CN115490890A - Preparation method of thermoplastic cross-linked polyethylene resin - Google Patents
Preparation method of thermoplastic cross-linked polyethylene resin Download PDFInfo
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- CN115490890A CN115490890A CN202211243037.8A CN202211243037A CN115490890A CN 115490890 A CN115490890 A CN 115490890A CN 202211243037 A CN202211243037 A CN 202211243037A CN 115490890 A CN115490890 A CN 115490890A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/24—Crosslinking, e.g. vulcanising, of macromolecules
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- 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
- B29B7/00—Mixing; Kneading
- B29B7/02—Mixing; Kneading non-continuous, with mechanical mixing or kneading devices, i.e. batch type
- B29B7/06—Mixing; Kneading non-continuous, with mechanical mixing or kneading devices, i.e. batch type with movable mixing or kneading devices
- B29B7/10—Mixing; Kneading non-continuous, with mechanical mixing or kneading devices, i.e. batch type with movable mixing or kneading devices rotary
- B29B7/12—Mixing; Kneading non-continuous, with mechanical mixing or kneading devices, i.e. batch type with movable mixing or kneading devices rotary with single shaft
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2323/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2323/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
- C08J2323/04—Homopolymers or copolymers of ethene
- C08J2323/06—Polyethene
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Abstract
The invention discloses a preparation method of thermoplastic cross-linked polyethylene resin (TPEXa), which takes high-density polyethylene resin (HDPE) or heat-resistant polyethylene resin (PERT) as raw material resin, adopts peroxide to carry out dynamic synchronous cross-linking modification, the obtained product is TPEXa resin, the comprehensive performance of the TPEXa resin is superior to that of PERT II and is close to that of PEX, because the thermoplasticity is reserved, the TPEXa resin can be extruded, injected, blow molded and the like, waste products can be hot-melted and reproduced, a pipe made of the TPEXA resin can be hot-melted and welded, the preparation method is low-carbon and environment-friendly, main equipment used for dynamic synchronous cross-linking is common general equipment, a plastic molding processing enterprise is easy to implement, and the implementation advantage of the HDPE raw material synthesis enterprise is greater.
Description
Technical Field
The invention belongs to the technical field of plastic processing, and particularly relates to a preparation method of modified plastic, in particular to a dynamic crosslinking preparation method of peroxide crosslinked thermoplastic crosslinked polyethylene resin (TPEXa).
Background
The crosslinking technology is an important effective method for modifying PE. The deep crosslinking of PE, the linear PE macromolecules mostly form a network structure, are insoluble and infusible, and completely lose thermoplasticity, is called crosslinked Polyethylene (PEX). The crosslinking of PEX is classified according to ISO 15875:
PEXa, a peroxide crosslinked product of HDPE;
PEXb, a silane crosslinked product of HDPE;
PEXc, a high energy ray irradiation crosslinked product of HDPE;
PEXd, azo-crosslinked product of HDPE.
During the crosslinking process of PEXa, no relative motion is allowed between the macromolecular chains of PE, which is called static crosslinking. Static cross-linking is further divided into static synchronous cross-linking and static post-cross-linking, for example, a PEXa (polyethylene-acrylic) pipe or profile by extrusion molding of a plunger type extruder is adopted, melting, plasticizing, molding and cross-linking processes of materials are completed in a slit of a machine head of the extruder at the same time, the processes are called static synchronous cross-linking, when the processes are completed, a product parison moves integrally in the slit of the machine head and is pushed out of a neck mold for molding and freezing, and relative motion does not occur between macromolecular chains; for another example, in the continuous extrusion molding of PEXa tube by screw extruder, the melting and plasticizing of the material are completed in the extruder, and the molding of the parison is completed in the slit of the head, and in the extruder or the slit of the head, theoretically, the cross-linking reaction is not allowed to occur, and the relative motion between the macromolecular chains of the material is allowed. But the product parison is discharged from the neck mold and enters a high-temperature crosslinking region for crosslinking reaction until the product parison is shaped and frozen, and at the moment, relative motion among macromolecular chains of the material is not allowed to occur, which is called static post-crosslinking. PEXa can be static synchronous crosslinking, also can be static postcrosslinking, but in the crosslinked process, the relative motion is not allowed to take place between the macromolecular chains of the material, if the relative motion takes place, because lose the thermoplastic that can weld gradually between the macromolecular chains, will unable the shaping.
The present inventors have invented a peroxide crosslinked thermoplastic crosslinked polyethylene (TPEXa) resin by peroxide micro-crosslinking PE. Wherein a small part of PE macromolecular chains are subjected to crosslinking reaction, most of the PE macromolecular chains are only subjected to chain growth, and the PE macromolecular chains are mutually entangled to form a final product which is soluble and meltable and still maintains thermoplasticity. The heat resistance and the creep resistance of the thermoplastic elastomer are improved, and the thermoplastic property is still kept. It can be used for processing and forming by extrusion, injection and the like in the same forming and processing method as common PE, and the comprehensive performance is superior to PERT II and PEX.
The preparation of the TPEXA resin continues to use the PEXa static cross-linking method, which comprises the static synchronous cross-linking by adopting a plunger type extruder and the static post-cross-linking by adopting a screw type extruder, and has the disadvantages that: the former has low efficiency, the granulation of the latter resin only can be strip granulation, the fillet of the prepared TPEXa resin particles is obvious, even the phenomenon of particle connection can occur, and the TPEXa resin particles are not beneficial to material conveying; the process equipment is complex, the process flow is long, and the operation is difficult; both are not conducive to mass production.
Disclosure of Invention
The invention aims to solve the technical problem of providing a preparation method of thermoplastic cross-linked polyethylene resin (TPEXa) aiming at the defects of the prior art, which takes high-density polyethylene resin (HDPE) or heat-resistant polyethylene resin (PERT) as raw material resin, adopts peroxide to carry out dynamic synchronous cross-linking modification, obtains TPEXa resin as a product, has comprehensive performance superior to PERT II and close to PEX, can carry out extrusion molding, injection molding, blow molding and the like due to the reservation of thermoplasticity, can carry out hot melting and reproduction on waste products, can carry out hot melting welding on a pipe made of the TPEXa resin, is low-carbon and environment-friendly, uses common general equipment as main equipment for dynamic synchronous cross-linking, is easy to implement by plastic molding and processing enterprises, and has greater implementation advantages by HDPE raw material synthesis enterprises.
The technical problem to be solved by the invention is realized by the following technical scheme:
a process for preparing thermoplastic cross-linked polyethylene resin (TPEXa) includes such steps as adding organic peroxide cross-linking agent, antioxidizing agent and other functional assistants to high-density polyethylene resin (HDPE) or heat-resistant polyethylene resin (PERT), and dynamic synchronous cross-linking modification.
The raw material resin, the organic peroxide cross-linking agent, the antioxidant and other functional auxiliaries are blended to be uniform, and then are subjected to initial melt blending, and then the cross-linking process is completed while the melt blending is continued.
The HDPE resin has a density of more than 0.945g/cm 3 The weight average molecular weight is 20-26 ten thousand, the heat-resistant polyethylene resin is provided with an alpha carrying chain, and the raw material resin comprises powder materials or granular materials;
the crosslinking modification refers to a process that the crosslinking agent is heated and decomposed to generate free radicals and deprives hydrogen carried by PE macromolecules, and then the PE macromolecules generate the free radicals and generate a bridging reaction.
The dynamic synchronous crosslinking modification is completed in the relative motion of PE macromolecular chains.
The dynamic synchronous crosslinking adopts a second-order single-screw extruder set, when the raw material resin is granular, the screw of the extruder 1 is a BM type separation screw, L/D = 20-24, the compression ratio is 3.0-3.2, and the screw is cooled to bear the melting and blending of materials; the screw of the extruder 2 is a screw with equal moment and unequal depth and gradual change, L/D =20, the compression ratio is 3.0-3.2, and the blending, crosslinking and molding of materials are borne; when the raw material resin is powder, the screw of the extruder 1 is a gradual change screw with a mixing head, L/D = 28-30, the compression ratio is 4.2-5.0, forced feeding and screw cooling are carried out, melt blending of the materials is carried out, the screw of the extruder 2 is a gradual change screw with equal moment and unequal depth, L/D =24, the compression ratio is 3.0-3.2, and blending and crosslinking forming of the materials are carried out. Or the dynamic synchronous crosslinking adopts a continuous mixing unit, the continuous mixing unit comprises a mixing unit and an extruder, the mixing unit undertakes the blending of materials, and the extruder undertakes the crosslinking molding of the materials. Or the dynamic synchronous crosslinking is carried out by adopting a co-rotating parallel double-screw extruder with an exhaust function to carry out melt blending crosslinking molding, wherein L/D =40, the front section of the extruder mainly finishes melt blending plasticization, and the rear section of the extruder mainly finishes blending crosslinking molding.
The preparation method of the thermoplastic crosslinked polyethylene resin adopts a dynamic synchronous crosslinking technology of melt blending of a double-stage screw extruder or a continuous banburying machine set or a parallel co-rotating double screw machine set with a large length-diameter ratio to carry out micro crosslinking modification on HDPE resin, and PE macromolecular chains complete a blending process and a crosslinking process including melting, plasticizing and forming in relative motion, thereby reducing working procedures, shortening process flow, and breaking through the traditional theory and idea that DYBP is the only peroxide crosslinking agent for HDPE crosslinking and the crosslinking modification of HDPE can only be static crosslinking.
The technical solution of the present invention will be described in detail with reference to the accompanying drawings and specific embodiments.
Drawings
FIG. 1 is a process flow diagram of the method for preparing a thermoplastic crosslinked polyethylene resin according to the present invention.
Detailed Description
FIG. 1 is a process flow diagram of the method for preparing a thermoplastic crosslinked polyethylene resin according to the present invention. As shown in figure 1, in the preparation of the TPEXa resin, the raw materials and auxiliary materials are metered according to the formula and then are mixed uniformly, and the TPEXa resin can be prepared by adopting a large length-diameter ratio exhaust type parallel co-rotating twin-screw extruder for melt blending and crosslinking molding, a double-stage single-screw extruder unit for melt blending and crosslinking molding or a continuous mixing unit for melt blending and crosslinking molding.
The blending temperature is strictly controlled, a high-speed mixer can be used as blending equipment, the high-speed mixer is required to be provided with a cooling jacket, the blending temperature can be guaranteed not to exceed 35 ℃, a gravity batching system can also be used, and the blending process is finished under the protection of inert gas nitrogen or carbon dioxide.
The melt blending and crosslinking molding, wherein the melt blending and crosslinking molding are divided into a primary melt blending stage and a melt blending and crosslinking molding stage, and the blending temperature of the primary melt blending stage is higher than the melting temperature of HDPE or PERT resin and is close to or lower than the decomposition temperature of a peroxide crosslinking agent; in the melt blending crosslinking molding stage, the blending temperature is higher than the melting temperature of the used HDPE resin and the decomposition temperature of the peroxide crosslinking agent with half-life of one minute, and is determined according to the requirement of crosslinking speed; cut grain, including two kinds of schemes of cooling cutting grain and cutting grain cooling, the brace is cut grain and is belonged to the cooling and cut grain, and water ring cuts grain and cuts grain then and cut grain cooling under water.
In FIG. 1, the PE resin is HDPE or PERT resin, the crosslinking agent is BiBP or DTBP or DYBP or DBPH or two or more peroxide composite crosslinking agents and assistant crosslinking agents TAC or TAIC, a main antioxidant, an auxiliary antioxidant and a functional assistant; blending by a high-speed mixer at normal temperature. When a co-rotating parallel double-screw extruder with the length-diameter ratio of more than 40 and an exhaust function is adopted for preparing the TPEXa resin, the material is subjected to preliminary melt blending at the front section of an exhaust port of the extruder, and the material is subjected to blending crosslinking and shaping at the rear section of the exhaust port. When a continuous mixing unit is adopted, the continuous mixing machine only completes the preliminary melting of the materials, and an extruder of the continuous mixing unit undertakes the blending, crosslinking and shaping of the materials. When a second-order single-screw extruder set is adopted, the extruder 1 bears the primary melt blending of materials, and the extruder 2 bears the blending, crosslinking and shaping of the materials.
The pellets may be cooled pellets, such as strand pellets; or the granules can be cooled, such as water ring granules and underwater granules.
And (4) inspecting, collecting the uniform particles for later use, and returning the particles with particles to the blender.
HDPE is deeply crosslinked into PEX, and many properties such as heat resistance, creep resistance, tensile strength and the like are greatly improved, for example, the temperature of the HDPE water delivery pipe is not higher than 40 ℃, after crosslinking modification, the temperature of the delivered water can reach 70 ℃, and the deduced service life can reach 50 years; however, the thermoplastic property of the deep cross-linked HDPE is lost, the PEX pipe made of the deep cross-linked HDPE cannot be connected by a hot-melting method, and the waste materials cannot be reproduced by the hot-melting method. TPEXa resins, many of which have significantly improved properties over HDPE or PERT resins, most importantly have higher thermal strength and higher creep resistance than PERT II, which is close to PEX. Although slightly lower than PEX, TPEXa still retains the thermoplasticity of HDPE or PERT, and the manufactured pipes can be welded and connected by a hot melting method, and the waste materials can also be reproduced by the hot melting method, which is incomparable with PEX.
TPEXa resin has high melt strength, can be used for manufacturing closed-cell PE foam plastics, and does not need to perform additional crosslinking modification on PE resin; the extrusion molding method is used for extrusion molding of large-caliber solid-wall pipes and blow molding of large hollow containers, and can effectively overcome the defect of uneven wall thickness caused by molten sag.
The TPEXa resin has high creep resistance, is used for manufacturing injection molding plastic trays, and can improve the compression creep resistance of the plastic trays.
TPEXa resin has good wear resistance and can be used for manufacturing water pipelines with high solid content.
TPEXa has high heat resistance and good wear resistance, is used for manufacturing the oil extraction plastic-lined pipe, and has better heat resistance and wear resistance than UHMWPE.
TPEXa resin has high melt strength, high heat resistance and high creep resistance, can be used for extrusion molding of plastic pipes, and the pipes can be used in hot water systems; because of good weldability, the composite material is used for manufacturing a working pipe of a heat distribution pipeline, and has advantages over PERT and PEX;
the TPEXa resin can almost replace HDPE, PERT and PEX, can be formed by various processing methods such as extrusion, injection, blow molding, die pressing and the like, can be subjected to hot melt welding, can be recycled as waste materials, and has the advantages of being more than those of HDPE, PERT ll and PEX. Therefore, the development of a preparation method for manufacturing the TPEXa resin is more general.
Example 1
PERT II (granule) 99.93%
DBPH 0.07％
Proper amount of other auxiliary agents
And melting, blending, crosslinking, forming and granulating by using a second-order single-screw extruder set.
The second-order single-screw extruder unit is characterized in that: the extruder 1 is a BM type separation screw, L/D = 20-24, the compression ratio is 3.0-3.2, the screw is cooled and bears the melting and blending of materials, the temperature of each zone of the extruder 1 is set to be 100 ℃ in the zone I, 145 ℃ in the zone III and the subsequent zones of the extruder 1, the rotating speed of the screw is 40-90 rpm, the screw of the extruder 2 is an equi-torque non-equal-depth gradually-changed screw, L/D =20, the compression ratio is 3.0-3.2 and bears the blending and crosslinking molding of materials, the temperature of each zone of the extruder 2 is 160 ℃ in the zone I, 190 ℃ in the zone II, 230 ℃ in the zone III and 220 ℃ in the zone IV, and the rotating speed of the screw is matched with that of the extruder 1. The material is molded into a strip through a porous machine head and is cooled and cut into granules or cut into granules and cooled to obtain dynamic synchronous crosslinking TPEXa resin particles for later use. The porous handpiece is characterized in that: the cross direction of the holes of the strand and grain cutting porous machine head should keep a certain distance.
Example 2
The method adopts a co-rotating parallel double-screw extruder with an exhaust function to perform melt blending and crosslinking molding, wherein L/D =40, the front section of the extruder mainly completes melt blending and plasticizing, and the rear section of the extruder mainly completes blending and crosslinking molding. The temperature of each zone before the air outlet of the extruder is 130-160 ℃, the temperature of each zone after the air outlet is gradually increased to 240 ℃ from 170 ℃, and the materials are formed into strips through a porous machine head and cooled and granulated or granulated and cooled to obtain the dynamic synchronous crosslinked TPEXa resin particles for later use. The porous handpiece is characterized in that: the holes of the brace grain-cutting porous machine head are transversely kept at a certain interval;
example 3
Adopting a continuous mixing unit to melt, blend, crosslink, mold and cut into particles.
Blending and crosslinking adopt a continuous mixing unit, the continuous mixing unit is used for blending materials, and the mixing temperature is strictly controlled at 138-145 ℃;
the extruder is used for carrying out cross-linking molding on the materials, the temperature of each area of the extruder is gradually increased to 230 ℃ from 155 ℃, the materials are molded into strips through a porous machine head and are cooled and cut into particles or are cooled, and the dynamic synchronous cross-linked TPEXa resin particles are obtained for later use. The holes of the multi-hole machine head are transversely kept at a certain interval;
example 4
And melting, blending, crosslinking, forming and granulating by using a second-order single-screw extruder set.
The screw of the second-order single-screw extruder unit, the extruder 1, its screw is a gradual change screw with mixing head, L/D = 28-30, its compression ratio is 4.2-5.0, force feed, screw cooling, undertake the melting and blending of the supplies, the temperature of every area of the extruder 1 is set as I area 100 degrees, II area III area and following area 155 degrees, the rotational speed of the screw is 40 rpm-90 rpm, the extruder 2, its screw is a gradual change screw with equal moment and unequal depth, L/D =24, its compression ratio is 3.0-3.2, undertake the blending and crosslinking molding of the supplies, the temperature of every area of the extruder 2 is I area 160 degrees, II area 190 degrees, III area 240 degrees, IV area 230 degrees, the rotational speed of the screw matches with that of the extruder 1. The material is molded into a strip through a porous machine head and is cooled and cut into granules or cut into granules and cooled to obtain dynamic synchronous crosslinking TPEXa resin particles for later use. The porous handpiece is characterized in that: the transverse direction of the holes of the brace grain cutting porous machine head is kept with a certain interval;
the resin particles can be used for extrusion molding of plastic pipes with high temperature resistance, blow molding to obtain large TPEXA hollow containers with uniform wall thickness, injection molding to obtain plastic products with strong creep resistance such as plastic trays, addition of foaming agents and the like to prepare closed-cell PE foamed plastics, and addition of auxiliaries such as electric conduction, heat conduction and flame retardance to achieve continuous modification with the aim of endowing new functions.
Comparative example 1
PERT (commercially available granule) 99.93%
BiBP 0.07％
Proper amount of other auxiliary agents
A common single-screw extruder is adopted, the L/D =32, the screw type is a gradual change screw with a mixing head, the temperature of each zone of the extruder is 130 ℃ in the I zone, 160 ℃ in the II zone, 190 ℃ in the III zone, 220 ℃ in the IV zone, 220 ℃ in the V zone, and the strand is cut into granules.
Comparative example 2
The material melting blending molding adopts an exhaust type co-rotating parallel double screw extruder, the temperature of each section of the extruder is controlled below 168 ℃, the material is molded into a strip through a porous machine head, enters a post-crosslinking furnace for high-temperature crosslinking, and is cooled and cut into granules, so as to obtain the static post-crosslinked TPEXa granules.
Table one: summary of data for examples and comparative examples
Claims (6)
1. A preparation method of thermoplastic cross-linked polyethylene resin is characterized in that high-density polyethylene resin or heat-resistant polyethylene resin is used as raw material resin, organic peroxide cross-linking agent, antioxidant and other functional auxiliaries are added, and the thermoplastic cross-linked polyethylene resin is prepared through dynamic synchronous cross-linking modification; wherein the melting, blending, plasticizing, molding and crosslinking of the materials are simultaneously completed.
2. The method for preparing a thermoplastic crosslinked polyethylene resin according to claim 1, wherein the raw material resin, the organic peroxide crosslinking agent, the antioxidant and other functional additives are blended to be uniform, and then the raw material resin, the organic peroxide crosslinking agent, the antioxidant and the other functional additives are initially melt-blended and then the crosslinking process is completed while continuing the melt-blending.
3. The method of claim 1, wherein the raw material resin has a weight-average molecular weight of 22 to 26 ten thousand and a density of more than 0.945g/cm 3 The HDPE resin of (1).
4. The method for preparing thermoplastic crosslinked polyethylene resin according to claim 1, wherein the dynamic synchronous crosslinking is performed by using a two-stage single-screw extruder set, when the raw material resin is in the form of particles, the screw of the extruder 1 is a BM type separation screw, L/D = 20-24, the compression ratio is 3.0-3.2, and the screw is cooled to undertake melt blending of materials; the screw of the extruder 2 is a screw with equal moment and unequal depth and gradual change, L/D =20, the compression ratio is 3.0-3.2, and the blending, crosslinking and molding of materials are borne; when the raw material resin is powder, the screw of the extruder 1 is a gradual change screw with a mixing head, L/D = 28-30, the compression ratio is 4.2-5.0, forced feeding and screw cooling are carried out, melt blending of the materials is carried out, the screw of the extruder 2 is a gradual change screw with equal moment and unequal depth, L/D =24, the compression ratio is 3.0-3.2, and blending and crosslinking forming of the materials are carried out.
5. The method of claim 1, wherein the dynamic synchronous crosslinking is performed by using a continuous mixer set comprising a mixer set and an extruder, the mixer is used for blending materials, and the extruder is used for crosslinking and molding materials.
6. The method for preparing thermoplastic crosslinked polyethylene resin according to claim 1, wherein the dynamic synchronous crosslinking is performed by melt blending and crosslinking molding using a co-rotating parallel twin-screw extruder with venting function, wherein L/D =40, the former stage mainly performs melt blending and plasticizing, and the latter stage mainly performs blend crosslinking and molding.
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