WO2021237655A1 - Liquid additive assisted polymer extrusion and blending method and device and use thereof - Google Patents

Liquid additive assisted polymer extrusion and blending method and device and use thereof Download PDF

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Publication number
WO2021237655A1
WO2021237655A1 PCT/CN2020/093191 CN2020093191W WO2021237655A1 WO 2021237655 A1 WO2021237655 A1 WO 2021237655A1 CN 2020093191 W CN2020093191 W CN 2020093191W WO 2021237655 A1 WO2021237655 A1 WO 2021237655A1
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Prior art keywords
liquid additive
liquid
additive
screw
melt
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PCT/CN2020/093191
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French (fr)
Chinese (zh)
Inventor
李东
马鹏涛
叶南飚
黄险波
廖洋威
于亚勇
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金发科技股份有限公司
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Publication of WO2021237655A1 publication Critical patent/WO2021237655A1/en

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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29CSHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/25Component parts, details or accessories; Auxiliary operations
    • B29C48/285Feeding the extrusion material to the extruder
    • B29C48/297Feeding the extrusion material to the extruder at several locations, e.g. using several hoppers or using a separate additive feeding
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29BPREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B9/00Making granules
    • B29B9/02Making granules by dividing preformed material
    • B29B9/06Making granules by dividing preformed material in the form of filamentary material, e.g. combined with extrusion
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29CSHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/25Component parts, details or accessories; Auxiliary operations
    • B29C48/285Feeding the extrusion material to the extruder
    • B29C48/29Feeding the extrusion material to the extruder in liquid form
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29CSHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/25Component parts, details or accessories; Auxiliary operations
    • B29C48/36Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die
    • B29C48/395Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die using screws surrounded by a cooperating barrel, e.g. single screw extruders
    • B29C48/40Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die using screws surrounded by a cooperating barrel, e.g. single screw extruders using two or more parallel screws or at least two parallel non-intermeshing screws, e.g. twin screw extruders
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29CSHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/25Component parts, details or accessories; Auxiliary operations
    • B29C48/36Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die
    • B29C48/50Details of extruders
    • B29C48/68Barrels or cylinders
    • B29C48/682Barrels or cylinders for twin screws
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29CSHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/25Component parts, details or accessories; Auxiliary operations
    • B29C48/36Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die
    • B29C48/50Details of extruders
    • B29C48/76Venting, drying means; Degassing means
    • B29C48/762Vapour stripping
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29CSHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/25Component parts, details or accessories; Auxiliary operations
    • B29C48/36Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die
    • B29C48/50Details of extruders
    • B29C48/76Venting, drying means; Degassing means
    • B29C48/765Venting, drying means; Degassing means in the extruder apparatus
    • B29C48/766Venting, drying means; Degassing means in the extruder apparatus in screw extruders
    • B29C48/767Venting, drying means; Degassing means in the extruder apparatus in screw extruders through a degassing opening of a barrel
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29CSHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/25Component parts, details or accessories; Auxiliary operations
    • B29C48/92Measuring, controlling or regulating
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29CSHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C2948/00Indexing scheme relating to extrusion moulding
    • B29C2948/92Measuring, controlling or regulating
    • B29C2948/92009Measured parameter
    • B29C2948/92019Pressure
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29CSHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C2948/00Indexing scheme relating to extrusion moulding
    • B29C2948/92Measuring, controlling or regulating
    • B29C2948/92009Measured parameter
    • B29C2948/92209Temperature
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29CSHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C2948/00Indexing scheme relating to extrusion moulding
    • B29C2948/92Measuring, controlling or regulating
    • B29C2948/92323Location or phase of measurement
    • B29C2948/92361Extrusion unit
    • B29C2948/9238Feeding, melting, plasticising or pumping zones, e.g. the melt itself
    • B29C2948/924Barrel or housing

Definitions

  • the invention belongs to the technical field of polymer materials, and specifically relates to a method, a device and an application of a liquid additive assisted polymer extrusion blending.
  • Polymer materials often need to be modified and prepared into blends to meet different product requirements. Usually, other polymers, fillers, reinforcements, flame retardants and other components are added to the polymer, and the twin-screw extruder, single-screw extruder, internal mixer and other equipment are used for melt mixing, extrusion granulation, etc. Preparation of modified polymer materials.
  • Conventional extrusion blending adopts changing the screw combination, screw speed, feeding method, processing temperature and other equipment and process conditions of the twin-screw extruder to achieve stable extrusion blending and achieve the required product performance. It is often necessary to dry the materials to remove water before extrusion and blending, such as polyamide, acrylonitrile-butadiene-styrene terpolymers, polyacrylates and other resins to avoid material degradation during processing , Discoloration and other defects. For hydrolysis-resistant multi-phase unstable polymer systems, vacuuming is often used during the blending modification process to drain the moisture and volatiles from the material.
  • additives that are melted by heating, easily decomposed by heating, and easily volatile when heated, such as low melting point additives, flame retardants, processing oils, etc., when the materials are blended, they are limited by the characteristics of the materials and are difficult to mix uniformly. The nature of the process changes, which affects the quality of the product.
  • the present invention provides a liquid additive assisted polymer extrusion blending method, device and application, which can effectively solve the above problems. problem.
  • the specific solution adopted by the present invention is: a liquid additive assisted polymer extrusion blending method
  • the technical solution is: after the raw material mixture is converted into a melt, the liquid additive is continuously injected into the melt Inside, the above additives and the above melt are fully fused to form a uniform fusion, and finally the target product is obtained after dehydration and devolatilization.
  • the raw material mixture of the solvent-resistant multiphase non-stable polymer is fed into the screw barrel through the feeding port of the twin-screw extruder, and the screw is conveyed through the screw;
  • step S2 a melt of the raw material mixture described in step S1 is formed in the melting zone in the barrel;
  • step S3 At the position of the melting zone described in step S2, the liquid additive to be added is continuously and quantitatively injected into the melting zone through a pressure applying device.
  • the liquid additive is in an overheated state and is fully mixed with the melt described in step S2 through the action of the screw Form a fusion;
  • step S4 The fusion material described in step S3 is transported forward through the screw, and dehydrated and devolatilized through the exhaust port downstream of the screw barrel;
  • a liquid additive assisted polymer extrusion and blending device comprising a plasticizing unit and an injection unit for preparing the target product; characterized in that: the injection unit is arranged on the plasticizing unit and forms a melt with the raw material The area is connected and arranged for injecting liquid additives into the plasticizing unit.
  • the plasticizing unit includes a screw barrel, a screw arranged in the screw barrel, and a feed assembly arranged at the feeding end of the screw barrel; wherein the screw barrel is provided with spaced exhaust ports near the discharge end; and The exhaust port and the vacuum chamber are respectively connected and arranged to form a negative pressure zone in the negative pressure area.
  • the screw barrel is provided with a mixing area for mixing the melt and the liquid additive, and the mixing area is provided with a sensor for detecting the pressure and temperature in the barrel; the vacuum chamber is connected with the external negative pressure system, and an instrument is set to detect the vacuum Room pressure.
  • the injection unit includes a compounding device, a storage device, and a conveying device for mixing two additives; wherein, the output end of the compounding device is connected with the input end of the storage device, and is used for quantitatively directing through a pipeline.
  • the conveying device conveys the mixed additives; the output end of the conveying device is connected with the area where the raw material in the plasticizing unit forms a melt.
  • the compounding device includes a silo I, a silo II, a container, a stirring paddle, and a metering module; wherein the output ends of the silo I and the silo II communicate with the input end of the container; the container is provided with a stirring Paddle; the bottom of the container is provided with a metering module for weighing; wherein the output end of the container is connected to the storage device.
  • the storage device includes a storage container, a stirrer, and a weighing unit; wherein the input end of the storage container is connected with the output end of the compounding device; the storage container is provided with a stirrer; the bottom of the storage container is provided with a meter for weighing Unit; wherein the output end of the storage container is connected to the input end of the conveying device.
  • the delivery device includes a high-pressure metering pump; the input end of the high-pressure metering pump is connected to the output end of the storage device, and the output end of the high-pressure metering pump forms a region where a melt is formed by a one-way injection valve with the raw materials on the plasticizing unit Connected.
  • the basic principle of the liquid additive-assisted polymer extrusion and blending method of the present invention is: the raw material mixture of the solvent-resistant multiphase non-stable polymer is added through the feed port of the twin-screw extruder, and it is conveyed through the action of the screw.
  • liquid additives and solvents at room temperature will not immediately vaporize after being heated in a high-temperature melt, but will exist in a superheated state.
  • a superheated state For example, when water is used as a solvent, they will exist in the form of superheated water, that is, subcritical water.
  • the superheated additives and solvent components are evenly dispersed in the melt, and are transported to the downstream area with the screw. No less than one exhaust port connected to the atmosphere or negative pressure system is provided on the screw barrel in the downstream area to reduce the pressure of the fusion and vaporize the solvent in the additive, thereby smoothly extruding into a strip, and then granulating .
  • subcritical water refers to: when the pressure is 2.4MPa, the boiling point of water is about 220°C; when the pressure is 2.9MPa, the boiling point of water is about 230°C; when the pressure is 4MPa, the boiling point of water is about 251°C; when the pressure is 8MPa, the boiling point of water is about 300. °C.
  • the present invention also provides an application of the liquid additive assisted polymer extrusion and blending device in the production of polymers as described in the foregoing solution.
  • polymers include low-odor polymers or other types of polymers.
  • the present invention helps to reduce the local high temperature inside the melt by adding the additives to the solvent to form a liquid additive, so that the overall temperature is reduced to a certain extent and is more uniform, which is beneficial to the uniformity of the mixing of the components;
  • the superheated liquid additives and solvent components are evenly dispersed in the melt formed by the raw materials; when transported to the rear end of the screw barrel, they vaporize as solvent vapor and are discharged or sucked away by the negative pressure system, and the fusion
  • a large number of bubble bursts occurred, which increased the effect of interface renewal, so that the residual monomers and small molecular components in the fusion were removed, and products with better odor and sensory were obtained; even for fillers and reinforcement components on polar surfaces, the original
  • the method of the invention can also increase the miscibility with the matrix, improve the dispersion distribution and the interface effect in the non-polar matrix, thereby improving the quality of the product.
  • the evaporation and loss process of the liquid additive produces a large number of bubbles and bursts, which increases the mixing effect of the fusion.
  • the additives that are easily melted by heating, easily decomposed by heating, and easily volatile when heated, they can be liquefied with the help of solvents, which can be accurately added on the basis of ensuring the characteristics of the additives, and the mixing is uniform.
  • the device of the invention has simple structure, can be directly modified on the existing double screw extruder, has small modification amount, stable operation, low failure rate, stable and reliable product quality, and solves the problems existing in the prior art.
  • Figure 1 is a schematic diagram of the structure of the present invention.
  • Figure 2 is a flow chart of a method for liquid additive assisted polymer extrusion blending.
  • Figure 3 is a flow chart when the two additives are mixed.
  • the area shown by 1021 in FIG. 1 is the area where the raw material is not completely melted; the area shown by 1023 refers to the area where the liquid additive in the superheated state and the raw material in the molten state are fused.
  • the present invention provides a liquid additive assisted polymer extrusion blending method. After being converted into a molten material, the liquid additive is continuously injected into the molten material, so that the additive and the molten material are fully fused to form a uniform fusion, and finally dehydration and devolatilization are performed to obtain the target product.
  • the above-mentioned method of liquid additive assisted polymer extrusion and blending may specifically include the following steps:
  • the raw material mixture of the solvent-resistant multiphase non-stable polymer is fed into the screw barrel through the feeding port of the twin-screw extruder, and the screw is conveyed through the screw;
  • step S2 a melt of the raw material mixture described in step S1 is formed in the melting zone in the barrel;
  • step S3 At the position of the melting zone described in step S2, the liquid additive to be added is continuously and quantitatively injected into the melting zone through a pressure applying device.
  • the liquid additive is in an overheated state and is fully mixed with the melt described in step S2 through the action of the screw Form a fusion;
  • step S4 The fusion described in step S3 is transported forward through the screw, and the superheated liquid additive is vaporized into solvent vapor downstream of the screw barrel, and the bubbles in the fusion burst, so that the negative pressure device is used to make the residue inside the fusion
  • the monomer and small molecule components are removed, dehydration and devolatilization are completed;
  • the liquid additive is in an overheated state after being injected into the melt.
  • the liquid additive is water or a single liquid additive or suspension or a liquid containing a gaseous additive; or, the liquid additive is water, a single liquid additive, a suspension, or a liquid containing a gaseous additive. A mixture of any two of them.
  • liquid additive is a mixture of any two of a single liquid additive, a suspension, and a liquid containing a gaseous additive
  • the mixing process is as follows:
  • step S2 Input the first-stage mixed liquid obtained in step S2 into the second-stage mixing unit to obtain the second-stage mixed liquid, and then pass the second metering to obtain the total amount of liquid output by the second-stage mixing unit;
  • the corresponding container is set as a closed container.
  • the single liquid additive can be a flame retardant or a coupling agent or a processing oil; the suspension can be a mixture of a powder additive and a solution; wherein the powder additive can be a nano filler, a dispersant, or a coloring agent. Any one or more of reagents and reaction aids; wherein the solution can be water or a water-alcohol mixture; the liquid containing gaseous additives can be an aqueous solution containing carbon dioxide or a water-alcohol solution containing carbon dioxide.
  • the process of dehydration and devolatilization of the fusion is as follows: when the fusion is transported to the rear end of the screw barrel, since the rear end of the screw barrel is arranged with a plurality of exhaust ports and the above-mentioned exhaust ports are all connected Negative pressure device; combined with the action of the screw, a large number of bubbles in the above fusion material are broken to complete the interface reorganization of the fusion, and the gas generated by the broken bubbles is drawn out of the barrel through the negative pressure device to achieve dehydration and devolatilization.
  • a liquid additive assisted polymer extrusion and blending device includes a plasticizing unit 1 and an injection unit 2 for preparing the target product, in which:
  • the plasticizing unit 1 can be modified from an existing double screw extruder. Specifically, it includes a screw barrel 101, a screw 102 arranged in the screw barrel 101, and a feeding end arranged at the feeding end of the screw barrel 101.
  • the above-mentioned screw barrel 101 is provided with spaced exhaust ports 1012, 1013 near the discharge end; and the exhaust ports 1012, 1013 and the vacuum chambers 107, 109 are respectively connected and arranged and the The vacuum chambers 107 and 109 are connected to the external vacuum system, and negative pressure meters 108 and 1010 are set to detect the pressure in the vacuum chambers 107 and 109 respectively.
  • a mixing area 1022 for mixing the melt and liquid additives is provided on the above-mentioned screw barrel 101, and a pressure sensor 105 and a temperature sensor 106 for detecting the pressure and temperature in the barrel are provided in the mixing area 1022.
  • the injection unit 2 includes a compounding device 201 for mixing two additives, a storage device 202, and a conveying device 204; wherein, the output end of the compounding device 201 is connected to the input end of the storage device 202, It is used to quantitatively deliver the mixed additive to the delivery device 204 through the pipeline 203; the output end of the delivery device 204 is connected to the mixing area 1022 and is used to inject the liquid additive into the melt in the mixing area 1022, and further The mixing, through the action of the screw 102, forms a uniform fusion.
  • the delivery device 204 includes a high-pressure metering pump 2041; the input end of the high-pressure metering pump 2041 is connected to the output end of the storage device 202, and the output end of the high-pressure metering pump 2041 can be connected to the plasticizing unit 1 through the one-way injection valve 205 The areas where the raw materials form the melt are connected.
  • the compounding device 201 includes a silo I2011, a silo II2012, a container 2013, a stirring paddle 2014, and a metering module 2015; Wherein, the output ends of the silo I2011 and II2012 communicate with the input of the container 2013; the container 2013 is provided with a stirring paddle 2014; the bottom of the container 2013 is provided with a weighing module 2015 for weighing;
  • the output end of the container 2013 is connected to the storage device 202.
  • the storage device 202 includes a storage container 2021, a stirrer 2022, and a metering unit 2023; wherein the input end of the storage container 2021 is connected to the output end of the compounding device 201; the storage container 2021 is provided with a stirrer 2022; the storage container 2021 A metering unit 2023 for weighing is provided at the bottom of the, wherein the output end of the storage container 2021 is connected to the input end of the conveying device 204; the conveying device 204 includes a high-pressure metering pump 2041; the input of the high-pressure metering pump 2041 The end is connected with the output end of the storage device 202, and the output end of the high-pressure metering pump 2041 injects the liquid additive into the melt in the mixing zone 1022 through the regulating valve 2043.
  • the output end of the high-pressure metering pump 2041 is also provided with a pressure relief pipe and a safety valve 2042 in parallel to form a pressure relief pipeline, which is used to relieve the pressure when the pressure in the high-pressure metering pump 2041 is too high to ensure the safety of the pipeline system .
  • the metering feeding device 103 adds the material 104 to the screw barrel 101 and conveys it forward under the action of the screw 102.
  • the material is plasticized and melted in the mixing area 1022 by the screw 102 to form a melt, and then Under the action of 102, a certain pressure is formed in the mixing area 1022.
  • the multi-component additives are respectively placed in the silo I2011 and the silo II2012, are added to the compounding container 2013 in proportion, and are compounded into a uniform mixture under the action of the stirring paddle 2014.
  • the metering module 2015 is used to indicate the additive ratio and the weight of the mixture.
  • the above-mentioned uniform mixture is transported to the storage container 2021 for storing and compounding additives, and is kept uniform under the action of the agitator 2022, and the metering unit 2023 indicates the weight of the additive mixture.
  • the additive mixture in the storage device 202 is transported to the high-pressure metering pump 2041 through the delivery pipeline 203.
  • the high-pressure metering pump 2041 quantitatively outputs the additive mixture to the mixing area 1022 to ensure that the liquid additive is injected into the melt.
  • the output end of the high-pressure metering pump 2041 A pressure sensor 206 can be provided to collect the internal pressure when the additive mixture is injected into the melt in the extruder. In addition, when the pressure is too high, the safety valve 2042 on the pressure relief pipe triggers a protective effect.
  • the mixture of the additives and the melt is mixed under the action of the screw 102 in the mixing zone 1022 to form a uniform fusion.
  • the aforesaid fusion is moved to the exhaust ports 1012, 1013 area, and the water and volatiles in the fusion are evacuated by the vacuum system until the fusion with additives is conveyed to the granulation unit by the screw 102.
  • Example 1 provides an example using a single water as an additive, that is, a water-assisted polymer extrusion blending method to improve the odor of the product and produce a low-odor high-grade product.
  • the metering feeding device 103 adds the material 104 to the screw barrel 101 and conveys it forward under the action of the screw 102.
  • the material is plasticized and melted in the mixing area 1022 by the screw 102 to form a melt.
  • a certain pressure is formed in the mixing area 1022.
  • the multi-component additives are respectively placed in the silo I2011 and the silo II2012, are added to the compounding container 2013 in proportion, and are compounded into a uniform mixture under the action of the stirring paddle 2014.
  • the metering module 2015 is used to indicate the additive ratio and the weight of the mixture.
  • the above-mentioned uniform mixture is transported to the storage container 2021 for storing and compounding additives, and is kept uniform under the action of the agitator 2022, and the metering unit 2023 indicates the weight of the additive mixture.
  • the additive mixture in the storage device 202 is transported to the high-pressure metering pump 2041 through the delivery pipeline 203.
  • the high-pressure metering pump 2041 quantitatively outputs the additive mixture to the mixing area 1022 to ensure that the liquid additive is injected into the melt.
  • a pressure sensor 206 can be provided to collect the internal pressure when the additive mixture is injected into the melt in the extruder.
  • the safety valve 2042 on the pressure relief pipe triggers the pressure relief protection function.
  • the mixture of the additives and the melt is mixed under the action of the screw 102 in the mixing zone 1022 to form a uniform fusion.
  • the aforesaid fusion is moved to the exhaust ports 1012, 1013 area, and the water and volatiles in the fusion are evacuated by the vacuum system until the fusion with additives is conveyed to the granulation unit by the screw 102.
  • the superheated water and the melt are evenly dispersed through the spiral shear action of the screw 102, and then the water is vaporized and the fusion is carried through the exhaust ports 1012 and 1013.
  • the volatile matter in the medium is discharged to achieve devolatilization, and a high-grade low-odor product can be obtained.
  • Specific embodiment 2 Compared with embodiment 1, the main difference of this embodiment is that a single liquid auxiliary agent, such as a flame retardant, a coupling agent, a processing oil, etc., is used as an additive to obtain a better material mixing effect.
  • a single liquid auxiliary agent such as a flame retardant, a coupling agent, a processing oil, etc.
  • the method of adding the liquid additives is similar to that of the water in Example 1.
  • the main purpose is to solve the difficulties and risks of adding these liquid additives to the extruder after being conventionally mixed with materials, such as uneven mixing with materials, After mixing, agglomeration, volatilization of liquid additives, smell of liquid additives, premature decomposition of heat-sensitive additives, environmental problems, etc., the liquid additives are separately metered into the polymer melt and fully mixed to achieve uniform mixing effect and product quality Stable and easy to operate, it can further reduce the odor of the product and realize the production of high-grade and low-odor products.
  • Specific embodiment 3 Compared with embodiment 1 and embodiment 2, the main difference of this embodiment lies in the use of powder additives, such as nano fillers, dispersants, colorants, reaction aids, etc., and liquids, such as water, water- A method in which a suspension composed of an alcohol mixture and the like is used as an additive, that is, a powder additive is turned into a liquid additive to assist the extrusion and blending of a polymer.
  • powder additives such as nano fillers, dispersants, colorants, reaction aids, etc.
  • liquids such as water, water- A method in which a suspension composed of an alcohol mixture and the like is used as an additive, that is, a powder additive is turned into a liquid additive to assist the extrusion and blending of a polymer.
  • the additives and the liquid auxiliary additives are added to the silo I2011 and the silo II2012 respectively, and the container 2013 for compounding is added in proportion to the mixing paddle 2014 to form a homogeneous mixture.
  • the metering module 2015 is used to indicate the proportion of additives and the weight of the mixture.
  • the uniform mixture is mixed by the compounding device 201 and transported to the storage container 2021 for storing the compounded additives. The uniformity is maintained under the action of the stirrer 2022.
  • the metering unit 2023 indicates the weight of the additive mixture .
  • the additive mixture in the rear storage device 202 is delivered to the delivery device 204 via the delivery pipeline 203.
  • the other features of this embodiment are the same as those of Embodiments 1 and 2, and will not be repeated.
  • This embodiment mainly solves the problem that a small amount of powder additives such as nano fillers and toners are difficult to be fully dispersed in the melt, and solves the problem of uneven mixing of a small amount of additives and materials during conventional mixing, resulting in fluctuations in the quality of blended and extruded products.
  • a small amount of powder additives use liquid additives as a carrier, separately metered into the polymer melt, and fully mixed to achieve uniform mixing effect, stable product quality, and convenient operation, which can further reduce product odor and realize high-grade low-odor products, etc. Production of polymers.
  • Specific embodiment 4 Compared with embodiments 1, 2 and 3, the main difference of this embodiment lies in the use of gaseous additives, such as carbon dioxide and liquids, such as water, water-alcohol mixtures, etc., as additives, that is, gaseous additives Additives become liquid additives to assist polymer extrusion blending methods.
  • gaseous additives such as carbon dioxide and liquids, such as water, water-alcohol mixtures, etc.
  • gaseous additives and liquid auxiliary additives are added to the airtight and pressure-keeping silo I2011 and II2012 respectively, and are added to the mixing container 2013 in proportion, and the gas is dissolved under the action of the stirring paddle 2014 In the liquid, it is compounded into a homogeneous mixture with a certain gas solubility.
  • the metering module 2015 is used to collect the proportion of additives and the weight of the mixture, mix it into a homogeneous mixture through the sealing and pressure-keeping compounding device 201, and transport it to a sealed and pressure-keeping storage container In 2021, the metering unit 2023 indicates the weight of the additive mixture.
  • the additive mixture in the storage device 202 that can be sealed and pressure-maintained is delivered to the delivery device 204 via the delivery pipeline 203.
  • Other features of this embodiment are the same as those of Embodiments 1, 2 and 3, and will not be repeated here.
  • This embodiment mainly solves the problem that gaseous additives, such as carbon dioxide, are difficult to add in the melt and are difficult to fully disperse.
  • gaseous additives such as carbon dioxide
  • it can be accurately metered and injected into the polymer melt with the aid of the liquid auxiliary additive as a carrier for full mixing.
  • the volatile matter in the material is further carried and gas stripped to further reduce the odor of the product and realize the production of high-grade and low-odor products.
  • the metering module 2015 and the metering unit 2023 described herein may be pressure sensors; the agitating paddle 2014 and the agitator 2022 may have the same structure.
  • the single liquid additive described herein can be an aqueous liquid additive.

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Abstract

A liquid additive assisted polymer extrusion and blending method and device. The solution lies in that: converting a raw material mixture into a melt, continuously injecting a liquid additive into the interior of the melt so that the additive is fully fused with the melt to form a uniform fusion, and finally performing dehydration and devolatilization, so as to obtain a target product.

Description

一种液态添加剂辅助聚合物挤出共混的方法、装置及应用Method, device and application of liquid additive assisted polymer extrusion and blending 技术领域Technical field
本发明属于高分子材料技术领域,具体涉及一种液态添加剂辅助聚合物挤出共混的方法、装置及应用。The invention belongs to the technical field of polymer materials, and specifically relates to a method, a device and an application of a liquid additive assisted polymer extrusion blending.
背景技术Background technique
聚合物材料往往需要进行改性制备成共混物以满足不同的产品需求。通常在聚合物中加入其他聚合物、填料、增强体、阻燃剂等组分,通过双螺杆挤出机、单螺杆挤出机、密炼机等设备进行熔融混炼、挤出造粒等制备改性聚合物材料。Polymer materials often need to be modified and prepared into blends to meet different product requirements. Usually, other polymers, fillers, reinforcements, flame retardants and other components are added to the polymer, and the twin-screw extruder, single-screw extruder, internal mixer and other equipment are used for melt mixing, extrusion granulation, etc. Preparation of modified polymer materials.
常规挤出共混采用改变双螺杆挤出机的螺杆组合、螺杆转速、喂料方式、加工温度等设备和工艺条件以实现稳定的挤出共混和达到需求的产品性能。在进行挤出共混前往往需要对物料进行烘干除水,如聚酰胺、丙烯腈-丁二烯-苯乙烯的三元共聚物、聚丙烯酸酯类等树脂,以避免加工过程使材料降解、变色等缺陷。对于耐水解的多相非稳态聚合物体系,共混改性加工过程中也往往采取抽真空等方式使材料中的水分、挥发分等排出。对于应用于汽车内饰的多种组分进行增韧、增强等改性的聚丙烯材料,可向其粒子混合物中加入一定量的水,以改善其气味感官,但是粒子混合物中的水往往和高温的机筒接触后变成水蒸汽而大部分散失,作用效果有限,并且散失的水蒸汽通过挤出机加料口排出,影响了物料的顺利下料,在一定程度上影响了产量和生产稳定性。另外,对于一些受热熔化的、受热易分解的以及受热易挥发的添加剂,如低熔点助剂、阻燃剂、加工油等,在进行物料共混时受限于物料特性难以混合均匀,在添加过程中性质发生变化,影响产品品质。Conventional extrusion blending adopts changing the screw combination, screw speed, feeding method, processing temperature and other equipment and process conditions of the twin-screw extruder to achieve stable extrusion blending and achieve the required product performance. It is often necessary to dry the materials to remove water before extrusion and blending, such as polyamide, acrylonitrile-butadiene-styrene terpolymers, polyacrylates and other resins to avoid material degradation during processing , Discoloration and other defects. For hydrolysis-resistant multi-phase unstable polymer systems, vacuuming is often used during the blending modification process to drain the moisture and volatiles from the material. For polypropylene materials that have been modified to toughen and strengthen various components used in automotive interiors, a certain amount of water can be added to the particle mixture to improve its odor and sensory. However, the water in the particle mixture is often After the high-temperature barrel is in contact, it becomes water vapor and most of it is lost. The effect is limited, and the lost water vapor is discharged through the feed port of the extruder, which affects the smooth feeding of materials, and to a certain extent, it affects the output and production stability. sex. In addition, for some additives that are melted by heating, easily decomposed by heating, and easily volatile when heated, such as low melting point additives, flame retardants, processing oils, etc., when the materials are blended, they are limited by the characteristics of the materials and are difficult to mix uniformly. The nature of the process changes, which affects the quality of the product.
现有的,如中国专利申请CN11082007,《一种高性能纳米涤纶长丝的制备方法》中,公开的步骤(2)中,采用“将干燥后的聚酯切片与添加剂放入螺杆挤出机中熔融”的方法进行添加剂的添加。由于螺杆挤出机对聚合物加工是在螺杆旋转产生的剪切热和外加热的双重作用下实现的,并且剪切热占较大比例。聚合物是热的不良导体,过多的剪切热不能及时传递给螺杆而被冷却水带走,导致熔体物料温度往往高于显示温度,并且由于螺杆的结构特征导致在熔体内部的温度存在分布,甚至在螺棱的顶部出现局部温度过高,添加剂出现汽化,对共混物中的热稳定性较差组分不利。聚合物的黏度受温度影响非常大,加工过程不均匀温度和局部高温会影响产品品质。Existing, such as Chinese patent application CN11082007, "A method for preparing high-performance nano-polyester filament", in the disclosed step (2), "put the dried polyester chips and additives into the screw extruder" Additives are added by the method of "medium melting". Because the screw extruder processes the polymer under the dual action of the shear heat generated by the screw rotation and external heating, and the shear heat accounts for a large proportion. Polymer is a poor conductor of heat. Excessive shear heat cannot be transferred to the screw in time and is taken away by the cooling water. As a result, the temperature of the melt material is often higher than the displayed temperature, and the temperature inside the melt is caused by the structural characteristics of the screw. There is a distribution, and even local overheating occurs at the top of the spiral ridge, and the additive vaporizes, which is detrimental to the components with poor thermal stability in the blend. The viscosity of the polymer is greatly affected by the temperature, and the uneven temperature and local high temperature during the processing process will affect the product quality.
可见,现有技术中在使用添加剂时容易发生汽化、分布不均而导致产品品质下降。It can be seen that in the prior art, when additives are used, vaporization and uneven distribution are likely to occur, resulting in a decrease in product quality.
发明内容Summary of the invention
为了解决现有技术中在使用添加剂时容易发生汽化、分布不均而导致产品品质下降的问题,本发明提供一种液态添加剂辅助聚合物挤出共混的方法、装置及应用,能够有效解决上述问题。In order to solve the problem of product quality degradation caused by vaporization and uneven distribution of additives in the prior art, the present invention provides a liquid additive assisted polymer extrusion blending method, device and application, which can effectively solve the above problems. problem.
为了实现上述目的,本发明采用的具体方案为:一种液态添加剂辅助聚合物挤出共混的方法,其技术方案在于:将原料混合物转化为熔融物后,将液态添加剂连续注入至上述熔融物内部,使上述添加剂与上述熔融物充分融合形成均匀的融合物,最后进行脱水、脱挥后得到目标产物。In order to achieve the above object, the specific solution adopted by the present invention is: a liquid additive assisted polymer extrusion blending method, the technical solution is: after the raw material mixture is converted into a melt, the liquid additive is continuously injected into the melt Inside, the above additives and the above melt are fully fused to form a uniform fusion, and finally the target product is obtained after dehydration and devolatilization.
具体的包括以下步骤:Specifically, it includes the following steps:
S1.将耐溶剂的多相非稳态聚合物的原料混合物通过双螺杆挤出机的加料口加入螺筒内,通过螺杆进行螺旋输送;S1. The raw material mixture of the solvent-resistant multiphase non-stable polymer is fed into the screw barrel through the feeding port of the twin-screw extruder, and the screw is conveyed through the screw;
S2.经过S1步骤,在螺筒内的熔融区形成S1步骤所述原料混合物的熔融 物;S2. After step S1, a melt of the raw material mixture described in step S1 is formed in the melting zone in the barrel;
S3.在S2步骤所述的熔融区位置通过施压装置将待添加的液态添加剂连续、定量注入至该熔融区内,液态添加剂处于过热状态,通过螺杆作用与S2步骤所述的熔融物充分混合形成融合物;S3. At the position of the melting zone described in step S2, the liquid additive to be added is continuously and quantitatively injected into the melting zone through a pressure applying device. The liquid additive is in an overheated state and is fully mixed with the melt described in step S2 through the action of the screw Form a fusion;
S4.通过螺杆将S3步骤所述的融合物向前输送,并在螺筒下游通过排气口进行脱水、脱挥;S4. The fusion material described in step S3 is transported forward through the screw, and dehydrated and devolatilized through the exhaust port downstream of the screw barrel;
S5.在螺筒的出料端得到目标产物。S5. Obtain the target product at the discharge end of the screw barrel.
一种液态添加剂辅助聚合物挤出共混的装置,包括用于制备目标产物的塑化单元和注入单元;其特征在于:所述的注入单元设置在塑化单元上且与原料形成熔融物的区域连通设置,用于向塑化单元内注入液态添加剂。A liquid additive assisted polymer extrusion and blending device, comprising a plasticizing unit and an injection unit for preparing the target product; characterized in that: the injection unit is arranged on the plasticizing unit and forms a melt with the raw material The area is connected and arranged for injecting liquid additives into the plasticizing unit.
所述的塑化单元包括螺筒、设置在螺筒内的螺杆以及设置在螺筒进料端的进料组件;其中,所述的螺筒靠近出料端设置有间隔排列的排气口;且该排气口与真空室分别连通设置,在负压区域形成负压区。The plasticizing unit includes a screw barrel, a screw arranged in the screw barrel, and a feed assembly arranged at the feeding end of the screw barrel; wherein the screw barrel is provided with spaced exhaust ports near the discharge end; and The exhaust port and the vacuum chamber are respectively connected and arranged to form a negative pressure zone in the negative pressure area.
所述的螺筒上设置有用于混合熔融物与液态添加剂的混合区域且该混合区域内设置有用于检测筒内压力和温度的传感器;真空室与外界的负压系统连通,并设置仪表检测真空室内压力。The screw barrel is provided with a mixing area for mixing the melt and the liquid additive, and the mixing area is provided with a sensor for detecting the pressure and temperature in the barrel; the vacuum chamber is connected with the external negative pressure system, and an instrument is set to detect the vacuum Room pressure.
所述的注入单元包括用于混合两种添加剂的配混装置、存储装置以及输送装置;其中,所述的配混装置的输出端与存储装置的输入端连接,用于通过管路定量的向输送装置输送混合后的添加剂;所述的输送装置的输出端与塑化单元内的原料形成熔融物的区域连通设置。The injection unit includes a compounding device, a storage device, and a conveying device for mixing two additives; wherein, the output end of the compounding device is connected with the input end of the storage device, and is used for quantitatively directing through a pipeline. The conveying device conveys the mixed additives; the output end of the conveying device is connected with the area where the raw material in the plasticizing unit forms a melt.
所述的配混装置包括料仓I、料仓II、容器、搅拌桨以及计量模块;其中,所述的料仓I和料仓II的输出端与容器的输入端连通;容器内设置有搅拌桨;容器底部设置有用于称重的计量模块;其中,所述的容器的输出端与存储 装置连接。The compounding device includes a silo I, a silo II, a container, a stirring paddle, and a metering module; wherein the output ends of the silo I and the silo II communicate with the input end of the container; the container is provided with a stirring Paddle; the bottom of the container is provided with a metering module for weighing; wherein the output end of the container is connected to the storage device.
所述的存储装置包括存储容器、搅拌器和计量单元;其中,存储容器的输入端与配混装置的输出端连接;存储容器内设置有搅拌器;存储容器的底部设置有用于称量的计量单元;其中,所述存储容器的输出端与输送装置的输入端连接。The storage device includes a storage container, a stirrer, and a weighing unit; wherein the input end of the storage container is connected with the output end of the compounding device; the storage container is provided with a stirrer; the bottom of the storage container is provided with a meter for weighing Unit; wherein the output end of the storage container is connected to the input end of the conveying device.
所述的输送装置包括高压计量泵;该高压计量泵的输入端与存储装置的输出端连接,该高压计量泵的输出端通过单向注液阀与塑化单元上的原料形成熔融物的区域连通。The delivery device includes a high-pressure metering pump; the input end of the high-pressure metering pump is connected to the output end of the storage device, and the output end of the high-pressure metering pump forms a region where a melt is formed by a one-way injection valve with the raw materials on the plasticizing unit Connected.
本发明的所述液态添加剂辅助聚合物挤出共混的方法的基本原理是:将耐溶剂的多相非稳态聚合物的原料混合物通过双螺杆挤出机加料口加入,经过螺杆作用输送、熔融和混合,在螺筒对应混合物变为熔融物的区域开孔,安装单向的注入单元,使该区域的熔融物完全充满螺槽和机筒之间的空隙,对应注液阀的螺旋推进结构等具体推进结构,使液态添加剂深入到熔融物内部;然后,将液态添加剂或非液态添加剂加入到溶剂中形成溶液或悬浮液,形成液态添加剂,通过具有计量功能和高压输送能力的泵及管路系统,将上述液态添加剂通过注入单元连续、定量的泵送到熔融物内部。由于压力作用,室温下的液态添加剂及溶剂在高温的熔融物中受热后不会立即汽化,而以过热状态存在,如水做溶剂时会以过热水即亚临界水形式存在。同时,在高速旋转的螺杆作用下,过热状态的添加剂和溶剂组分被均匀分散分布在熔融物中,随着螺杆输送向下游区域。在下游区域的螺筒上设置有不少于1个与大气或负压系统连接的排气口,使融合物的压力降低,添加剂中的溶剂汽化,从而顺利挤出成条,然后进行造粒。The basic principle of the liquid additive-assisted polymer extrusion and blending method of the present invention is: the raw material mixture of the solvent-resistant multiphase non-stable polymer is added through the feed port of the twin-screw extruder, and it is conveyed through the action of the screw. Melt and mix, open a hole in the area where the screw barrel corresponds to the mixture becoming molten, install a one-way injection unit, so that the molten material in this area completely fills the gap between the screw groove and the barrel, corresponding to the screw advancement of the injection valve The structure and other specific advancement structures make the liquid additive penetrate deep into the melt; then, the liquid additive or non-liquid additive is added to the solvent to form a solution or suspension to form a liquid additive, which is passed through a pump and tube with metering function and high-pressure delivery capability. The circuit system, the above-mentioned liquid additive is continuously and quantitatively pumped to the inside of the melt through the injection unit. Due to pressure, liquid additives and solvents at room temperature will not immediately vaporize after being heated in a high-temperature melt, but will exist in a superheated state. For example, when water is used as a solvent, they will exist in the form of superheated water, that is, subcritical water. At the same time, under the action of the high-speed rotating screw, the superheated additives and solvent components are evenly dispersed in the melt, and are transported to the downstream area with the screw. No less than one exhaust port connected to the atmosphere or negative pressure system is provided on the screw barrel in the downstream area to reduce the pressure of the fusion and vaporize the solvent in the additive, thereby smoothly extruding into a strip, and then granulating .
需要明确的是:亚临界水指:压力2.4MPa时,水沸点约220℃;压力2.9MPa 时,水沸点约230℃;压力4MPa时,水沸点约251℃;压力8MPa时,水沸点约300℃。What needs to be clear is: subcritical water refers to: when the pressure is 2.4MPa, the boiling point of water is about 220℃; when the pressure is 2.9MPa, the boiling point of water is about 230℃; when the pressure is 4MPa, the boiling point of water is about 251℃; when the pressure is 8MPa, the boiling point of water is about 300. ℃.
本发明还提供了一种如前述方案所述的液态添加剂辅助聚合物挤出共混的装置在生产聚合物上的应用。其中,聚合物包括低气味级聚合物或其它类型的聚合物。The present invention also provides an application of the liquid additive assisted polymer extrusion and blending device in the production of polymers as described in the foregoing solution. Among them, polymers include low-odor polymers or other types of polymers.
有益效果:本发明通过将添加剂加入到溶剂中形成液态添加剂,有助于降低熔融物内部的局部高温,使整体温度有一定降低并且更均匀,有益于组分的混合均匀性;并且,在螺杆的作用下,过热状态的液态添加剂和溶剂组分被均匀分散分布在原料形成的熔融物中;在输送到螺筒的后端时,汽化为溶剂蒸汽排出或被负压系统抽走,融合物发生大量的气泡破裂,增加界面更新效果,使融合物内部的残留单体和小分子组分被除去,获得气味感官较好的产品;甚至,对于极性表面的填料、增强体组分,本发明所述的方法还可以增加与基体的混溶性,改善在非极性基体中的分散分布和界面效果,从而提高产品的质量。液态添加剂蒸发散失过程产生大量气泡并破裂,增加融合物的混合效果。另外,对于受热易熔化的、受热易分解的以及受热易挥发的添加剂,借助溶剂将其液态化,可以在保证添加剂本身特性的基础上进行准确添加,且混合均匀。Beneficial effects: The present invention helps to reduce the local high temperature inside the melt by adding the additives to the solvent to form a liquid additive, so that the overall temperature is reduced to a certain extent and is more uniform, which is beneficial to the uniformity of the mixing of the components; Under the action of, the superheated liquid additives and solvent components are evenly dispersed in the melt formed by the raw materials; when transported to the rear end of the screw barrel, they vaporize as solvent vapor and are discharged or sucked away by the negative pressure system, and the fusion A large number of bubble bursts occurred, which increased the effect of interface renewal, so that the residual monomers and small molecular components in the fusion were removed, and products with better odor and sensory were obtained; even for fillers and reinforcement components on polar surfaces, the original The method of the invention can also increase the miscibility with the matrix, improve the dispersion distribution and the interface effect in the non-polar matrix, thereby improving the quality of the product. The evaporation and loss process of the liquid additive produces a large number of bubbles and bursts, which increases the mixing effect of the fusion. In addition, for the additives that are easily melted by heating, easily decomposed by heating, and easily volatile when heated, they can be liquefied with the help of solvents, which can be accurately added on the basis of ensuring the characteristics of the additives, and the mixing is uniform.
本发明装置结构简单,可直接在现有双螺旋杆挤出机上进行修改,改动量小,运行稳定,故障率低,产品质量稳定可靠,解决了现有技术中存在的问题。The device of the invention has simple structure, can be directly modified on the existing double screw extruder, has small modification amount, stable operation, low failure rate, stable and reliable product quality, and solves the problems existing in the prior art.
附图说明Description of the drawings
图1为本发明的结构示意图。Figure 1 is a schematic diagram of the structure of the present invention.
图2为液态添加剂辅助聚合物挤出共混的方法的流程图。Figure 2 is a flow chart of a method for liquid additive assisted polymer extrusion blending.
图3为两种添加剂混合时的流程图。Figure 3 is a flow chart when the two additives are mixed.
其中,图1中的1021所示的区域为原料未完全熔融的区域;1023所示的区域指过热状态的液态添加剂与熔融物状态的原料融合的区域。Among them, the area shown by 1021 in FIG. 1 is the area where the raw material is not completely melted; the area shown by 1023 refers to the area where the liquid additive in the superheated state and the raw material in the molten state are fused.
具体实施方式Detailed ways
下面将结合本发明实施例中的附图,对本发明实施例中的技术方案进行清楚、完整地描述。The technical solutions in the embodiments of the present invention will be clearly and completely described below in conjunction with the drawings in the embodiments of the present invention.
为了解决现有技术中在使用添加剂时容易发生汽化、分布不均而导致产品品质下降的问题,本发明提供一种液态添加剂辅助聚合物挤出共混的方法,其技术方案为:将原料混合物转化为熔融物后,再将液态添加剂连续注入至上述熔融物内部,使上述添加剂与上述熔融物充分融合形成均匀的融合物,最后进行脱水、脱挥,得到目标产物。In order to solve the problems in the prior art that vaporization and uneven distribution of additives are likely to occur when additives are used in the prior art, the product quality is reduced, the present invention provides a liquid additive assisted polymer extrusion blending method. After being converted into a molten material, the liquid additive is continuously injected into the molten material, so that the additive and the molten material are fully fused to form a uniform fusion, and finally dehydration and devolatilization are performed to obtain the target product.
上述的一种液态添加剂辅助聚合物挤出共混的方法,具体可以包括以下步骤:The above-mentioned method of liquid additive assisted polymer extrusion and blending may specifically include the following steps:
S1.将耐溶剂的多相非稳态聚合物的原料混合物通过双螺杆挤出机的加料口加入螺筒内,通过螺杆进行螺旋输送;S1. The raw material mixture of the solvent-resistant multiphase non-stable polymer is fed into the screw barrel through the feeding port of the twin-screw extruder, and the screw is conveyed through the screw;
S2.经过S1步骤,在螺筒内的熔融区形成S1步骤所述原料混合物的熔融物;S2. After step S1, a melt of the raw material mixture described in step S1 is formed in the melting zone in the barrel;
S3.在S2步骤所述的熔融区位置通过施压装置将待添加的液态添加剂连续、定量注入至该熔融区内,液态添加剂处于过热状态,通过螺杆作用与S2步骤所述的熔融物充分混合形成融合物;S3. At the position of the melting zone described in step S2, the liquid additive to be added is continuously and quantitatively injected into the melting zone through a pressure applying device. The liquid additive is in an overheated state and is fully mixed with the melt described in step S2 through the action of the screw Form a fusion;
S4.通过螺杆将S3步骤所述的融合物向前输送,并在螺筒下游使过热状态的液态添加剂汽化为溶剂蒸汽排出,融合物内气泡破裂,从而利用负压装置使融合物内部的残留单体和小分子组分被除去,完成脱水、脱挥;S4. The fusion described in step S3 is transported forward through the screw, and the superheated liquid additive is vaporized into solvent vapor downstream of the screw barrel, and the bubbles in the fusion burst, so that the negative pressure device is used to make the residue inside the fusion The monomer and small molecule components are removed, dehydration and devolatilization are completed;
S5.在螺筒的出料端得到目标产物。S5. Obtain the target product at the discharge end of the screw barrel.
其中,所述的液态添加剂注入熔融物内部后处于过热状态。Wherein, the liquid additive is in an overheated state after being injected into the melt.
其中,所述的液态添加剂为水或单一液态助剂或悬浊液或含有气态添加剂的液体;或者,所述的液态添加剂为水、单一液态助剂、悬浊液、含有气态添加剂的液体中的任两种的混合物。Wherein, the liquid additive is water or a single liquid additive or suspension or a liquid containing a gaseous additive; or, the liquid additive is water, a single liquid additive, a suspension, or a liquid containing a gaseous additive. A mixture of any two of them.
如果液态添加剂为单一液态助剂、悬浊液、含有气态添加剂的液体中的任两种的混合物时,其混合的过程如下:If the liquid additive is a mixture of any two of a single liquid additive, a suspension, and a liquid containing a gaseous additive, the mixing process is as follows:
A.依据配比将上述的两种液态添加剂分别加入各自的容器中;A. Add the above two liquid additives into their respective containers according to the ratio;
B.将上述两种液态添加剂输出至第一混配单元中,进行搅拌混合,同时进行第一次计量,得到一级混合液体;B. Output the above two liquid additives to the first mixing unit, stir and mix, and perform the first metering at the same time to obtain a first-level mixed liquid;
C.将S2步骤获得的一级混合液体输入至第二级混配单元中,得到第二级混合液体,再通过第二次计量,获得第二级混配单元输出的液体总量;C. Input the first-stage mixed liquid obtained in step S2 into the second-stage mixing unit to obtain the second-stage mixed liquid, and then pass the second metering to obtain the total amount of liquid output by the second-stage mixing unit;
其中,如果A步骤所述的两种液态添加剂中存在含有气态添加剂的液体,则对应的容器设置为密闭容器。Wherein, if there is a liquid containing a gaseous additive in the two liquid additives described in step A, the corresponding container is set as a closed container.
所述的单一液态助剂可以是阻燃剂或偶联剂或加工油;所述的悬浊液可以是粉体添加剂和溶液的混合物;其中,粉体添加剂可以是纳米填料、分散剂、着色剂、反应助剂中的任意一种或多种;其中,溶液可以是水或水-醇混合液;含有气态添加剂的液体可以是含有二氧化碳的水溶液或含有二氧化碳的水-醇溶液。The single liquid additive can be a flame retardant or a coupling agent or a processing oil; the suspension can be a mixture of a powder additive and a solution; wherein the powder additive can be a nano filler, a dispersant, or a coloring agent. Any one or more of reagents and reaction aids; wherein the solution can be water or a water-alcohol mixture; the liquid containing gaseous additives can be an aqueous solution containing carbon dioxide or a water-alcohol solution containing carbon dioxide.
所述的融合物进行脱水、脱挥的过程是:所述的融合物在输送到螺筒的后端时,由于螺筒的后端间隔排列有多个排气口且上述排气口均连接负压装置;结合螺杆作用,上述融合物发生大量的气泡破裂,完成融合物界面重组,同时破裂气泡产生的气体通过负压装置抽离螺筒,实现脱水、脱挥。The process of dehydration and devolatilization of the fusion is as follows: when the fusion is transported to the rear end of the screw barrel, since the rear end of the screw barrel is arranged with a plurality of exhaust ports and the above-mentioned exhaust ports are all connected Negative pressure device; combined with the action of the screw, a large number of bubbles in the above fusion material are broken to complete the interface reorganization of the fusion, and the gas generated by the broken bubbles is drawn out of the barrel through the negative pressure device to achieve dehydration and devolatilization.
如图1所示,一种液态添加剂辅助聚合物挤出共混的装置,包括用于制 备目标产物的塑化单元1和注入单元2,其中:As shown in Figure 1, a liquid additive assisted polymer extrusion and blending device includes a plasticizing unit 1 and an injection unit 2 for preparing the target product, in which:
优选的,该塑化单元1可以由现有的双螺旋杆挤出机改造而来,具体的,包括螺筒101、设置在螺筒101内的螺杆102以及设置在螺筒101进料端的进料组件;为了方便脱水、脱挥,上述的螺筒101靠近出料端设置有间隔排列的排气口1012,1013;且该排气口1012,1013与真空室107,109分别连通设置且该真空室107,109居于外界的真空系统相连,并设置负压仪表108,1010分别检测真空室107,109内压力。Preferably, the plasticizing unit 1 can be modified from an existing double screw extruder. Specifically, it includes a screw barrel 101, a screw 102 arranged in the screw barrel 101, and a feeding end arranged at the feeding end of the screw barrel 101. In order to facilitate dehydration and devolatilization, the above-mentioned screw barrel 101 is provided with spaced exhaust ports 1012, 1013 near the discharge end; and the exhaust ports 1012, 1013 and the vacuum chambers 107, 109 are respectively connected and arranged and the The vacuum chambers 107 and 109 are connected to the external vacuum system, and negative pressure meters 108 and 1010 are set to detect the pressure in the vacuum chambers 107 and 109 respectively.
重要的是,在上述的螺筒101上设置有用于混合熔融物与液态添加剂的混合区域1022且该混合区域1022内用于检测筒内压力和温度的压力传感器105和温度传感器106。What is important is that a mixing area 1022 for mixing the melt and liquid additives is provided on the above-mentioned screw barrel 101, and a pressure sensor 105 and a temperature sensor 106 for detecting the pressure and temperature in the barrel are provided in the mixing area 1022.
需要明确的是:上述的混合区域1022可以根据实际情况自行灵活设置。What needs to be clear is that the aforementioned mixing area 1022 can be flexibly set according to actual conditions.
其中,所述的注入单元2包括用于混合两种添加剂的配混装置201、存储装置202以及输送装置204;其中,所述的配混装置201的输出端与存储装置202的输入端连接,用于通过管路203定量的向输送装置204输送混合后的添加剂;所述的输送装置204的输出端与混合区域1022连通设置,用于将液态添加剂注入混合区域1022内的熔融物中,进一步混合,通过螺杆102的作用,形成均匀的融合物。Wherein, the injection unit 2 includes a compounding device 201 for mixing two additives, a storage device 202, and a conveying device 204; wherein, the output end of the compounding device 201 is connected to the input end of the storage device 202, It is used to quantitatively deliver the mixed additive to the delivery device 204 through the pipeline 203; the output end of the delivery device 204 is connected to the mixing area 1022 and is used to inject the liquid additive into the melt in the mixing area 1022, and further The mixing, through the action of the screw 102, forms a uniform fusion.
所述的输送装置204包括高压计量泵2041;该高压计量泵2041的输入端与存储装置202的输出端连接,该高压计量泵2041的输出端可以通过单向注液阀205与塑化单元1上的原料形成熔融物的区域连通。The delivery device 204 includes a high-pressure metering pump 2041; the input end of the high-pressure metering pump 2041 is connected to the output end of the storage device 202, and the output end of the high-pressure metering pump 2041 can be connected to the plasticizing unit 1 through the one-way injection valve 205 The areas where the raw materials form the melt are connected.
具体的,如果液态添加剂为两种液态添加剂或非液态添加剂与溶剂形成的溶液或悬浮液,则所述的配混装置201包括料仓I2011、料仓II2012、容器2013、搅拌桨2014以及计量模块2015;其中,所述的料仓I2011和料仓II2012 的输出端与容器2013的输入端连通;容器2013内设置有搅拌桨2014;容器2013底部设置有用于称重的计量模块2015;Specifically, if the liquid additive is a solution or suspension formed by two liquid additives or a non-liquid additive and a solvent, the compounding device 201 includes a silo I2011, a silo II2012, a container 2013, a stirring paddle 2014, and a metering module 2015; Wherein, the output ends of the silo I2011 and II2012 communicate with the input of the container 2013; the container 2013 is provided with a stirring paddle 2014; the bottom of the container 2013 is provided with a weighing module 2015 for weighing;
其中,所述的容器2013的输出端与存储装置202连接。Wherein, the output end of the container 2013 is connected to the storage device 202.
所述的存储装置202包括存储容器2021、搅拌器2022和计量单元2023;其中,存储容器2021的输入端与配混装置201的输出端连接;存储容器2021内设置有搅拌器2022;存储容器2021的底部设置有用于称量的计量单元2023;其中,所述存储容器2021的输出端与输送装置204的输入端连接;所述的输送装置204包括高压计量泵2041;该高压计量泵2041的输入端与存储装置202的输出端连接,该高压计量泵2041的输出端经调节阀2043将液态添加剂注入混合区域1022内的熔融物中。The storage device 202 includes a storage container 2021, a stirrer 2022, and a metering unit 2023; wherein the input end of the storage container 2021 is connected to the output end of the compounding device 201; the storage container 2021 is provided with a stirrer 2022; the storage container 2021 A metering unit 2023 for weighing is provided at the bottom of the, wherein the output end of the storage container 2021 is connected to the input end of the conveying device 204; the conveying device 204 includes a high-pressure metering pump 2041; the input of the high-pressure metering pump 2041 The end is connected with the output end of the storage device 202, and the output end of the high-pressure metering pump 2041 injects the liquid additive into the melt in the mixing zone 1022 through the regulating valve 2043.
为了保证安全,高压计量泵2041的输出端还并联设置有泄压管和安全阀2042构成泄压管路,用于在高压计量泵2041内压力过高时,进行泄压,保证管路系统安全。In order to ensure safety, the output end of the high-pressure metering pump 2041 is also provided with a pressure relief pipe and a safety valve 2042 in parallel to form a pressure relief pipeline, which is used to relieve the pressure when the pressure in the high-pressure metering pump 2041 is too high to ensure the safety of the pipeline system .
在工作过程中,计量喂料装置103将物料104加入到螺筒101中,在螺杆102的作用下向前输送,物料经螺杆102的作用在混合区域1022塑化熔融形成熔融物,并在螺杆102的作用下在混合区域1022形成一定的压力。多组分的添加剂分别置于料仓I2011和料仓II2012中,按比例加入配混的容器2013中,在搅拌桨2014作用下配混成均一混合物,计量模块2015用以指示添加剂比例和混合物重量。将上述均一的混合物输送至存储配混添加剂的存储容器2021中,在搅拌器2022作用下保持均一,计量单元2023指示添加剂混合物重量。经存储装置202中的添加剂混合物经输送管路203输送至高压计量泵2041,高压计量泵2041定量将添加剂混合物输出至混合区域1022,保证将液态添加剂注入熔融物内部,高压计量泵2041的输出端可以设置压力传感器206,采集添加剂混 合物注入挤出机内的熔融物时的内部压力,另外,压力过高时,泄压管上的安全阀2042触发保护作用。添加剂和熔融物的混合物料在混合区域1022通过螺杆102的作用下混合形成均一的融合物。经过螺杆102输送,上述融合物移动至排气口1012,1013区域,融合物中的水、挥发分等被真空系统抽离,直至添加了添加剂的融合物被螺杆102输送至造粒单元。In the working process, the metering feeding device 103 adds the material 104 to the screw barrel 101 and conveys it forward under the action of the screw 102. The material is plasticized and melted in the mixing area 1022 by the screw 102 to form a melt, and then Under the action of 102, a certain pressure is formed in the mixing area 1022. The multi-component additives are respectively placed in the silo I2011 and the silo II2012, are added to the compounding container 2013 in proportion, and are compounded into a uniform mixture under the action of the stirring paddle 2014. The metering module 2015 is used to indicate the additive ratio and the weight of the mixture. The above-mentioned uniform mixture is transported to the storage container 2021 for storing and compounding additives, and is kept uniform under the action of the agitator 2022, and the metering unit 2023 indicates the weight of the additive mixture. The additive mixture in the storage device 202 is transported to the high-pressure metering pump 2041 through the delivery pipeline 203. The high-pressure metering pump 2041 quantitatively outputs the additive mixture to the mixing area 1022 to ensure that the liquid additive is injected into the melt. The output end of the high-pressure metering pump 2041 A pressure sensor 206 can be provided to collect the internal pressure when the additive mixture is injected into the melt in the extruder. In addition, when the pressure is too high, the safety valve 2042 on the pressure relief pipe triggers a protective effect. The mixture of the additives and the melt is mixed under the action of the screw 102 in the mixing zone 1022 to form a uniform fusion. After being conveyed by the screw 102, the aforesaid fusion is moved to the exhaust ports 1012, 1013 area, and the water and volatiles in the fusion are evacuated by the vacuum system until the fusion with additives is conveyed to the granulation unit by the screw 102.
具体实施例1:本实施例提供了使用单一的水作为添加剂的实施例,即水辅助聚合物挤出共混的方法,用以改善产品的气味,生产低气味的高等级产品。Specific Example 1: This example provides an example using a single water as an additive, that is, a water-assisted polymer extrusion blending method to improve the odor of the product and produce a low-odor high-grade product.
具体的,如图1~3,计量喂料装置103将物料104加入到螺筒101中,在螺杆102的作用下向前输送,物料经螺杆102的作用在混合区域1022塑化熔融形成熔融物,并在螺杆102的作用下在混合区域1022形成一定的压力。多组分的添加剂分别置于料仓I2011和料仓II2012中,按比例加入配混的容器2013中,在搅拌桨2014作用下配混成均一混合物,计量模块2015用以指示添加剂比例和混合物重量。将上述均一的混合物输送至存储配混添加剂的存储容器2021中,在搅拌器2022作用下保持均一,计量单元2023指示添加剂混合物重量。经存储装置202中的添加剂混合物经输送管路203输送至高压计量泵2041,高压计量泵2041定量将添加剂混合物输出至混合区域1022,保证将液态添加剂注入熔融物内部,高压计量泵2041的输出端可以设置压力传感器206,采集添加剂混合物注入挤出机内的熔融物时的内部压力,另外,压力过高时,泄压管上的安全阀2042触发泄压保护功能。添加剂和熔融物的混合物料在混合区域1022通过螺杆102的作用下混合形成均一的融合物。经过螺杆102输送,上述融合物移动至排气口1012,1013区域,融合物中的水、挥发分等被真空系统抽离,直至添加了添加剂的融合物被螺杆102输送至造粒单元。在本实施例中,通过将水定量注入熔融物内部的方法,通过螺杆102的螺旋剪切作用将过热水 与熔融物分散均匀,再通过排气口1012,1013将水汽化并携带融合物中的挥发分物质排出,实现脱挥,获得高等级的低气味产品。Specifically, as shown in Figures 1 to 3, the metering feeding device 103 adds the material 104 to the screw barrel 101 and conveys it forward under the action of the screw 102. The material is plasticized and melted in the mixing area 1022 by the screw 102 to form a melt. , And under the action of the screw 102, a certain pressure is formed in the mixing area 1022. The multi-component additives are respectively placed in the silo I2011 and the silo II2012, are added to the compounding container 2013 in proportion, and are compounded into a uniform mixture under the action of the stirring paddle 2014. The metering module 2015 is used to indicate the additive ratio and the weight of the mixture. The above-mentioned uniform mixture is transported to the storage container 2021 for storing and compounding additives, and is kept uniform under the action of the agitator 2022, and the metering unit 2023 indicates the weight of the additive mixture. The additive mixture in the storage device 202 is transported to the high-pressure metering pump 2041 through the delivery pipeline 203. The high-pressure metering pump 2041 quantitatively outputs the additive mixture to the mixing area 1022 to ensure that the liquid additive is injected into the melt. The output end of the high-pressure metering pump 2041 A pressure sensor 206 can be provided to collect the internal pressure when the additive mixture is injected into the melt in the extruder. In addition, when the pressure is too high, the safety valve 2042 on the pressure relief pipe triggers the pressure relief protection function. The mixture of the additives and the melt is mixed under the action of the screw 102 in the mixing zone 1022 to form a uniform fusion. After being conveyed by the screw 102, the aforesaid fusion is moved to the exhaust ports 1012, 1013 area, and the water and volatiles in the fusion are evacuated by the vacuum system until the fusion with additives is conveyed to the granulation unit by the screw 102. In this embodiment, through the method of quantitatively injecting water into the melt, the superheated water and the melt are evenly dispersed through the spiral shear action of the screw 102, and then the water is vaporized and the fusion is carried through the exhaust ports 1012 and 1013. The volatile matter in the medium is discharged to achieve devolatilization, and a high-grade low-odor product can be obtained.
具体实施例2:与实施例1相比,本实施例的主要区别在于:使用单一液态助剂,如阻燃剂、偶联剂、加工油等作为添加剂,获得更好的物料混合效果。Specific embodiment 2: Compared with embodiment 1, the main difference of this embodiment is that a single liquid auxiliary agent, such as a flame retardant, a coupling agent, a processing oil, etc., is used as an additive to obtain a better material mixing effect.
如图1~3,本液态助剂和实施例1中的水的方式添加类似,主要在于解决这些液态添加剂常规与物料混合后加入挤出机加工的困难和风险,如与物料混合不均匀、混合后结块、液态助剂挥发、液态助剂有气味、热敏感助剂提前分解、环境问题等,将液态添加剂单独计量注入聚合物熔融物内部,进行充分混合,实现混合效果均匀、产品品质稳定、操作方便,能够进一步降低产品的气味,实现高等级低气味级产品的生产。As shown in Figures 1 to 3, the method of adding the liquid additives is similar to that of the water in Example 1. The main purpose is to solve the difficulties and risks of adding these liquid additives to the extruder after being conventionally mixed with materials, such as uneven mixing with materials, After mixing, agglomeration, volatilization of liquid additives, smell of liquid additives, premature decomposition of heat-sensitive additives, environmental problems, etc., the liquid additives are separately metered into the polymer melt and fully mixed to achieve uniform mixing effect and product quality Stable and easy to operate, it can further reduce the odor of the product and realize the production of high-grade and low-odor products.
本实施例的其它特征与实施例1相同,不再赘述。The other features of this embodiment are the same as those of Embodiment 1, and will not be repeated here.
具体实施例3:与实施例1和实施例2相比,本实施例的主要区别在于:使用粉体添加剂,如纳米填料、分散剂、着色剂、反应助剂等和液体,如水、水-醇混合液等,构成的悬浊液作为添加剂,即将粉体添加剂变为液态添加剂辅助聚合物挤出共混的方法。Specific embodiment 3: Compared with embodiment 1 and embodiment 2, the main difference of this embodiment lies in the use of powder additives, such as nano fillers, dispersants, colorants, reaction aids, etc., and liquids, such as water, water- A method in which a suspension composed of an alcohol mixture and the like is used as an additive, that is, a powder additive is turned into a liquid additive to assist the extrusion and blending of a polymer.
本实施例中,如图1~3,将添加剂和液态辅助添加剂分别加入到料仓I2011和料仓II2012中,按比例加入用于配混的容器2013,在搅拌桨2014作用下配混成均一混合物,计量模块2015用以指示添加剂比例和混合物重量,经配混装置201配混均一的混合物输送至存储配混添加剂的存储容器2021,在搅拌器2022作用下保持均一,计量单元2023指示添加剂混合物重量,后存储装置202中的添加剂混合物经输送管路203输送至输送装置204。本实施例的其它特征与实施例1和2相同,不再赘述。In this embodiment, as shown in Figures 1 to 3, the additives and the liquid auxiliary additives are added to the silo I2011 and the silo II2012 respectively, and the container 2013 for compounding is added in proportion to the mixing paddle 2014 to form a homogeneous mixture. , The metering module 2015 is used to indicate the proportion of additives and the weight of the mixture. The uniform mixture is mixed by the compounding device 201 and transported to the storage container 2021 for storing the compounded additives. The uniformity is maintained under the action of the stirrer 2022. The metering unit 2023 indicates the weight of the additive mixture , The additive mixture in the rear storage device 202 is delivered to the delivery device 204 via the delivery pipeline 203. The other features of this embodiment are the same as those of Embodiments 1 and 2, and will not be repeated.
本实施例主要解决少量粉体添加剂如纳米填料、色粉难以在熔融物中充 分分散的情况,并解决常规混料时少量添加剂与物料混合不均匀造成共混挤出产品质量波动等问题。少量粉体添加剂使用液态添加剂作为载体,单独计量注入聚合物熔体内部,进行充分混合,实现混合效果均匀、产品品质稳定、操作方便,能够进一步降低产品的气味,实现高等级低气味级产品等聚合物的生产。This embodiment mainly solves the problem that a small amount of powder additives such as nano fillers and toners are difficult to be fully dispersed in the melt, and solves the problem of uneven mixing of a small amount of additives and materials during conventional mixing, resulting in fluctuations in the quality of blended and extruded products. A small amount of powder additives use liquid additives as a carrier, separately metered into the polymer melt, and fully mixed to achieve uniform mixing effect, stable product quality, and convenient operation, which can further reduce product odor and realize high-grade low-odor products, etc. Production of polymers.
具体实施例4:与实施例1、2和3相比,本实施例的主要区别在于:使用气态添加剂,如二氧化碳和液体,如水、水-醇混合液等,构成的溶液作为添加剂,即将气态添加剂变为液态添加剂辅助聚合物挤出共混的方法。Specific embodiment 4: Compared with embodiments 1, 2 and 3, the main difference of this embodiment lies in the use of gaseous additives, such as carbon dioxide and liquids, such as water, water-alcohol mixtures, etc., as additives, that is, gaseous additives Additives become liquid additives to assist polymer extrusion blending methods.
本实施例中,如图1~3,将气态添加剂和液态辅助添加剂分别加入到可密闭保压的料仓I2011和料仓II2012,按比例加入配混容器2013,在搅拌桨2014作用下气体溶解在液体中,配混成一定气体溶解度的均一混合物,计量模块2015用以采集添加剂比例和混合物重量,经可密闭保压的配混装置201配混为均一的混合物,输送至密闭保压的存储容器2021,计量单元2023指示添加剂混合物重量。经可密闭保压的存储装置202中的添加剂混合物经输送管路203输送至输送装置204。本实施例的其它特征与实施例1、2和3相同,不再赘述。In this embodiment, as shown in Figures 1 to 3, gaseous additives and liquid auxiliary additives are added to the airtight and pressure-keeping silo I2011 and II2012 respectively, and are added to the mixing container 2013 in proportion, and the gas is dissolved under the action of the stirring paddle 2014 In the liquid, it is compounded into a homogeneous mixture with a certain gas solubility. The metering module 2015 is used to collect the proportion of additives and the weight of the mixture, mix it into a homogeneous mixture through the sealing and pressure-keeping compounding device 201, and transport it to a sealed and pressure-keeping storage container In 2021, the metering unit 2023 indicates the weight of the additive mixture. The additive mixture in the storage device 202 that can be sealed and pressure-maintained is delivered to the delivery device 204 via the delivery pipeline 203. Other features of this embodiment are the same as those of Embodiments 1, 2 and 3, and will not be repeated here.
本实施例主要解决气态添加剂,如二氧化碳,在熔融物中难以添加并且难以充分分散的问题,通过控制溶解度,使其借助液态辅助添加剂作为载体准确计量注入聚合物熔体内部,进行充分混合,实现对物料中的挥发分进一步携带、气提,进一步降低产品的气味,实现高等级低气味级产品的生产。This embodiment mainly solves the problem that gaseous additives, such as carbon dioxide, are difficult to add in the melt and are difficult to fully disperse. By controlling the solubility, it can be accurately metered and injected into the polymer melt with the aid of the liquid auxiliary additive as a carrier for full mixing. The volatile matter in the material is further carried and gas stripped to further reduce the odor of the product and realize the production of high-grade and low-odor products.
需要明确的是:本文所述的计量模块2015和计量单元2023可以是压力传感器;所述的搅拌桨2014和搅拌器2022可以具有相同的结构。It should be clarified that: the metering module 2015 and the metering unit 2023 described herein may be pressure sensors; the agitating paddle 2014 and the agitator 2022 may have the same structure.
需要明确的是:本文所述的单一液态助剂可以是水性液态助剂。What needs to be clear is that the single liquid additive described herein can be an aqueous liquid additive.
以上所述,仅为本发明的具体实施方式,但本发明的保护范围并不局限于此,任何熟悉本技术领域的技术人员在本发明揭露的技术范围内,可轻易变 化或替换,都属于本发明的保护范围之内。因此本发明的保护范围所述以权利要求的保护范围为准。The above are only specific embodiments of the present invention, but the protection scope of the present invention is not limited to this. Anyone familiar with the technical field can easily change or replace within the technical scope disclosed by the present invention. Within the protection scope of the present invention. Therefore, the protection scope of the present invention is subject to the protection scope of the claims.

Claims (19)

  1. 一种液态添加剂辅助聚合物挤出共混的方法,其特征在于:将原料混合物转化为熔融物后,将液态添加剂连续注入至上述熔融物内部,使上述添加剂与上述熔融物充分融合形成均匀的融合物,最后进行脱水、脱挥,得到目标产物。A liquid additive assisted polymer extrusion blending method is characterized in that: after the raw material mixture is converted into a melt, the liquid additive is continuously injected into the melt, so that the additive and the melt are fully fused to form a uniform The fusion is finally dehydrated and devolatilized to obtain the target product.
  2. 根据权利要求1所述的一种液态添加剂辅助聚合物挤出共混的方法,其特征在于:包括以下步骤:A method of liquid additive assisted polymer extrusion blending according to claim 1, characterized in that it comprises the following steps:
    S1.将耐溶剂的多相非稳态聚合物的原料混合物通过双螺杆挤出机的加料口加入螺筒内,通过螺杆进行螺旋输送;S1. The raw material mixture of the solvent-resistant multiphase non-stable polymer is fed into the screw barrel through the feeding port of the twin-screw extruder, and the screw is conveyed through the screw;
    S2.经过S1步骤,在螺筒内的熔融区形成S1步骤所述原料混合物的熔融物;S2. After step S1, a melt of the raw material mixture described in step S1 is formed in the melting zone in the barrel;
    S3.在S2步骤所述的熔融区位置通过施压装置将待添加的液态添加剂连续、定量注入至该熔融区内,液态添加剂处于过热状态,通过螺杆作用与S2步骤所述的熔融物充分混合形成融合物;S3. At the position of the melting zone described in step S2, the liquid additive to be added is continuously and quantitatively injected into the melting zone through a pressure applying device. The liquid additive is in an overheated state and is fully mixed with the melt described in step S2 through the action of the screw Form a fusion;
    S4.通过螺杆将S3步骤所述的融合物向前输送,并在螺筒下游使过热状态的液态添加剂汽化为溶剂蒸汽排出,融合物内气泡破裂,从而利用负压装置使融合物内部的残留单体和小分子组分被除去,完成脱水、脱挥;S4. The fusion described in step S3 is transported forward through the screw, and the superheated liquid additive is vaporized into solvent vapor downstream of the screw barrel, and the bubbles in the fusion burst, so that the negative pressure device is used to make the residue inside the fusion The monomer and small molecule components are removed, dehydration and devolatilization are completed;
    S5.在螺筒的出料端得到目标产物。S5. Obtain the target product at the discharge end of the screw barrel.
  3. 根据权利要求1所述的一种液态添加剂辅助聚合物挤出共混的方法,其特征在于:所述的液态添加剂注入熔融物内部后处于过热状态。The method for extrusion and blending of a liquid additive-assisted polymer according to claim 1, wherein the liquid additive is in an overheated state after being injected into the melt.
  4. 根据权利要求1或2所述的一种液态添加剂辅助聚合物挤出共混的方法,其特征在于:所述的液态添加剂为水或单一液态助剂或悬浊液或含有气态添加剂的液体;The method of liquid additive assisted polymer extrusion blending according to claim 1 or 2, wherein the liquid additive is water or a single liquid additive or suspension or a liquid containing gaseous additives;
    或者,所述的液态添加剂为水、单一液态助剂、悬浊液、含有气态添加剂的液体中的任两种的混合物。Alternatively, the liquid additive is a mixture of any two of water, a single liquid additive, a suspension, and a liquid containing a gaseous additive.
  5. 根据权利要求4所述的一种液态添加剂辅助聚合物挤出共混的方法,其特征 在于:如果液态添加剂为单一液态助剂、悬浊液、含有气态添加剂的液体中的任两种的混合物时,其混合的过程如下:The method for extrusion and blending of a liquid additive assisted polymer according to claim 4, characterized in that: if the liquid additive is a mixture of any two of a single liquid additive, a suspension, and a liquid containing a gaseous additive When, the mixing process is as follows:
    A.依据配比将上述的两种液态添加剂分别加入各自的容器中;A. Add the above two liquid additives into their respective containers according to the ratio;
    B.将上述两种液态添加剂输出至第一混配单元中,进行搅拌混合,同时进行第一次计量,得到一级混合液体;B. Output the above two liquid additives to the first mixing unit, stir and mix, and perform the first metering at the same time to obtain a first-level mixed liquid;
    C.将S2步骤获得的一级混合液体输入至第二级混配单元中,得到第二级混合液体,再通过第二次计量,获得第二级混配单元输出的液体总量;C. Input the first-stage mixed liquid obtained in step S2 into the second-stage mixing unit to obtain the second-stage mixed liquid, and then pass the second metering to obtain the total amount of liquid output by the second-stage mixing unit;
    其中,如果A步骤所述的两种液态添加剂中存在含有气态添加剂的液体,则对应的容器设置为密闭容器。Wherein, if there is a liquid containing a gaseous additive in the two liquid additives described in step A, the corresponding container is set as a closed container.
  6. 根据权利要求4或5所述的一种液态添加剂辅助聚合物挤出共混的方法,其特征在于:所述的单一液态助剂为阻燃剂或偶联剂或加工油。A liquid additive assisted polymer extrusion blending method according to claim 4 or 5, wherein the single liquid additive is a flame retardant or a coupling agent or a processing oil.
  7. 根据权利要求4或5所述的一种液态添加剂辅助聚合物挤出共混的方法,其特征在于:所述的悬浊液为粉体添加剂和溶液的混合物;The method of liquid additive assisted polymer extrusion blending according to claim 4 or 5, wherein the suspension is a mixture of powder additive and solution;
    其中,粉体添加剂为纳米填料、分散剂、着色剂、反应助剂中的任意一种或多种;Among them, the powder additives are any one or more of nano fillers, dispersants, colorants, and reaction aids;
    其中,溶液为水或水-醇混合液。Among them, the solution is water or a water-alcohol mixture.
  8. 根据权利要求4或5所述的一种液态添加剂辅助聚合物挤出共混的方法,其特征在于:含有气态添加剂的液体为含有二氧化碳的水溶液或含有二氧化碳的水-醇溶液。The method for extrusion and blending of a liquid additive-assisted polymer according to claim 4 or 5, wherein the liquid containing the gaseous additive is an aqueous solution containing carbon dioxide or a water-alcohol solution containing carbon dioxide.
  9. 根据权利要求1或2所述的一种液态添加剂辅助聚合物挤出共混的方法,其特征在于:所述的融合物进行脱水、脱挥的过程是:The method of liquid additive assisted polymer extrusion blending according to claim 1 or 2, wherein the process of dehydrating and devolatilizing the fusion is:
    所述的融合物在输送到螺筒的后端时,由于螺筒的后端间隔排列有多个排气口且上述排气口均连接负压装置;结合螺杆作用,上述融合物发生大量的气泡破 裂,完成融合物界面重组,同时破裂气泡产生的气体通过负压装置抽离螺筒,实现脱水、脱挥。When the fusion is delivered to the rear end of the screw barrel, since the rear end of the screw barrel is arranged with multiple exhaust ports and the exhaust ports are all connected to a negative pressure device; combined with the action of the screw, a large amount of the fusion occurs The bubble bursts to complete the reorganization of the fusion interface, and at the same time the gas generated by the burst bubble is drawn out of the screw barrel through the negative pressure device to achieve dehydration and devolatilization.
  10. 根据权利要求1或2所述的一种液态添加剂辅助聚合物挤出共混的方法在生产低气味级产品上的应用。The application of a liquid additive-assisted polymer extrusion blending method according to claim 1 or 2 in the production of low-odor products.
  11. 一种液态添加剂辅助聚合物挤出共混的装置,包括用于制备目标产物的塑化单元(1)和注入单元(2);其特征在于:所述的注入单元(2)设置在塑化单元(1)上且与原料形成熔融物的区域连通设置,用于向塑化单元(1)内注入液态添加剂。A liquid additive assisted polymer extrusion and blending device, comprising a plasticizing unit (1) and an injection unit (2) for preparing the target product; it is characterized in that: the injection unit (2) is set in the plasticizing unit (2) The unit (1) is provided in communication with the area where the raw material forms a melt, and is used for injecting liquid additives into the plasticizing unit (1).
  12. 根据权利要求11所述的一种液态添加剂辅助聚合物挤出共混的装置,其特征在于:所述的塑化单元(1)包括螺筒(101)、设置在螺筒(101)内的螺杆(102)以及设置在螺筒(101)进料端的进料组件;A liquid additive-assisted polymer extrusion and blending device according to claim 11, characterized in that: the plasticizing unit (1) comprises a screw barrel (101), and a screw barrel (101) arranged in the screw barrel (101). The screw (102) and the feed assembly arranged at the feed end of the screw barrel (101);
    其中,所述的螺筒(101)靠近出料端设置有间隔排列的排气口(1012,1013);且该排气口(1012,1013)与真空室(107,109)分别连通设置。Wherein, the screw barrel (101) is provided with spaced exhaust ports (1012, 1013) near the discharge end; and the exhaust ports (1012, 1013) are connected with the vacuum chamber (107, 109) respectively.
  13. 根据权利要求12所述的一种液态添加剂辅助聚合物挤出共混的装置,其特征在于:螺筒(101)上设置有用于混合熔融物与液态添加剂的混合区域(1022)且该混合区域(1022)内设置有用于检测筒内压力和温度的传感器;真空室(107,109)与外界的负压系统连通,并设置仪表检测真空室(107,109)内压力。A liquid additive-assisted polymer extrusion and blending device according to claim 12, characterized in that: the screw barrel (101) is provided with a mixing zone (1022) for mixing the melt and the liquid additive, and the mixing zone (1022) is provided with a sensor for detecting the pressure and temperature in the cylinder; the vacuum chamber (107, 109) is connected with an external negative pressure system, and an instrument is set to detect the pressure in the vacuum chamber (107, 109).
  14. 根据权利要求11所述的一种液态添加剂辅助聚合物挤出共混的装置,其特征在于:注入单元(2)包括用于混合两种添加剂的配混装置(201)、存储装置(202)以及输送装置(204);A liquid additive assisted polymer extrusion blending device according to claim 11, characterized in that: the injection unit (2) comprises a compounding device (201) and a storage device (202) for mixing two additives And the conveying device (204);
    其中,所述的配混装置(201)的输出端与存储装置(202)的输入端连接,用于通过管路(203)定量的向输送装置(204)输送混合后的添加剂;所述的输送装置(204)的输出端与塑化单元(1)内的原料形成熔融物的区域连通设置。Wherein, the output end of the compounding device (201) is connected with the input end of the storage device (202), and is used to quantitatively deliver the mixed additive to the delivery device (204) through the pipeline (203); The output end of the conveying device (204) is connected to the area where the raw material in the plasticizing unit (1) forms a melt.
  15. 根据权利要求14所述的一种液态添加剂辅助聚合物挤出共混的装置,其特征在于:所述的配混装置(201)包括料仓I(2011)、料仓II(2012)、容器(2013)、搅拌桨(2014)以及计量模块(2015);A liquid additive assisted polymer extrusion and blending device according to claim 14, characterized in that: the compounding device (201) comprises silo I (2011), silo II (2012), container (2013), stirring paddle (2014) and metering module (2015);
    其中,所述的料仓I(2011)和料仓II(2012)的输出端与容器(2013)的输入端连通;容器(2013)内设置有搅拌桨(2014);容器(2013)底部设置有用于称重的计量模块(2015);Wherein, the output ends of the silo I (2011) and the silo II (2012) are connected with the input end of the container (2013); the container (2013) is provided with a stirring paddle (2014); the container (2013) is provided at the bottom There is a metering module for weighing (2015);
    其中,所述的容器(2013)的输出端与存储装置(202)连接。Wherein, the output end of the container (2013) is connected to the storage device (202).
  16. 根据权利要求14所述的一种液态添加剂辅助聚合物挤出共混的装置,其特征在于:所述的存储装置(202)包括存储容器(2021)、搅拌器(2022)和计量单元(2023);A liquid additive assisted polymer extrusion blending device according to claim 14, characterized in that: the storage device (202) comprises a storage container (2021), a stirrer (2022) and a metering unit (2023) );
    其中,存储容器(2021)的输入端与配混装置(201)的输出端连接;存储容器(2021)内设置有搅拌器(2022);存储容器(2021)的底部设置有用于称量的计量单元(2023);Among them, the input end of the storage container (2021) is connected with the output end of the compounding device (201); the storage container (2021) is provided with a stirrer (2022); the bottom of the storage container (2021) is provided with a meter for weighing Unit (2023);
    其中,所述存储容器(2021)的输出端与输送装置(204)的输入端连接。Wherein, the output end of the storage container (2021) is connected to the input end of the conveying device (204).
  17. 根据权利要求14所述的一种液态添加剂辅助聚合物挤出共混的装置,其特征在于:所述的输送装置(204)包括高压计量泵(2041);A liquid additive assisted polymer extrusion and blending device according to claim 14, characterized in that: the delivery device (204) comprises a high-pressure metering pump (2041);
    该高压计量泵(2041)的输入端与存储装置(202)的输出端连接,该高压计量泵(2041)的输出端通过单向注液阀(205)与塑化单元(1)上的原料形成熔融物的区域连通。The input end of the high-pressure metering pump (2041) is connected to the output end of the storage device (202), and the output end of the high-pressure metering pump (2041) is connected to the raw material on the plasticizing unit (1) through the one-way injection valve (205) The areas where the melt is formed are connected.
  18. 根据权利要求17所述的一种液态添加剂辅助聚合物挤出共混的装置,其特征在于:高压计量泵(2041)的输出端还并联设置有泄压管路。A liquid additive assisted polymer extrusion and blending device according to claim 17, characterized in that the output end of the high-pressure metering pump (2041) is also provided with a pressure relief pipeline in parallel.
  19. 一种如权利要求11至18任一权利要求所述的液态添加剂辅助聚合物挤出共混的装置在生产聚合物上的应用。An application of the liquid additive assisted polymer extrusion blending device according to any one of claims 11 to 18 in the production of polymers.
PCT/CN2020/093191 2020-05-26 2020-05-29 Liquid additive assisted polymer extrusion and blending method and device and use thereof WO2021237655A1 (en)

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