée au niveau de l'extrémité d'entrée des cigarettes, et n'affecte pas la résistance à l'aspiration et l'efficacité de filtration de la barre de filtre de refroidissement.
PCT/CN2021/122583 2020-12-11 2021-10-08 Ensemble de refroidissement entièrement dégradable, son procédé de préparation et son utilisation WO2022121480A1 (fr)

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