CN110614732A - High-performance processing technology and equipment for supercritical fluid micro-explosion disentanglement of polymer - Google Patents
High-performance processing technology and equipment for supercritical fluid micro-explosion disentanglement of polymer Download PDFInfo
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C49/00—Blow-moulding, i.e. blowing a preform or parison to a desired shape within a mould; Apparatus therefor
- B29C49/071—Preforms or parisons characterised by their configuration, e.g. geometry, dimensions or physical properties
-
- 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
- B29B11/00—Making preforms
- B29B11/06—Making preforms by moulding the material
- B29B11/10—Extrusion moulding
-
- 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
- B29B11/00—Making preforms
- B29B11/14—Making preforms characterised by structure or composition
-
- 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
-
- 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
- B29B9/12—Making granules characterised by structure or composition
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/14—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor characterised by the particular extruding conditions, e.g. in a modified atmosphere or by using vibration
- B29C48/144—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor characterised by the particular extruding conditions, e.g. in a modified atmosphere or by using vibration at the plasticising zone
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C2949/00—Indexing scheme relating to blow-moulding
- B29C2949/07—Preforms or parisons characterised by their configuration
- B29C2949/0715—Preforms or parisons characterised by their configuration the preform having one end closed
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29K—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR MOULDS, REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
- B29K2027/00—Use of polyvinylhalogenides or derivatives thereof as moulding material
- B29K2027/06—PVC, i.e. polyvinylchloride
Abstract
The invention discloses a supercritical fluid micro-explosion unwinding polymer high-performance processing technology and equipment, which utilizes supercritical fluid to immerse into a molecular chain group, conduct orientation on the chain section while conducting micro-explosion unwinding on the single molecular chain group, and conduct secondary orientation and gas discharge while keeping the orientation effect after micro-explosion in a mode of mixing and exhausting; completely orienting the chain groups in the materials by matching with a laminating process to obtain a woven structure material; the resulting reinforced material is free of air bubbles. The equipment comprises a drying system, a dipping system, a micro-explosion system, an exhaust extrusion system, a temperature control system and other basic systems. The processing technology and equipment can continuously, efficiently and inexpensively utilize a supercritical fluid micro-explosion mode to unwind the high polymer chain groups/primary particles, keep the chain segments which are already subjected to micro-explosion orientation to smoothly enter the next stage for orientation through a mechanical exhaust mode, combine the lamination extrusion technology to form a material which has higher orientation degree and orderly arranged molecular chains and does not contain bubbles, and optimize the use performance of the high polymer.
Description
Technical Field
The invention relates to the field of processing and forming and advanced manufacturing of high polymer materials, in particular to a high-performance processing technology and equipment for a supercritical fluid micro-explosion disentanglement polymer.
Background
In the polymerization process, the macroscopic molecular chain of the amorphous high molecular polymer is bent under the action of rotation in the chain link, so that a macroscopic structure in the forms of random coils, chain links, chain balls and the like is formed; during application, it is often desirable to obtain an oriented or woven isotactic structure or an aligned structure to enhance the performance of the article. The existing processing modes of high polymers, such as mixing, uniaxial stretching, biaxial stretching and the like, can achieve certain effects in the processing of materials, but the processing modes of the high polymers are still chain segment orientation rather than molecular chain orientation for part of materials, such as PVC and the like, and part of chain segments still exist in an agglomerated form, so that the physical properties of the high polymers cannot be completely reflected macroscopically. In contrast, it is important to completely open the polymer molecular chain or long chain segment, which is not easily opened in the conventional processing method, and then further orient the polymer molecular chain or long chain segment.
Supercritical fluids typically take on a variety of forms, gaseous, liquid and solid, when the pressure and temperature are different. Particularly, supercritical carbon dioxide has very unique physicochemical properties, and has the characteristics of large diffusion coefficient, small viscosity and the like in a supercritical state. Because of higher diffusivity, the mass transfer resistance is reduced, the method is particularly favorable for extracting porous loose solid substances and compounds in cell materials, and the impregnation effect is better; and because it is particularly sensitive to operating conditions (e.g., pressure, temperature), this provides convenience for flexibility and adjustability of operation; meanwhile, the composite material has low chemical activity and toxicity, stable chemical performance, greenness and safety. Therefore, the supercritical fluid has wide application in the aspects of polymer material forming and biological material processing.
In the molding of polymer materials, supercritical fluids are generally used as blowing agents to mold foamed materials. The foaming process has better advantage of light weight of the product, but also reduces the original strength of the product. Typical foaming includes both direct foaming and batch foaming. The direct foaming is to mix supercritical fluid into melted high polymer melt, then release pressure to expand, cool and shape to obtain a foaming material, and generally has the problems of uneven dispersion of foam nuclei or low refinement degree of the foam nuclei caused by easy aggregation of the fluid; the intermittent foaming is a foaming material obtained by re-foaming after pre-foaming, and the pre-foaming generally adopts an impregnation method to immerse supercritical fluid into the material, so that the dispersion is better and the degree of refining bubbles is high. However, both foaming processes are relatively static foams that are cooled directly after the material is spread apart, keeping the bubbles in the product. And the foaming process only utilizes gas to prop open the molecular chains without subsequent treatment, and when the pressure of the bubbles is consistent with the external pressure and the bubbles are not cooled in time, the molecular chains return to a relaxed state, so that the orientation effect of the bubbles fails. The related process similar to foaming has not been used as an auxiliary orientation or the like, and a situation where stretching is caused but the orientation effect cannot be maintained is formed.
It is therefore necessary to open the molecular chains and to retain the orientation effect in order to obtain a stronger material for subsequent stretch orientation.
Taking polyvinyl chloride (PVC) material as an example: polyvinyl chloride (PVC) materials have stable physicochemical properties, are not easy to be corroded by acid, alkali and the like, have good flame retardant property, and are often used as raw materials of flame retardant parts. PVC can be changed from hard to soft by adding plasticizer, is easier to process and mold through various processing modes, can recycle waste, is an environment-friendly material, and is used in various places in modern industry and life. The processing of polyvinyl chloride includes various modes such as mixing, injection molding, extrusion stretch molding, blown film stretch molding and the like, but in the polymerization process of polyvinyl chloride, the long chain of the polyvinyl chloride usually takes an initiator as a center to coat and form primary particles, and in the common processing mode, the chain groups of the primary particles are difficult to open and entangle with other molecular chains, so the excellent performance of the formed product cannot be completely reflected. China also has made many studies on the disentanglement of polyvinyl chloride. The lamination method described in patent "ZL 200910237622 a nano-laminated composite material preparation device" and patent "ZL 2014101359933 nano-laminated composite extrusion device" can strengthen the stretching orientation of the molten material for multiple times by means of uniform lamination, and the lamination method has great advantages in the aspects of film blowing and extrusion granulation of PVC, but still fails to completely open primary particles of PVC. Aiming at the problems, the invention provides a supercritical fluid micro-explosion disentanglement polymer high-performance processing technology, which opens polymer chain groups from the surface of primary particles in a supercritical fluid micro-explosion mode to form loose long chains capable of being entangled with other long chains, and simultaneously combines a laminating extrusion technology to further release the potential performance of the polymer.
Disclosure of Invention
Aiming at the problem that the prior art can not completely unwind the primary particles of the high polymer to cause that the use performance of the material can not be continuously optimized, the invention provides a high-performance processing technology and equipment for the polymer through supercritical fluid micro-explosion unwinding, and the invention is explained by detailed description of processing of an exemplary material (PVC). The main innovation points of the invention are as follows: orienting the chain segments while micro-exploding and winding the single molecular chain groups by immersing the supercritical fluid into the molecular chain groups, and secondarily orienting and exhausting gas while retaining the orientation effect after micro-explosion in a mode of mixing and exhausting gas (mechanical exhausting); completely orienting the chain groups in the materials by matching with a laminating process to obtain a woven structure material; the resulting reinforced material is free of air bubbles. The method is characterized in that a supercritical fluid is utilized to open single molecular clusters, then mixing and exhausting are carried out in a molten state, lamination and orientation enhancement are carried out, so that a high-performance material without bubbles is obtained, and corresponding manufacturing equipment is designed and improved aiming at the process.
The present invention is to solve the problem of coating long chain of PVC primary particle to entangle with the surrounding long chain or to raise the orientation, so as to release the original performance potential of PVC material and raise the physical strength of the formed product.
The invention discloses a high-performance processing technology and a process route of equipment for micro-explosion and disentanglement of polymers by supercritical fluid, which comprises the following steps: drying materials, low-temperature high-pressure impregnation, heating micro-explosion, mixing and exhausting and laminating extrusion. The basic idea of the process route is to unwind the primary particles of the material by supercritical fluid micro-explosion to form loose molecular clusters with chain segment orientation, then deform the unwound particles by mixing and exhausting (mechanical exhausting) to retain the chain segment orientation effect and perform secondary chain segment orientation, simultaneously exhaust all gases in the material, and finally further orient the molecular chains by lamination process to obtain the woven structure material.
The drying material in the process route of the invention is to evaporate all the non-bound water in the material, so as to prevent the non-bound water from influencing the dipping effect in the dipping process.
The low-temperature high-pressure impregnation refers to that the dried material is added into an impregnation kettle through a metering system, and supercritical CO2 is added through a supercritical fluid injection system, and the environment in the impregnation kettle is maintained at a supercritical point (temperature 31.26OC, pressure 72.9 atm). After sufficient supercritical fluid is injected, immediately sealing the impregnation kettle to ensure that the material is impregnated in the impregnation environment of the supercritical fluid for 2-6 hours, wherein auxiliary stirring measures can be adopted in the impregnation process to optimize the impregnation efficiency, and the stirring measures can be a mechanical stirring method, an ultrasonic method and the like; the specific time of the impregnation is determined by the material, so that the supercritical fluid is completely immersed in the material, and the efficiency is improved.
The heating micro-explosion means that the impregnated raw materials are introduced into a melting extruder, the temperature of the raw materials is raised to a viscous state in the melting extruder, and the space occupied by the materials in unit mass is always kept unchanged in the temperature raising process, and the solution is that the size of the space is controlled by controlling the groove depth and the lead of a screw; after all the materials reach a viscous state, the materials are guided to rapidly enter a larger space from a smaller space, and primary particles are instantly opened by utilizing the advantage of the vaporization volume expansion of the supercritical fluid, so that the primary particles are unwound; the materials after micro-explosion continuously flow to the machine head in the screw rod, so that the materials are prevented from being accumulated.
The micro-explosion of the materials from small space to large space comprises two solving measures: the first is to introduce the material into a transition pipeline, the flowing direction of the material in the transition pipeline is parallel to the gravity direction and downward, thus preventing the material from collapsing, rebounding molecular chain part and the like caused by the material still in a viscous state after micro-explosion, and simultaneously, the material parallel to the gravity direction and downward can vacate space for the material of the subsequent micro-explosion and keep continuity. The feeding quantity and the discharging quantity of the microexplosion section are controlled by the material conveying quantity of the double-stage screw rod adjacent to the microexplosion section.
The second solution is to change the groove depth and lead of the screw to make the space occupied by the material in unit mass rapidly increase. The method for removing the materials at the micro-explosion section in the measure is to improve the material conveying speed at the discharging position of the micro-explosion section by changing the axial roughness of the machine barrel and the like.
The mixing and exhausting process means that the melt after micro explosion is exhausted in the mixing process, gas in the material is extruded out mainly in a mechanical exhausting mode, the molecular chains continue to deform in the mechanical extruding process due to air gaps among molecules, the molecular chains are promoted to be unfolded due to uniform flowing of the gas in the air gaps, meanwhile, the entanglement among different single molecular chains is promoted through the mixing action of a screw, the single molecular chains are prevented from returning to primary particles again, and the material strength is improved.
The above-mentioned discharge while kneading (mechanical discharge) means that the screw groove depth is reduced to discharge the gas in the material while kneading by the screw. It should be noted that the gas inside the material cannot be evacuated from the outside by means of evacuation when the material is static: when the material is static, the direct extraction of gas easily causes the unidirectional uneven flow of gas left in the material after micro-explosion to cause the quality defect of the material; meanwhile, the gas in the material is pumped out in advance, so that the movement space of the molecular chain is reduced, and the molecular chain is not easy to unfold again. In the operation process, the materials do not need to stay in the machine barrel for too long time to prevent decomposition, and all gas in the materials is discharged to avoid the influence on the material performance due to the air holes in the subsequently processed materials.
The lamination extrusion is to build pressure on the material after the air exhaust is finished, and to utilize the stretching orientation effect of the laminator to stretch, orient and laminate the molecular chains, so as to enhance the ordering of the molecular chains in the PVC material. The extruded melt can be directly used for manufacturing products, and can also be used for manufacturing products after being extruded and granulated.
Aiming at the high-performance processing technology of the supercritical fluid microexplosion disentanglement polymer, the special processing equipment designed by the invention comprises basic systems such as a drying system, a dipping system, a microexplosion system, an exhaust extrusion system, a temperature control system and the like. The impregnation system comprises a metering feeding device, a supercritical fluid injection system, an impregnation kettle, a pneumatic conveying part, a ventilation part and the like; the micro-explosion system comprises a metering feeding part, a micro-explosion part and the like; the extrusion system comprises a mixing and exhausting integrated extruder, a laminator, a cutting device and the like.
The micro-explosion system and the extrusion system can be integrated on the same extruder, but the structure is complex, which easily causes the reduction of yield and the increase of control difficulty, so the arrangement form of a double-stage extruder is preferably adopted, the arrangement form of the double-stage extruder means that the micro-explosion part is composed of a melting extruder and a micro-explosion pipeline, and the structure form will be described in detail below.
The specific installation mode of the supercritical fluid micro-explosion disentanglement polymer high-performance processing equipment is as follows: the discharge port of the drying system injects materials into the feed port of the dipping kettle through the metering and feeding equipment, the supercritical fluid injection system is connected with the air inlet of the dipping kettle through an electromagnetic valve, and the electromagnetic valve controls the communication state of the supercritical fluid injection system and the air inlet of the dipping kettle. The two dipping kettles are connected through basic elements such as a filter, an electromagnetic valve and an air compressor, the electromagnetic valve is installed between the filter and the air compressor, and the electromagnetic valve and the filter are installed between the air compressor and each dipping kettle. The discharge port of the dipping kettle is connected with an electromagnetic valve and is connected with a metering feeding component through a pneumatic conveying pipeline, and materials enter the melting extruder through the combined action of gas pushing and the metering feeding component arranged at the feed port of the melting extruder. The heating and cooling part of the melting extruder strictly controls the temperature of the feeding port and the temperature of the heating and cooling part close to the machine barrel, so that the phenomenon that the gas in the material is released in advance due to overheating of the feeding port, overpressure and bridging are caused is avoided. The head of the melting extruder is connected with the port of the mixing exhaust extruder through a microexplosion pipeline, the axis of the main body of the microexplosion pipeline is parallel to the gravity direction, and the feed port of the mixing exhaust extruder is lower than the discharge port of the melting extruder. The head part of the mixing and exhausting extruder is provided with a laminator, the other end of the laminator is connected with a granulating device, and the cut granules enter an aggregate device after being rapidly air-cooled by an air cooling cavity.
The supercritical fluid of the present invention is preferably supercritical CO2 because it is easier to obtain and control, non-toxic and harmless; the microexplosion can also be carried out by using fluid such as H2, N2, water vapor and the like.
The impregnation kettle of the impregnation system is mainly designed in a pressure reaction kettle mode, the pressure reaction kettle is designed to be a high-pressure kettle, the design pressure of the high-pressure kettle is designed to be at least 15MPa, a sufficient safety factor is reserved, and overpressure is prevented. The storage amount of the impregnation kettle is designed according to the productivity, and a daily storage tank with large storage amount is preferably selected; the number of the impregnation kettle can be one or more, and two impregnation kettles are preferably selected in the invention, so that the cost is saved and the efficiency is improved.
The ventilation component mainly comprises an airflow circulating pipeline, a filter, an electromagnetic valve and a bidirectional air compressor, and the design requirement of the ventilation component is the same as the design safety factor of the dipping kettle. The filter is mainly used for preventing PVC materials from entering the air compressor when CO2 is extracted/exchanged, and a multi-stage filtration mode filter is preferably adopted to improve the filtration effect; the air compressor is mainly used for extracting most of redundant CO2 after impregnation into another impregnation kettle, so that the waste of supercritical CO2 is reduced; it should be noted that the air compressor should not create a negative pressure in the impregnation vessel in order to facilitate the later normal operation of the pneumatic transport.
The pneumatic conveying component takes CO2 which is not completely extracted in the impregnation kettle and is not impregnated into the materials as driving gas to drive the materials in the kettle to move along a pneumatic conveying pipeline, and the materials in the kettle are conveyed into the mixing extruder by matching with the metering feeding component.
The metering and feeding device at the feed inlet of the melt extruder according to the invention should have a venting function. The exhaust function of the pneumatic power machine is mainly used for exhausting the power gas conveyed by the pneumatic power machine, so that the influence of the part of the gas on subsequent processing is reduced.
The melt extruder of the micro-explosion system is mainly used for melting materials, meanwhile, the space occupied by the materials with unit mass is kept unchanged in the melting process, and the condition can be controlled by controlling the groove depth of the screw. The microexplosion pipeline is preferably a cylindrical pipeline, the axial length of a vertical section of the microexplosion pipeline is larger than the inner diameter, the inner diameter of the vertical section is larger than the diameter of an outlet of the melting extruder, and the specific diameter proportion is determined by the required microexplosion coefficient. In the design process, the diameter of the micro explosion pipeline is fixed, the diameter ratio is controlled by reducing the outlet diameter of the melting extruder, and the diameter of the micro explosion pipeline does not exceed the diameter of a feed inlet of the mixing and exhausting extruder or the inner diameter of a machine barrel.
The groove depth of the screw of the mixing and exhausting extruder is gradually reduced, and the screw is ensured to have a strong mixing effect according to the material type, so that the opened single long chain is entangled with other long chains, the single long chain is prevented from being coated again, and the combination forms of single screw, double screw, planetary screw and the like can be selected. The mixing and air-exhausting extruder has the action mode that air is exhausted while mixing, air is exhausted at normal pressure in the air exhausting process, and pressure building extrusion is carried out after the air is completely exhausted. During the design process of the screw, consideration should be given to preventing the materials from decomposing due to overhigh temperature and long-time stay.
In the processing of PVC materials, the screw form of the mixing and exhausting extruder is preferably a planetary screw, and a double-cone screw, a single screw and the like can also be selected. The processing of other high polymers should select screw combination form according to specific mixing effect.
According to the micro-explosion unwrapping process, the supercritical fluid is impregnated at low temperature and high pressure, so that the defect that the fluid is aggregated into larger bubble nuclei due to the fact that the fluid is not well dispersed after materials are melted and then the supercritical fluid is added can be avoided, or the fluid is mostly aggregated between molecular chains instead of gaps of single molecular chains. The invention utilizes the action mode of mixing and exhausting after the disentanglement to exhaust the gas in the material, deforms the opened loose molecular chain group, is not easy to return to the original state, retains the orientation effect in the micro-explosion process, is easy for the orientation processing of the molecular chain at the later stage, obtains the molecular chain with higher proportion of the stretched orientation, and solves the problem that partial material can not completely open the molecular chain in the melt orientation process.
The supercritical fluid micro-explosion disentanglement polymer high-performance processing technology and equipment can continuously, efficiently and inexpensively disentangle polymer chain groups/primary particles by utilizing a supercritical fluid micro-explosion mode, keep the chain segments oriented by micro-explosion to smoothly enter the next stage for orientation by a mechanical exhaust mode, form a material without bubbles with higher orientation degree and orderly arranged molecular chains by combining a lamination extrusion technology, and optimize the use performance of the polymer.
Drawings
FIG. 1 is a schematic view of the main body of the equipment for the supercritical fluid micro-explosion de-winding polymer high-performance processing technology and equipment.
FIG. 2 is a partial schematic view of the micro-explosion and mixing exhaust part of the supercritical fluid micro-explosion de-entangling polymer high-performance processing process and equipment.
FIG. 3 is a schematic view of a micro-explosion pipeline of a supercritical fluid micro-explosion de-winding polymer high-performance processing process and equipment.
FIG. 4 is a schematic view of the disentanglement principle of the supercritical fluid microexplosion disentanglement polymer high-performance processing technology and equipment.
FIG. 5 is a schematic view of an alternative type of screw of the mixing and degassing extruder for the supercritical fluid microexplosion entangling polymer with high performance and the equipment.
In the figure: 1-first impregnation kettle; 2-second impregnation kettle; 3-an air inlet; 4-a stirring motor; 5-a feed inlet of the impregnation kettle; 6-air compressor; 7-micro explosion pipeline; 8-mixing and exhausting extruder; 9-a laminator; 10-a blanking member; 11-melt extruder; 12-a dosing member; 13-a solenoid valve; 14-discharge hole of the dipping kettle; 15-a filter; 16-a solenoid valve; 7-1-primary particle schematic; 17-2-schematic representation of loose chain groups after micro-explosion; 17-3-schematic view of semi-oriented molecular chain after mechanical degassing; schematic diagram of 17-4-oriented molecular chain.
Detailed Description
The invention discloses a high-performance processing technology and a process route of equipment for micro-explosion and disentanglement of polymers by supercritical fluid, which comprises the following steps: drying materials, low-temperature high-pressure impregnation, heating micro-explosion, mixing and exhausting, and laminating and extruding. As shown in FIG. 4, the basic idea of the process route is to detangle the primary particles 17-1 of the material by supercritical fluid microexplosion to form a loose molecular chain group 17-2 with chain segment orientation, then deform the detangled particles by means of mixing and exhausting (mechanical exhausting), retain the chain segment orientation effect and perform secondary chain segment orientation, simultaneously exhaust all the gas in the material to obtain a semi-oriented molecular chain 17-3, and finally further orient the molecular chain by lamination process to obtain an oriented molecular chain 17-4.
As shown in FIG. 1, the supercritical fluid micro-explosion disentanglement equipment for high performance processing of polymers comprises a drying system, a dipping system, a micro-explosion system, an exhaust extrusion system, a temperature control system and other basic systems. The impregnation system comprises a metering feeding device, a supercritical fluid injection system, an impregnation kettle 1 (or 2), a pneumatic conveying part, a ventilation part and the like; the micro-explosion system comprises a metering feeding part 12, a micro-explosion part and the like; the extrusion system includes a kneading and degassing integrated extruder 8, a laminator 9, a blanking device 10, and the like.
As shown in FIG. 1, the specific installation manner of the supercritical fluid micro-explosion disentanglement polymer high-performance processing equipment of the invention is as follows: the discharge port of the drying system injects materials into the feed port 5 of the dipping kettle through the metering and feeding equipment, the supercritical fluid injection system is connected with the air inlet 3 of the dipping kettle through an electromagnetic valve, and the communication state of the supercritical fluid injection system and the air inlet 3 of the dipping kettle is controlled by the electromagnetic valve. The two steeping kettles are connected through basic elements such as a filter 15, an electromagnetic valve 16 and an air compressor 6, the electromagnetic valve 16 is arranged between the filter 15 and the air compressor 6, and the electromagnetic valve 16 and the filter 15 are arranged between the air compressor 6 and each steeping kettle 1 (or 2). The discharge port 14 of the dipping kettle is connected with an electromagnetic valve 13 and is connected with a metering and feeding part 12 through a pneumatic conveying pipeline, and materials enter the melting and extruding machine 11 through the combined action of gas pushing and the metering and feeding part 12 arranged at the feed port of the melting and extruding machine 11. The heating and cooling unit of the melt extruder 11 strictly controls the temperature at the feed port and the temperature in the vicinity of the feed barrel, and prevents the feed port from overheating, which leads to premature release of fluid inside the material, which leads to overpressure and bridging. The head of the melting extruder 11 is connected with the feed inlet of the mixing exhaust extruder 8 through a microexplosion pipeline 7, the axis of the main body of the microexplosion pipeline 7 is parallel to the gravity direction, and the feed inlet of the mixing exhaust extruder 8 is lower than the discharge outlet of the melting extruder 11. The head part of the mixing and exhausting extruder 8 is provided with a laminator 9, the other end of the laminator is connected with a granulating device 10, and the cut granules enter an aggregate device after being rapidly air-cooled by an air cooling cavity.
The heating micro-explosion means that the impregnated raw materials are introduced into a melting extruder 11, the temperature of the raw materials is raised to a viscous state in the melting extruder 11, and the space occupied by the unit mass of the materials is always kept unchanged in the temperature raising process, and the solution is to control the size of the space by controlling the groove depth and the lead of a screw; after all the materials reach a viscous state, the materials are guided to rapidly enter a larger space from a smaller space, and primary particles are instantly opened by utilizing the advantage of the vaporization volume expansion of the supercritical fluid, so that the primary particles are unwound; it is especially noted that the discharge amount at the micro-explosion section is slightly larger than the feed amount thereof so as to remove the micro-exploded material at the micro-explosion section as soon as possible and prevent the accumulation of the material.
The measures for changing the micro-explosion space in the invention comprise two types: first, as shown in fig. 2, the material is introduced into a microexplosion circuit 7, and the flowing direction of the material in the microexplosion circuit 7 is parallel to the gravity direction and downward. The feeding amount and the discharging amount of the microexplosion pipeline 7 are controlled by the material conveying amount of the double-stage screw rod adjacent to the microexplosion pipeline. The second solution is to change the groove depth and lead of the screw to make the space occupied by the material in unit mass rapidly increase. The method for removing the materials at the micro-explosion section in the measure is to improve the material conveying speed at the discharging position of the micro-explosion section by changing the axial roughness of the machine barrel and the like.
As shown in fig. 3, the micro-explosion pipe 7 is preferably a cylindrical pipe, the axial length of the vertical section of the pipe is larger than the inner diameter, the inner diameter of the vertical section is larger than the outlet diameter of the melt extruder, and the specific diameter ratio is determined by the required micro-explosion coefficient. It is recommended in the design process to fix the diameter of the micro-explosion tube 7 and control the diameter ratio by reducing the outlet diameter of the melt extruder 11, and the diameter of the micro-explosion tube 7 should not exceed the diameter of the feed port or the inner diameter of the cylinder of the mixing and degassing extruder 8.
As shown in fig. 5, the groove depth of the screw of the mixing and degassing extruder 8 should be gradually reduced, and the screw should be ensured to have a strong mixing effect according to the material type, so that the opened single long chain is entangled with other long chains, and the single long chain is prevented from being coated by itself again, and a combination form of a single screw, a double screw, a planetary screw and the like can be selected. The mixing and air-discharging extruder 8 operates in a mode that air is discharged while mixing, air is discharged at normal pressure in the air discharging process, and pressure is built for extrusion after the air is completely discharged. During the design process of the screw, consideration should be given to preventing the materials from decomposing due to overhigh temperature and long-time stay.
The specific operation mode of the invention is as follows: the drying system dries the material to ensure that the pores of the primary particles 17-1 contain no moisture; meanwhile, high-pressure air tightness detection is carried out on the dipping kettle 1 (or 2), the ventilation component, the pneumatic conveying component and the like (the air tightness detection is required before the equipment is started every time), and the next stage of work is carried out after the detection is qualified.
The dried materials are fed into the first impregnation kettle 1 through a metering and feeding system, the volume of the materials in the first impregnation kettle 1 is not more than 2/3 of the volume of the impregnation kettle, after all the materials are fed into the first impregnation kettle 1, air in the first impregnation kettle is preferably extracted completely, and then supercritical CO2 is injected into the first impregnation kettle 1 through a supercritical fluid injection system. After the supercritical fluid is immersed in the materials in the first impregnation kettle 1, the first impregnation kettle (1) is sealed for 2-6h, and meanwhile, the stirring element 4 in the kettle is kept continuously stirring to accelerate the impregnation.
In the process of material impregnation in the first impregnation kettle 1, adding a material to be impregnated into the second impregnation kettle 2, sealing the second impregnation kettle 2, adding a certain amount of supercritical fluid (determined by the supercritical fluid lost by the material impregnated in the first impregnation kettle in the experiment) into the second impregnation kettle 2, and sealing the second impregnation kettle 2. After the materials in the first impregnation kettle 1 are impregnated for enough time, opening an air compressor 6 between the first impregnation kettle 1 and the second impregnation kettle 2, wherein the air suction direction of the air compressor is from the first impregnation kettle 1 to the second impregnation kettle 2; after the air compressor 6 operates stably, opening the electromagnetic valves 16 between the air compressor 6 and each kettle, pumping part of supercritical fluid which is not dipped into the materials in the first dipping kettle 1 into the second dipping kettle 2 through the ventilation part, and keeping the materials in the first dipping kettle 1 due to the blockage of the filter 15; after the gas extraction is finished, the electromagnetic valve 16 is closed to seal the second dipping kettle 2, and then the air compressor 6 is closed. The electromagnetic valve 13 at the discharge port 14 of the first impregnation kettle 1 is opened, and the materials enter the melt extruder 11 through the combined action of the pushing of the CO2 remained in the first impregnation kettle 1 and not entering the material pores and a metering feeding part arranged at the feed port of the melt extruder 11. After the materials are completely emptied from the first impregnation kettle 1, the discharge hole 14 is closed through the electromagnetic valve 13, and then the materials which are not impregnated and the supercritical fluid are added into the first impregnation kettle 1, and the steps are repeated, so that the first impregnation kettle 1 and the second impregnation kettle 2 operate alternately.
The temperature at the feed port of the melt extruder 11 should be maintained at about 31.26OC to prevent bridging and premature expansion of the supercritical fluid. The melting extruder 11 plasticizes and extrudes the material under the condition of ensuring that the space occupied by the material per unit mass is unchanged. The material extruded from the discharge port of the melt extruder 11 enters the microexplosion pipeline 7 for disentanglement, and the disentangled material directly enters the mixing exhaust extruder 8 for mixing and exhausting. The feeding amount of the mixing and air-exhausting extruder 8 is slightly larger than the discharging amount of the melting extruder 11, and can be controlled by controlling the rotating speed of the corresponding screw. The molecular chain is oriented secondarily through the mixing action of the mixing extruder 8, other additives (such as color master batches and the like) can be added into the material as required in the mixing process, after all exhaust is completed, the pressure is built for the material, the material is further stretched, oriented and laminated and extruded through the laminator 9, the extruded material is granulated through the granulating equipment 10 and then cooled by air, and high-performance high polymer granules are obtained and used for processing products. The above description is provided for the specific apparatus and process conditions of the present invention, and is illustrated with reference to the drawings. The present invention is not limited to the specific apparatus and process described above, and any modification or replacement of the related apparatus or any local adjustment of the related process based on the above description is within the spirit and scope of the present invention.
Claims (8)
1. The supercritical fluid micro-explosion disentanglement polymer high-performance processing technology is characterized in that:
step one, drying materials: evaporating all the non-bound water in the material;
step two, low-temperature high-pressure impregnation: adding the dried material into an impregnation kettle through a metering system, adding supercritical CO2 through a supercritical fluid injection system, keeping the environment in the impregnation kettle at a supercritical point, immediately sealing the impregnation kettle after sufficient supercritical fluid is injected, and impregnating the material in the impregnation environment of the supercritical fluid for 2-6 hours to ensure that the material is completely immersed in the supercritical fluid;
thirdly, heating and micro-blasting: introducing the impregnated raw materials into a melt extruder, heating the raw materials to a viscous state in the melt extruder, and keeping the space occupied by the materials per unit mass unchanged all the time in the heating process; after all the materials reach a viscous state, the materials are guided to rapidly enter a larger space from a smaller space, and primary particles are unfolded by utilizing the instant of vaporization volume expansion of the supercritical fluid so as to unwind the primary particles; the materials after micro-explosion continuously flow to the machine head in the screw;
step four, mixing and exhausting: exhausting the melt after micro explosion in a mixing process, mainly extruding gas in the material in a mechanical exhaust mode, continuously deforming the molecular chains in the mechanical extrusion process due to air gaps among molecules, promoting the molecular chains to be unfolded due to uniform flow of the gas in the air gaps, promoting the different single molecular chains to be tangled under the mixing action of a screw rod, and avoiding the single molecular chains from returning to primary particles again;
fifthly, laminating and extruding: after the air exhaust is finished, pressure is built on the materials, molecular chains are stretched, oriented and laminated by utilizing the stretching and orienting action of a laminator, the orderliness of the molecular chains in the PVC materials is enhanced, and extruded melt is directly used for manufacturing products or is used for manufacturing the products after being extruded and granulated.
2. The supercritical fluid micro-explosion entanglement polymer high-performance processing technology according to claim 1, characterized in that: in the second step of dipping process, auxiliary stirring measures can be adopted to optimize the dipping efficiency, and the stirring measures can be a mechanical stirring method or an ultrasonic wave method.
3. The supercritical fluid micro-explosion entanglement polymer high-performance processing technology according to claim 1, characterized in that: the material is microexposed from a small space to a large space, the material is introduced into a transition pipeline, the flowing direction of the material in the transition pipeline is downward parallel to the gravity direction, the material is prevented from collapsing and the molecular chain is partially rebounded due to the fact that the material is still in a viscous state after the microexplosion, meanwhile, the downward direction parallel to the gravity direction can vacate the space for the subsequent microexplosion material and keep continuity, and the feeding amount and the discharging amount of the microexplosion section are controlled by the material conveying amount of the double-stage screw rod adjacent to the microexplosion section.
4. The supercritical fluid micro-explosion entanglement polymer high-performance processing technology according to claim 1, characterized in that: the materials are microexposed from a small space to a large space, the groove depth and the lead of the screw rod are changed to rapidly increase the space occupied by the materials of unit mass, and the material conveying speed at the discharge part of the microexplosion section is improved by changing the axial roughness of the machine barrel.
5. The supercritical fluid micro-explosion disentanglement polymer high-performance processing equipment is characterized in that: the system comprises a drying system, an impregnation system, a micro-explosion system, an exhaust extrusion system and a temperature control system, wherein the impregnation system comprises metering feeding equipment, a supercritical fluid injection system, an impregnation kettle, a pneumatic conveying part and a ventilation part; the micro-explosion system comprises a metering feeding part, a micro-explosion part and the like; the extrusion system comprises a mixing and exhausting integrated extruder, a laminator and a cutting device; the microexplosion system and the extrusion system adopt the arrangement form of a two-step extruder, a discharge port of the drying system injects materials into a feed port of the dipping kettle through metering feed equipment, the supercritical fluid injection system is connected with a gas inlet of the dipping kettle through an electromagnetic valve, and the electromagnetic valve controls the communication state of the supercritical fluid injection system and the gas inlet of the dipping kettle; the two dipping kettles are connected through basic elements such as a filter, an electromagnetic valve, an air compressor and the like, the electromagnetic valve is arranged between the filter and the air compressor, and the electromagnetic valve and the filter are arranged between the air compressor and each dipping kettle; the discharge port of the dipping kettle is connected with an electromagnetic valve and is connected with a metering feeding part through a pneumatic conveying pipeline, and materials enter the melting extruder through the combined action of gas pushing and the metering feeding part arranged at the feed port of the melting extruder; the heating and cooling part of the melting extruder strictly controls the temperature at the feeding port and the temperature close to the machine barrel; the head of the melting extruder is connected with the port of the mixing exhaust extruder through a microexplosion pipeline, the axis of a main body of the microexplosion pipeline is parallel to the gravity direction, and the feed port of the mixing exhaust extruder is lower than the discharge port of the melting extruder; the head part of the mixing and exhausting extruder is provided with a laminator, the other end of the laminator is connected with a granulating device, and the cut granules enter an aggregate device after being rapidly air-cooled by an air cooling cavity.
6. The supercritical fluid microexplosion entangling polymer high performance processing equipment according to claim 5, wherein: the supercritical fluid is supercritical CO2, H2, N2 or water vapor.
7. The supercritical fluid microexplosion entangling polymer high performance processing equipment according to claim 5, wherein: the ventilation component mainly comprises an airflow circulation pipeline, a filter, an electromagnetic valve and a bidirectional air compressor, wherein the filter is mainly used for preventing PVC materials from entering the air compressor when CO2 is extracted/exchanged, and a multi-stage filtration mode filter is preferably adopted to improve the filtration effect; the air compressor is mainly used for extracting most of the redundant CO2 after the impregnation is finished into the other impregnation kettle, and waste of supercritical CO2 is reduced.
8. The supercritical fluid microexplosion entangling polymer high performance processing equipment according to claim 5, wherein: the pneumatic conveying component takes CO2 which is not completely extracted in the impregnation kettle and is not impregnated into the materials as driving gas to drive the materials in the kettle to move along a pneumatic conveying pipeline, and the materials in the kettle are conveyed into the mixing extruder by matching with the metering feeding component.
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