WO2006056128A1 - Procede de production en continu d'une solution de polyethylene de poids moleculaire ultraleger - Google Patents

Procede de production en continu d'une solution de polyethylene de poids moleculaire ultraleger Download PDF

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Publication number
WO2006056128A1
WO2006056128A1 PCT/CN2005/001989 CN2005001989W WO2006056128A1 WO 2006056128 A1 WO2006056128 A1 WO 2006056128A1 CN 2005001989 W CN2005001989 W CN 2005001989W WO 2006056128 A1 WO2006056128 A1 WO 2006056128A1
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Prior art keywords
molecular weight
weight polyethylene
static mixer
screw
solution
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Ceased
Application number
PCT/CN2005/001989
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English (en)
Chinese (zh)
Inventor
Yin Shi
Yedong Yin
Lin Tan
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BEIJING TEX-STRONG NEW MATERIAL DEVELOPMENT Co Ltd
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BEIJING TEX-STRONG NEW MATERIAL DEVELOPMENT Co Ltd
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Publication of WO2006056128A1 publication Critical patent/WO2006056128A1/fr
Anticipated expiration legal-status Critical
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    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D1/00—Treatment of filament-forming or like material
    • D01D1/02—Preparation of spinning solutions
    • 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
    • B29C48/022—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor characterised by the choice of material
    • 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
    • B29C48/25—Component parts, details or accessories; Auxiliary operations
    • B29C48/267—Intermediate treatments, e.g. relaxation, annealing or decompression step for the melt
    • 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
    • B29C48/25—Component parts, details or accessories; Auxiliary operations
    • B29C48/36—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die
    • B29C48/375—Plasticisers, homogenisers or feeders comprising two or more stages
    • B29C48/387—Plasticisers, homogenisers or feeders comprising two or more stages using a screw extruder and a gear pump
    • 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
    • B29C48/25—Component parts, details or accessories; Auxiliary operations
    • B29C48/36—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die
    • B29C48/395—Means 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
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/02—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D01F6/04—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolymers obtained by reactions only involving carbon-to-carbon unsaturated bonds from polyolefins
    • 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
    • B29C48/03—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor characterised by the shape of the extruded material at extrusion
    • B29C48/04—Particle-shaped
    • 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
    • B29C48/03—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor characterised by the shape of the extruded material at extrusion
    • B29C48/05—Filamentary, e.g. strands
    • 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
    • B29C48/25—Component parts, details or accessories; Auxiliary operations
    • B29C48/30—Extrusion nozzles or dies
    • B29C48/345—Extrusion nozzles comprising two or more adjacently arranged ports, for simultaneously extruding multiple strands, e.g. for pelletising
    • 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
    • B29C48/25—Component parts, details or accessories; Auxiliary operations
    • B29C48/36—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die
    • B29C48/365—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die using pumps, e.g. piston pumps
    • 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
    • B29K2023/00—Use of polyalkenes or derivatives thereof as moulding material
    • B29K2023/04—Polymers of ethylene
    • B29K2023/06—PE, i.e. polyethylene

Definitions

  • the invention belongs to the technical field of polymer material preparation, and particularly relates to an improved method of the first process in the production process of ultra high molecular weight polyethylene fibers. Background technique
  • Ultra high molecular weight polyethylene fiber with high strength, high modulus and high orientation, is widely used in the manufacture of protective equipment, ropes, fishing nets and sports equipment.
  • Ultra-high molecular weight polyethylene fiber also known as high-strength high-modulus polyethylene fiber, high-orientation polyethylene fiber, high-performance polyethylene fiber.
  • Smith and Lemstra of DSM of the Netherlands invented the process of producing ultra-high molecular weight polyethylene fibers by gel spinning, and obtained British patents GB2042414 and GB2051667.
  • AlliedSignal of the United States also proposed its own patent for the production of ultra-high molecular weight polyethylene fibers.
  • the US4413110o DSM realized the industrial production of ultra-high molecular weight polyethylene fibers by gel spinning.
  • the main process steps in the manufacture of ultrahigh molecular weight polyethylene fibers by the gel spinning method which is common in the world are as follows:
  • the ultrahigh molecular weight polyethylene is dissolved in a first solvent to prepare a polyethylene solution, and the solution is extruded by a screw extruder. After being spun out through the spinning box, it is cooled and solidified into gel fibers, and the first solvent is extracted with a volatile second solvent, dried, and super-folded to obtain a finished fiber.
  • DSM and Toyobo
  • Honeywell and Mitsui The main difference between the two is the use of different solvents.
  • the DSM process uses decahydronaphthalene as the solvent. Due to the volatility of decahydronaphthalene, the process eliminates the subsequent extraction section; Honeywell uses a paraffinic oil solvent, requires a subsequent extraction section, and extracts the first solvent with a second solvent. come out.
  • the polyethylene powder as a raw material has an intrinsic viscosity of at least 5 dL/g, and thus has a fiber strength of at least 25 cN/dtex and a modulus of at least 700 cN/dtex.
  • the relative molecular weight of the raw material polyethylene must be greater than 1 million, preferably greater than 4 million.
  • the first step in the ultra high molecular weight polyethylene fiber process is the preparation of a polyethylene solution.
  • This step is also a very important step, because the uniformity of the solution mixture directly affects the quality of the spinning. If the solution cannot be mixed, it will affect the spinning and stretching sections, which will ultimately affect the performance and quality of the finished fiber.
  • the preparation of the solution is not described in detail in the original patents GB2042414 and GB2051667, but simply describes the solvent used as decalin and the like, and the operating temperature is 145 degrees Celsius.
  • the preparation process of the polymer solution is complicated, and unlike the solution of the small molecule substance, a special process is required.
  • Polymers have special physical properties different from small molecular substances, and the preparation of bismuth molecular polymer solutions has its own special features.
  • the polymer solution is very different in behavior from the small molecule solution. Since the size of the polymer is large, the molecular motion speed is much smaller than that of the small molecule, and the diffusion of the polymer into the solvent is very slow, so the dissolution process of the polymer is much slower than the dissolution process of the small molecule.
  • the dissolution process of the polymer goes through two stages, the first being swelling, ie the penetration of solvent molecules into the interior of the polymer, causing the polymer to expand in volume. Then the polymer is evenly dispersed into the solvent to achieve complete dissolution.
  • the viscosity of the polymer solution is large, especially as the molecular weight of the polymer increases, so that the viscosity increases, which increases the power required to transport the solution.
  • the solubility of the polymer is related to the molecular weight. Generally, the larger the molecular weight, the smaller the solubility, and the smaller the molecular weight, the greater the solubility. Increasing the temperature generally also increases the solubility, so the dissolution process uses more heating.
  • increasing the relative molecular weight of the polyethylene can increase the strength of the finished fiber, the relative molecular weight of the raw material polyethylene powder should not be too large because the viscosity of the solution increases the energy consumption of the processing, particularly the extrusion process. Under normal circumstances, no more than 10 million.
  • the flow behavior of polymer solutions is mostly non-Newtonian fluids.
  • Ultrahigh molecular weight polyethylene solutions are typical pseudoplastic fluids.
  • the polymer solution flows, there are special phenomena such as the climbing rod effect, the expansion of the extrudate, the unstable flow and the melt fracture.
  • the concentrated polymer solution is stirred in a container, the fluid will rise along the inner cylinder wall or the shaft due to the action of the rotary shear, and the shaft or the climbing rod will occur. Wesenburg first discovered this phenomenon, hence the so-called Weissenberg effect.
  • the Weissenberg effect is caused by the shear flow of the polymer fluid near the shaft, causing the coiled macromolecular chain to be pulled up in the streamline direction, and the thermal motion energy of the macromolecular chain makes it Spontaneous return to the original curl state, resulting in a normal stress difference in equilibrium with the stretch.
  • the phenomenon of the inclusion axis is limited by the tendency of this recovery to curl, which is attributed to the enveloping force of the shaft, which causes the polymer molecules to be axially extruded.
  • the concentration of the polymer solution increases and the agitation speed increases, the Weissenberg effect becomes more apparent.
  • the preparation section of the ultrahigh molecular weight polyethylene solution undergoes a stage of swelling and dissolution.
  • the whole section is intermittent operation, which takes a long time, occupies a large area, and occupies a large number of containers.
  • EP0255618 mentions the use of hydrotreated kerosene and subsequent rectification to obtain naphthalene-free and biphenyl-free
  • the concentration of the polyethylene solution is not more than 50%.
  • Japanese Patent JP59232123 mentions that the ultrahigh molecular weight polyethylene and a small amount of solvent are mixed for several minutes and then heated, and the solvent is continuously added under stirring to finally prepare a solution. In the example mentioned in Japanese Patent Publication No.
  • a method for continuously preparing a polyethylene solution, a high molecular weight polyethylene and a solvent which is liquid at room temperature, is also proposed in the European Patent No. EP 0 183 285 and U.S. Patent No. 4,668,17, which are mixed into a screw extruder for a screw rotation speed of 30 to 300 rpm.
  • the residence time is 0.3D, the unit is minutes, and D is the value of the extruder diameter in millimeters.
  • the solution is extruded from the extruder and directly into the spinneret to form a filament.
  • the screw extruder is a single screw or multi-screw extruder.
  • the rotational speed of the screw is relatively high, the rotational speed of the twin-screw extruder must be greater than 30 rev / min, typically 150 to 300 r / min, a shear rate of 30 to 2000 seconds 4 .
  • the hybrid method proposed in this patent is more practical than the previous patent.
  • the shortcoming of this patent is that under the high shearing effect of the polyethylene material, although the mixing effect is good, the molecular chain is also seriously damaged, and as a result, the relative molecular weight of the polyethylene is inevitably decreased.
  • DSM's subsidiary, Stamika, in Chinese patent CN85107352 provides a method for continuously preparing a homogeneous solution of a high molecular polymer, comprising: forming a finely divided polymer in a suitable solvent or solvent mixture. Suspended material, processed by a positive rotary screw extruder, rotating at 30 ⁇ 300 rpm, with alternating mixing and conveying parts, suspension residence time of up to 0.3D (minutes), where D is the pressure in millimeters Outlet diameter. This method also severely destroys the molecular chain of the ultra-molecular weight polyethylene and lowers the molecular weight. Summary of the invention
  • the combination of a screw extruder with a length to diameter ratio of 2 to 40 and a static mixer can reduce the probability of molecular weight reduction of ultra high molecular weight polyethylene, improve product quality, speed up the dissolution rate, and ensure uniform mixing of materials;
  • the increase can increase the concentration of the solution, and the corresponding low can reduce the processing amount of the extraction section in the subsequent process, and reduce the operation cost.
  • the method for continuously preparing and mixing a super-molecular weight polyethylene solution of the invention comprises the following steps -
  • the metering pump can be used to replenish the lost mechanical energy between the two static mixers, and then enter the next level static mixer, from static
  • the mixer continuously delivers a homogeneously mixed ultrahigh molecular weight polyethylene solution. That is, the preparation process of the first polyethylene solution of the ultrahigh molecular weight polyethylene fiber process is completed.
  • multiple static mixers can also be used in parallel.
  • the above static mixer can be one or more stages, and a metering pump is added between adjacent static mixers to supplement the kinetic energy loss of the material during the mixing process.
  • the subsequent process can be continuously operated by a conventional mature process, that is, the above-mentioned prepared uniformly mixed ultrahigh molecular weight polyethylene solution is sent out and filtered into the filter; after the filtered material is extruded into the second screw extruder, The spinning box is sprayed, cooled to form a gel fiber, the solvent is extracted, dried, drawn, and wound to form an ultrahigh molecular weight polyethylene fiber.
  • the polyethylene powder used in the present invention has an intrinsic viscosity of more than 5 dL/g, a relative molecular weight of more than 1,000,000, and preferably more than 4,000,000.
  • the solvent in the first step is a solvent which is not volatile at normal temperature. It may be a hydrocarbon, a cyclic hydrocarbon, a derivative of a hydrocarbon or a cycloalkane, an aromatic hydrocarbon, or an aromatic hydrocarbon derivative. Or a mixture of several of them.
  • the short length to diameter ratio screw extruder described above functions to provide flowing mechanical energy to the material.
  • the screw of the short aspect ratio screw extruder may be a single screw, a twin screw, or a three screw, or a four screw, and the outer wall of the screw is heated by electric heating or heat carrier. In order to reduce the shearing action of the screw, it is preferred to use a single screw extruder.
  • the screw extruder has a length to diameter ratio of 2 to 40. It should be noted that although the length is not specified, the range of any two points within the range of 2-40, for example, 3-36, 5-30, 10-30, etc., They are all disclosed here as specifically pointed out.
  • Static mixers can be used with spiral sheet static mixers, twill plate mixers, flow channel static mixers, enhanced mixers, or other new static mixers that can be used for high viscosity fluid mixing.
  • the outer wall of the mixer is jacketed and heated by electric heating or heat carrier.
  • the metering pump uses a metering pump that delivers high viscosity fluids.
  • the temperature of the above mixing process is generally maintained at 140 ⁇ 16i) °C. . . ,
  • the screw extruder in the subsequent process can employ a twin-screw extruder.
  • the extractant in the subsequent process is a volatile solvent such as benzene, toluene, xylene, acetone, gasoline, kerosene, and the like.
  • the extracted fiber is hot drawn, and the total draw ratio is 30 or more.
  • FEATURES AND TECHNOLOGICAL EFFECTS OF THE INVENTION - The present invention has found and proved for the first time that a static mixer can be used in a continuous mixing and mixing process of an ultrahigh molecular weight polyethylene solution, with a stirrer, a colloid mill, a homogenizer, a venturi, and the like. Compared with the dynamic mixing device, it has the advantages of compact structure, simple process, low energy consumption, large operation flexibility, low investment, and good mixing performance. However, static mixers need to add energy to the input materials to mix them. Choosing the right energy input device is an important task, which increases the difficulty of design work.
  • the static mixer used in the present invention was originally a common equipment in melt spinning.
  • a static mixer is an efficient mixing device with no moving parts.
  • a variety of additives are mixed. It is generally believed that the static mixer mainly plays a role of dispersing and mixing, and the effect of mixing is limited; while the effect of the dynamic mixer such as a stirrer on the material is mainly mixing.
  • Static mixers can be divided into four types according to different mixing elements: spiral type, twill type, flow path type, and enhanced type. It is proved by experiments that these four types of static mixers can be used for ultra high molecular weight polyethylene. The solution mixes uniformly and achieves continuous operation of the process.
  • the invention provides a continuous production process for preparing a mixed ultrahigh molecular weight polyethylene solution. It reduces production time, reduces the number of container equipment, and more importantly avoids the damage of polyethylene molecular chains caused by high shear.
  • the present invention uses a combination of a short aspect ratio screw extruder and a static mixer as compared with the prior art technique of simply using a screw extruder.
  • the screw extruder provides the power to flow the material.
  • the long-diameter ratio of the screw extruder is small, which ensures that the lower the rotation speed can guarantee the shorter residence time under a certain production capacity.
  • the rotation speed is low, the shearing force of the screw on the material is small, the probability of reducing the molecular weight of the polyethylene is reduced, and the product quality is improved; the residence time of the material in the screw extruder is short, and the molecular weight of the polymer is also reduced. possibility.
  • the addition of the static mixer accelerates the dissolution rate and reduces the possibility of molecular weight reduction; it also ensures that the materials can be mixed evenly.
  • the invention can increase the concentration of the solution and reduce the processing amount of the extraction section in the subsequent process, thereby reducing the operation cost.
  • FIG. 1 is a process flow for the production of ultra high molecular weight polyethylene fibers using the process of the present invention. detailed description The continuous preparation and mixing method of the ultrahigh molecular weight polyethylene solution proposed by the present invention is described in detail below with reference to the accompanying drawings and non-limiting examples:
  • Fig. 1 is a flow chart showing the manufacturing process of an ultrahigh molecular weight polyethylene fiber in which a mixed solution is continuously prepared by using a static mixer of the present invention.
  • the static mixer-metering pump is a three-stage design, and the actual application can be one, two, or multiple stages.
  • the ultrahigh molecular weight polyethylene powder material 1 and the auxiliary agent (may not be added) and the solvent 2 are continuously metered into the hopper 3, and the material is then introduced into the screw extruder 4 for preliminary mixing and providing kinetic energy for the flow, and the material is subsequently introduced.
  • the first stage static mixer 5 mixes, and then the material is replenished by the metering pump 6 to lose kinetic energy during the flow, and then enters the second stage static mixer 7 and the metering pump 8 for further mixing and replenishing kinetic energy, and finally the material enters the
  • the tertiary static mixer 9 and the metering pump 10 perform the final mixing and supplemental kinetic energy to complete the continuous mixing process of the ultrahigh molecular weight polyethylene solution of the present invention.
  • the mixed material is then passed through the filter 11, into the screw extruder 12, and then ejected through the spinneret 13, into the condenser 14 for solidification, and then through the extraction section 15, the drying section 16, for the super-folding section 17, and finally The winding station 18 is finished.
  • Example 1 The examples of the continuous preparation and mixing method of the ultrahigh molecular weight polyethylene solution of the present invention are respectively described as follows: Example 1
  • a polyethylene powder having a weight average molecular weight of 5 million was introduced into the feed port through a hopper.
  • the powder feed rate is 0.5 kg / min.
  • the solvent paraffin oil is metered by the rotameter from the storage tank and enters the feed port.
  • the solvent paraffin oil has a feed rate of 0.005 cubic meters per minute.
  • the two materials then enter the screw extruder, which is a single screw with a diameter of 80 mm and a screw length of 1500 mm.
  • the outer sleeve of the screw has a wall thickness of 15 mm and is electrically heated at a temperature of 140 °C.
  • the screw speed is 30 rpm and the motor is rated at 15 kW.
  • the static mixer uses a KM type spiral static mixer manufactured by Kenics.
  • the metering pump is a JRG-1.2 metering pump manufactured by Shanghai Jingfang.
  • the uniformly mixed ultrahigh molecular weight polyethylene solution was continuously fed through a two-stage
  • the mixture was filtered through a filter, passed through a twin-screw extruder, spun, and extruded into filaments. After cooling and solidification, gel fibers are formed, which are extracted by gasoline, dried by hot nitrogen, and subjected to three-stage heat drawing, and the total draw ratio is 40. Finally, a high strength and high modulus ultra high molecular weight polyethylene fiber is produced.
  • the fiber has a weight average molecular weight of about 4.5 million.
  • the fiber has a strength of 30 cN/dtex or more and a modulus of 960 cN/dtex or more.
  • the residence time of the material in the screw extruder was approximately 15 minutes.
  • a polyethylene powder having a weight average molecular weight of 5 million was introduced into the feed port through a hopper.
  • Powder feed rate is 0.5 Kg/min.
  • the solvent paraffin oil is metered by the rotameter from the storage tank and enters the feed port.
  • the feed rate of the solvent paraffin oil is 0.005 cubic meters per minute.
  • the two materials then enter the screw extruder, which is a single screw with a diameter of 80 mm, a screw length of 3,200 mm and a length to diameter ratio of 40.
  • the outer sleeve of the screw has a wall thickness of 15 mm and is electrically heated at a temperature of 140 °C.
  • the screw speed is 30 rpm and the motor is rated at 25 kW.
  • the metering pump is the JRG-1.2 metering pump produced by Shanghai Jingfang Chemical Fiber Machinery Factory.
  • the mixture was filtered through a filter, passed through a twin-screw extruder, spun, and extruded into filaments. After cooling and solidification, gel fibers are formed, which are extracted by gasoline, dried by hot nitrogen, and subjected to three-stage heat drawing, and the total draw ratio is 40. Finally, ultrahigh molecular weight polyethylene fibers are produced.
  • the fiber has a weight average molecular weight of about 4 million.
  • the residence time of the material in the screw extruder was approximately 25 minutes.
  • the linear polyethylene powder with a weight average molecular weight of 5 million was metered into the feed port of the screw extruder through a hopper, the feed rate of the powder was 0.1 kg/min, and the feed rate of the solvent decalin was 0.0015 m3/min. .
  • the screw extruder is a twin screw with a screw diameter of 60 mm, a screw length of 1000 mm, and a material of 38CrMoAlA alloy steel.
  • the outer sleeve wall of the screw is electrically heated and has a temperature of 140 °C.
  • the screw speed is 60 rpm and the motor power is 15 kW.
  • the static mixer uses a SX type twill plate type static mixer manufactured by Nantong Shendong Filter Manufacturing.
  • the metering pump is the JRG-1.2 metering pump produced by Shanghai Jingfang Chemical Fiber Machinery Factory.
  • the uniformly mixed ultrahigh molecular weight polyethylene solution was continuously fed through a three-stage static mixer-metering pump.
  • the mixture was filtered into a filter. Then enter the twin-screw extruder, spin through the box, extrude into a wire, and solidify by cooling to form a gel fiber. It is then dried by hot nitrogen at 70 degrees Celsius. After three stages of hot drawing, the total draw ratio is 40. Finally, a high strength and high modulus ultra high molecular weight polyethylene fiber is produced.
  • the fiber has a weight average molecular weight of about 4.4 million. The strength of the fiber is above 30 cN/dtex and the modulus is above 960 cN/dtex.
  • the linear polyethylene powder with a weight average molecular weight of 5 million was metered into the feed port of the screw extruder through a hopper, the feed rate of the powder was 0.1 kg/min, and the feed rate of the solvent decalin was 0.0015 m3/min. .
  • the screw extruder is a twin screw with a screw diameter of 60 mm and a screw length of 2000 mm.
  • the material is 38CrIvloAlA alloy steel.
  • the outer sleeve wall of the screw is electrically heated and has a temperature of 140 ⁇ .
  • the screw speed is 60 rpm and the motor power is 15 kW.
  • the metering pump is the JRG-1.2 metering pump produced by Shanghai Jingfang Chemical Fiber Machinery Factory.
  • the mixture was filtered into a filter. Then enter the twin-screw extruder, spin through the box, extrude into a wire, and solidify by cooling to form a gel fiber. Thereafter, it was dried by hot nitrogen at 70 degrees Celsius. After three levels of heat drawing, The total draw ratio is 40. Finally, ultrahigh molecular weight polyethylene fibers are produced. The fiber has a weight average molecular weight of about 3.9 million.
  • the linear polyethylene powder having a weight average molecular weight of 5 million was metered into the feed port of the screw extruder through a hopper, the feed rate of the powder was 0.5 kg / min, and the feed rate of the paraffin oil was 0.006 m 3 /min.
  • the material then enters the screw extruder.
  • the screw extruder is a twin screw with a diameter of 60 mm and a screw length of 900 mm.
  • the material is 38CrMoAlA alloy steel.
  • the outer sleeve wall of the screw is electrically heated at a temperature of 145 °C.
  • the screw speed is 50 rpm and the motor power is 10 kW.
  • the static mixer uses a SX type twill plate static mixer manufactured by Nantong Shendong Filter Manufacturing.
  • the metering pump is the JRG-1.2 metering pump produced by Shanghai Jingfang Chemical Fiber Machinery Factory.
  • the uniformly mixed ultrahigh molecular weight polyethylene solution was continuously fed through a two-stage static mixer-metering pump.
  • the mixture is filtered into a filter, and then introduced into a twin-screw extruder, which is extruded into a filament through a spinning box and solidified by cooling to form a gel fiber. After the toluene was extracted, it was purged with nitrogen. After three stages of hot drawing, the total draw ratio is 40. The finished product is finally produced.
  • the fiber has a weight average molecular weight of about 4.5 million. The strength of the fiber is above 30 cN/dtex, and the modulus is above 960 cN/dtex.
  • a polyethylene powder having a weight average molecular weight of 5 million was introduced into the feed port through a hopper.
  • the powder feed rate is 1.5 kg / min.
  • the solvent paraffin oil is metered by the rotameter from the storage tank and enters the feed port.
  • the feed rate of the solvent paraffin oil is 0.01 cubic meters per minute, and a small amount of antioxidant anti-oxidation 264, stabilizer salicylate is added to the solvent.
  • a flame retardant such as phosphate ester.
  • the two materials then enter the screw extruder, which is a twin screw with a diameter of 70 mm and a screw length of 1100 mm.
  • the outer sleeve of the screw has a wall thickness of 15 mm and is electrically heated at a temperature of 135 °C.
  • the screw speed is 60 rpm and the motor is rated at 20 kW.
  • the static mixer uses a SH-type enhanced static mixer manufactured by Nantong Shendong Filter Manufacturing.
  • the metering pump is the JRG-1.2 metering pump produced by Shanghai Jingfang Chemical Fiber Machinery Factory. After the first stage static mixer-metering pump, the ultra-high molecular weight polyethylene solution of the mixed hook is continuously sent out.
  • the mixture was filtered through a filter, passed to the next twin-screw extruder, spun, and extruded into filaments. After cooling and solidification, a gel fiber is formed, which is extracted by toluene extraction and hot nitrogen gas, and subjected to three-stage heat drawing, and the total draw ratio is 40. Finally, a high strength and high modulus ultra high molecular weight polyethylene fiber is produced.
  • the fiber has a weight average molecular weight of about 4.4 million. The strength of the fiber is above 30 cN/dtex and the modulus is above 960 cN/dtex.
  • a polyethylene powder having a weight average molecular weight of 5 million was introduced into the feed port through a hopper.
  • the feed rate of the powder is 1 Jin / minute.
  • the solvent paraffin oil is metered by the rotameter from the storage tank and enters the feed port.
  • the feed rate of the solvent paraffin oil is 0.01 cubic meters per minute, and a small amount of antioxidant anti-oxidation 264, stabilizer salicylate is added to the solvent.
  • a flame retardant such as phosphate ester.
  • the two materials then enter the screw extruder, which is a twin screw with a diameter of 80 mm, a screw length of 800 mm and an aspect ratio of 30.
  • the outer sleeve of the screw has a wall thickness of 15 mm and is electrically heated at a temperature of 135 °C.
  • the screw speed is 40 rpm and the motor is rated at 20 kW.
  • the static mixer uses a JHF static mixer produced by Nantong Shendong Filter Manufacturing.
  • the metering pump is the JRG-2.4 metering pump produced by Shanghai Jingfang Chemical Fiber Machinery Factory.
  • the uniformly mixed ultrahigh molecular weight polyethylene solution was continuously fed through a two-stage static mixer-metering pump.
  • the mixture was filtered through a filter, passed to the next twin-screw extruder, spun, and extruded into filaments. After cooling and solidification, gel fibers were formed, extracted with toluene, dried with hot nitrogen, and subjected to three-stage heat drawing, and the total draw ratio was 40. Finally, a high strength and high modulus ultra high molecular weight polyethylene fiber is produced.
  • the fiber has a weight average molecular weight of about 4.4 million. The strength of the fiber is above 30 cN/dtex and the modulus is above 960 cN/dtex.
  • a polyethylene powder having a weight average molecular weight of 6 million was introduced into the feed port through a hopper.
  • the feed rate of the powder was 1 kg / min.
  • the solvent paraffin oil is metered by the rotameter from the storage tank and enters the feed port.
  • the feed rate of the solvent paraffin oil is 0.01 cubic meters per minute.
  • the material enters the screw extruder.
  • the screw extruder is a twin screw with a diameter of 80 mm, a screw length of 2400 mm, a length to diameter ratio of 30, and a material of 38Q O alloy steel.
  • the outer sleeve of the screw has a wall thickness of 15 mm and is electrically heated to a temperature of 140 ⁇ .
  • the screw speed is 45 rpm and the motor is rated at 20 kW.
  • the static mixer uses a SL-type flow channel static mixer manufactured by Nantong Shendong Filter Manufacturing.
  • the metering pump is the JRG-2.4 metering pump produced by Shanghai Jingfang Chemical Fiber Machinery Factory.
  • the uniformly mixed ultrahigh molecular weight polyethylene solution is continuously fed through the first stage static mixer-metering pump.
  • the mixture was filtered through a filter, passed to the next twin-screw extruder, spun, and extruded into filaments. After cooling and solidification, gel fibers are formed, extracted with benzene, dried with hot nitrogen, and subjected to three-stage heat drawing, and the total draw ratio is 40. Finally, a high strength and high modulus ultra high molecular weight polyethylene fiber is produced.
  • the fiber has a weight average molecular weight of about 5.3 million. The strength of the fiber is above 30 cN/dtex and the modulus is above 960 cN/dtex.
  • the linear polyethylene powder with a weight average molecular weight of 5.5 million was metered into the feed port of the screw extruder through a hopper, the feed rate of the powder was 0.15 kg/min, and the solvent tetrahydronaphthalene feed rate was 0.001 m3/min. .
  • the screw extruder was a twin screw with a screw diameter of 60 mm and a screw length of 480 mm.
  • the outer sleeve wall of the screw is powered Heating, the temperature is 140 ° C.
  • the screw speed is 70 rpm and the motor power is 15 kW.
  • the static mixer uses a SX type twill plate type static mixer produced by Nantong Shendong Filter Manufacturing.
  • the metering pump is the JRG-1.2 metering pump produced by Shanghai Jingfang Chemical Fiber Machinery Factory.
  • the uniformly mixed ultrahigh molecular weight polyethylene solution is continuously sent through the three-stage static mixer-metering pump.
  • the mixture was filtered into a filter. Then enter the twin-screw extruder, spin through the box, extrude into a wire, and solidify by cooling to form a gel fiber. It was dried by hot nitrogen at 70 °C. After three stages of hot drawing, the total draw ratio is 40. Finally, a high strength and high modulus ultra high molecular weight polyethylene fiber is produced.
  • the fiber has a weight average molecular weight of about 4.7 million. The strength of the fiber is above 30 cN/dtex and the modulus is above 960 cN/dtex.

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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Textile Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Artificial Filaments (AREA)
  • Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)

Abstract

L'invention concerne un procédé de production en continu d'une solution de polyéthylène de poids moléculaire ultraléger. Selon le procédé, une poudre de polyéthylène de poids moléculaire ultraléger et un solvant sont acheminés en continu jusqu'à une trémie. La matière de la trémie est ajoutée à une extrudeuse à vis possédant une largeur/un diamètre de petite taille. La matière extrudée à partir de l'extrudeuse est, ensuite, chargée dans un mixeur statique et mélangée. Ainsi, est obtenue, du statique mixeur, la solution de polyéthylène unifiée de poids moléculaire ultraléger. Selon cette invention, ce mixeur statique permet de préparer et de mélanger en continu la solution. Il permet d'économiser de l'espace, du temps et de réduire l'intensité du travail. Le procédé de cette invention permet, en outre, d'accroître la concentration de la solution, ce qui permet de diminuer la quantité à extraire, ainsi que les coûts de production.
PCT/CN2005/001989 2004-11-29 2005-11-24 Procede de production en continu d'une solution de polyethylene de poids moleculaire ultraleger Ceased WO2006056128A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
CNB2004100960765A CN1256366C (zh) 2004-11-29 2004-11-29 超高分子量聚乙烯溶液的连续配制混合方法
CN200410096076.5 2004-11-29

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CN108441971A (zh) * 2018-05-23 2018-08-24 史小军 高强高模聚乙烯纤维纺丝原液制备装置
CN108560063A (zh) * 2018-02-07 2018-09-21 浙江千禧龙纤特种纤维股份有限公司 一种uhmwpe纤维溶解和混炼工艺

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CN101153079B (zh) * 2006-09-29 2010-05-12 上海化工研究院天地科技发展有限公司 一种纺丝用超高分子量聚乙烯的预处理方法
MX2009012564A (es) * 2007-05-23 2009-12-09 Dsm Ip Assets Bv Sutura coloreada.
CN101956238B (zh) * 2010-08-24 2012-05-30 北京同益中特种纤维技术开发有限公司 一种超高分子量聚乙烯纤维纺丝溶液的制备方法
CN101967686B (zh) * 2010-09-21 2012-04-25 中国科学院宁波材料技术与工程研究所 一种超高分子量聚乙烯纤维纺丝溶液的制备方法
CN103465452A (zh) * 2012-06-07 2013-12-25 常州市永明机械制造有限公司 塑料挤出草坪单丝机组
CN103554523A (zh) * 2013-10-24 2014-02-05 中国科学院化学研究所 一种利用绿色可再生溶剂溶解聚烯烃的方法
CN109366780A (zh) * 2018-11-19 2019-02-22 镇江康源新材料科技有限公司 一种高分子材料混料挤出装置
CN111074358A (zh) * 2019-12-31 2020-04-28 中国纺织科学研究院有限公司 双计量输送法制备聚乙烯纤维的方法
CN111389288A (zh) * 2020-03-30 2020-07-10 上海青昀新材料科技有限公司 一种将聚合物溶解到溶剂中的方法及设备
AT523528B1 (de) * 2020-07-27 2021-09-15 Haubner Alexander Holz-Kunststoff-Verbundwerkstoff
CN112921426B (zh) * 2021-01-29 2023-04-25 江苏厚生新能源科技有限公司 一种基于金属骨架的阻燃聚乙烯复合面料及其制备工艺
CN114381811A (zh) * 2021-12-21 2022-04-22 北京同益中新材料科技股份有限公司 一种原液着色超高分子量聚乙烯纤维纺丝母液的制备方法

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