CN115678084B - Single-polyester reinforced foaming composite lightweight material and preparation method thereof - Google Patents
Single-polyester reinforced foaming composite lightweight material and preparation method thereof Download PDFInfo
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Classifications
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
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- Manufacture Of Porous Articles, And Recovery And Treatment Of Waste Products (AREA)
Abstract
The invention discloses a single-polyester reinforced foaming composite lightweight material and a preparation method thereof, wherein the raw materials of the single-polyester reinforced foaming composite lightweight material consist of main materials, auxiliary materials and foaming agents; the main material consists of polyester resin and polyester fiber, wherein the polyester resin: polyester fiber=100:0 to 70:30 by weight ratio; the auxiliary materials consist of a chain extender, an antioxidant and a nucleating agent; the auxiliary material accounts for 0.1 to 5 percent of the weight of the main material; the foaming agent accounts for 0.5-5% of the weight of the main material; and mixing the main materials, the auxiliary materials and the foaming agent, extruding to obtain the single-polyester foam, and cooling to obtain the single-polyester reinforced foaming composite lightweight material. The invention reduces the complexity of the production process by a one-step method, improves the production efficiency, and prepares the single-polyester composite material with lighter weight and higher strength.
Description
Technical Field
The invention relates to the field of preparation of a single-polyester foaming composite lightweight material, in particular to a single-polyester reinforced foaming composite lightweight material and a preparation method thereof.
Background
With the rapid development of industries such as aerospace, national defense, energy, traffic, construction, packaging, electrical appliances, sports equipment and the like in China, the demand for lightweight high-performance materials is more and more urgent. The early stage of the lightweight technology mainly comprises the step of replacing steel with plastic. Currently, high molecular weight lightweight materials mainly include two types: (1) high-performance polymer foaming material; (2) fiber reinforced composite polymer material.
Conventional fiber reinforced composites are mostly reinforced with Glass Fibers (GF), carbon Fibers (CF), etc. However, since the reinforcing fibers and the matrix resin are heterogeneous materials, the compatibility is poor, and thus the overall performance of the composite material is easily degraded due to poor interfacial bonding. In addition, the separation of different types of reinforcing fibers and matrixes during composite material recovery is difficult, so that the difficulty of material recovery and reutilization is high, the efficiency is low, the cost is high, and the recycling and regenerating capacity of composite material products is severely limited. Although patent CN102152589a prepared a mono-Polyester (PET) composite lightweight material by hot pressing a low melting point polyester resin and a polyester fiber cloth, foaming was not involved and the molding cycle was long. The literature (Journal of Applied Polymer Science,2020,137 (41): 49268-49284) prepares LCB-PET with high melt strength by twin-screw extrusion modification through mixing a chain extender and fiber-grade PET, and single-screw extrusion foaming is carried out with the aid of scCO 2 by taking the LCB-PET as a raw material. The cell diameter and cell density of the sample were moderate, but the electron microscopy image showed that the cell walls of the foam were thicker. The method uses a single PET for foaming, and the foam cells are nonuniform in size and poor in foaming effect due to low melt strength. Document (Composites Part A: APPLIED SCIENCE AND Manufacturing,2009,40 (11): 1747-1755) reports PET mono-polyester composites prepared using PET, low melting point co-polyester films. Based on the temperature difference of the melting points of the copolyester film, good interfacial adhesion is achieved when the PET tape/copolyester film assembly is hot pressed. The method only uses polyester fiber to improve the tensile strength of PET, but the improvement effect is not obvious, the foaming technology is not involved in weight reduction, and the production process is complex.
The single polymer composite material (SPCs) is a high polymer material with the same chemical components as the matrix and the reinforcing material, the compatibility between the matrix and the reinforcing material is good, the interface problem of the traditional fiber composite material does not exist, and the high orientation of the fiber material molecular chains in the SPCs composite material enables the material to have enough initial strength, so that the SPCs are endowed with more excellent specific rigidity, specific strength, low density and other characteristics, and particularly, the improvement on impact toughness and elongation at break is more remarkable. In addition, the matrix and the reinforcing material are the same polymer, which is more favorable for recycling materials and meets the current requirement of green recycling economy, thus becoming a hot spot for the current composite material research.
The polypropylene single polymer composite material is prepared by an insert injection molding process from polypropylene fibers treated with hot silicone oil and polypropylene in literature (Composites SCIENCE AND Technology,2015, 106:47-54). The mechanical properties of the composite material are enhanced by using a fiber-reinforced method only, and foaming light weight treatment is not carried out. Literature (Composites: part A,2016, 90:567-576) reports the use of polypropylene and polypropylene fibers to prepare PP homopolymer foam by embedded micro-pore molding, but the weight reduction effect is not significant, with a maximum weight reduction of only 15.2%. Although the technology couples the single polymer and the foaming technology, the layering between the fiber and the matrix after foaming is obvious, and the improvement of the mechanical property is not obvious. The foaming process of the monopolyester material is not found in the foaming process of the monopolyester material, and the foaming effect of other monopolyester is not obvious.
Compared with the traditional foaming materials such as polystyrene, polyurethane, polyvinyl chloride and the like, the polyester foaming material has the advantages of light weight, excellent mechanical property and fatigue resistance, good gas barrier property, recycling, low price and the like, and has wide application prospect in the fields of building materials, automobile and aerospace industries, wind power generation and the like. On the other hand, the prior art mainly adopts carbon fiber and glass fiber reinforcement technology, which makes recycling of materials difficult after use. In addition, there are single polymer reinforced composite materials, but at the same time, there are few foaming lightweight couplings involved, and the foaming ratio is not high, and the effect is not good. The prior art does not see the combination of reinforcement and foaming of polyester-based materials, and thus it is necessary to investigate a way to produce a mono-polyester foam material efficiently.
At present, relatively mature SPCs are developed in the industry, and SPCs products with Polypropylene (PP) as a main material are mainly proposed by Propex Fabrics Inc. and the like. The reinforcement (fiber) and the continuous phase substrate (resin) of the PP-SPCs are PP, so that all problems caused by heterogeneous characteristics of the fiber and the substrate in the traditional composite material are solved, the advantage of relatively low cost is achieved, and the PP-SPC has the characteristic of post-processing. However, polypropylene is a nonpolar substance, and has a stable surface and is not easily reacted with other substances. An excessively stable surface is disadvantageous in that the polypropylene polymer sheet is bonded (glued, adhered) with other materials or surface-coated, and thus causes a disadvantage in that it is difficult to process it later.
At present, the conventional polyester resin has the defects of poor melt strength, slow crystallization rate, easy degradation, difficult foam molding and the like due to the characteristics of low linear molecular structure and low molecular weight in the polyester foaming process, and cannot be directly applied to the preparation of polyester foaming materials. It is generally desirable to increase the melt strength of polyesters by increasing the molecular weight and its distribution, introducing long chain branching structures, blending with other components, and the like, in order to improve their foaming properties.
Disclosure of Invention
The invention aims to solve the technical problem of providing a single-polyester reinforced foaming composite lightweight material and a preparation method thereof.
According to the invention, the polyester fiber reinforcement and the reactive extrusion/injection foaming are combined to prepare the single-polyester composite material, and the technology reduces the complexity of a production process by a one-step method, improves the production efficiency, and prepares the single-polyester composite material with lighter weight and higher strength.
In order to solve the technical problems, the invention provides a preparation method of a single-polyester reinforced foaming composite lightweight material, which comprises the following steps: the raw materials of the single-polyester reinforced foaming composite lightweight material consist of main materials, auxiliary materials and foaming agents; the main material consists of polyester resin and polyester fiber, wherein the polyester resin: polyester fiber = 100:0 to 70:30 (preferably 95:5 to 70:30) by weight ratio;
The auxiliary materials consist of a chain extender, an antioxidant and a nucleating agent; the auxiliary material accounts for 0.1 to 5 percent of the weight of the main material;
The foaming agent accounts for 0.5-5% of the weight of the main material;
And mixing the main materials, the auxiliary materials and the foaming agent, extruding to obtain the single-polyester foam, and cooling to obtain the single-polyester reinforced foaming composite lightweight material.
The mixing reaction is at least one of extrusion preparation, injection molding preparation, bead foaming and hot press molding.
The preparation method of the single polyester reinforced foaming composite lightweight material is improved:
the polyester resin is 70-100 percent (preferably 70-95 percent) of the weight of the main material, and the melting point is 210-260 ℃;
The polyester fiber accounts for 0 to 30 percent (preferably 5 to 30 percent) of the weight of the main material, and the melting point of the polyester fiber is 250 to 265 ℃;
the chain extender is at least one of functional ionic liquid, multifunctional anhydride compounds, multifunctional hydroxyl compounds, multifunctional amino compounds and multifunctional epoxy compounds;
The antioxidant is at least one of an antioxidant 1010, an antioxidant 168, an antioxidant 1425 and an antioxidant 1098;
The nucleating agent is at least one of talcum powder, silicon dioxide, titanium dioxide, nano calcium carbonate, montmorillonite and kaolin;
The foaming agent is one or more of supercritical fluids with critical temperature lower than the melting point of polyester.
As a further improvement of the preparation method of the single polyester reinforced foaming composite lightweight material, the invention has the following advantages:
The polyester resin is preferably PET resin with a melting point of 220-255 ℃;
The polyester fiber is preferably PET fiber with a melting point of 260-265 ℃;
the functional ionic liquid has three or more hydroxyl groups, amino groups or carboxyl groups, and the ionic liquid has affinity to CO 2, so that the solubility of CO 2 in resin melt can be improved.
As a further improvement of the preparation method of the single polyester reinforced foaming composite lightweight material, the invention has the following advantages:
The functional ionic liquid is preferably tetra (2-hydroxyethyl) ammonium bromide and triethanolamine hydrochloride;
The polyfunctional acid anhydride compound is preferably pyromellitic dianhydride (PMDA);
The polyfunctional hydroxyl compound is preferably glycerol or pentaerythritol series;
the polyfunctional amino compound is preferably ethylenediamine, ethylenediamine tetraacetic acid series;
the multifunctional epoxy compound is preferably triglycidyl isocyanurate (TGIC) or Joncryl ADR series.
As a further improvement of the preparation method of the single polyester reinforced foaming composite lightweight material, the invention has the following advantages:
The supercritical fluid is supercritical carbon dioxide, and contains at least one (one or a combination of more) of isopentane, cyclopentane, hexane and heptane with the mass fraction of 0-10% as an entrainer.
As a further improvement of the preparation method of the single polyester reinforced foaming composite lightweight material, the invention has the following advantages:
Mode one: and (3) extruding and preparing the single-polyester reinforced foaming composite lightweight material:
Uniformly mixing 70-100 parts of polyester resin, 0-30 parts of polyester fiber, 0.1-2 parts of chain extender, 0.1-1.5 parts of antioxidant and 0.1-1.5 parts of nucleating agent, and then adding the mixture from a main feed inlet of an extruder; adding 0.5-5 parts (weight ratio) of supercritical fluid foaming agent into the extruder, and uniformly mixing; extruding and foaming through a mouth die, and forming and cooling to obtain a single-polyester composite foam board;
mode two: and (3) injection molding preparation of the single-polyester reinforced foaming composite lightweight material:
Uniformly mixing 70-100 parts of polyester resin, 0-30 parts of polyester fiber, 0.1-2 parts of chain extender, 0.1-1.5 parts of antioxidant and 0.1-1.5 parts of nucleating agent, and then adding the mixture from a main feed inlet of an injection molding machine; adding 0.5-5 parts (weight ratio) of supercritical fluid foaming agent into an injection molding machine, and uniformly mixing; injecting the melt mixture containing the foaming agent into a mold through an injection nozzle, and cooling and shaping to obtain a single-polyester composite foam board;
mode three: foaming the single polyester reinforced foaming composite lightweight material beads:
uniformly mixing 70-100 parts of polyester resin, 0-30 parts of polyester fiber, 0.1-2 parts of chain extender, 0.1-1.5 parts of antioxidant and 0.1-1.5 parts of nucleating agent, and then adding the mixture from a main feed inlet of an extruder; adding 0.5-5 parts (weight ratio) of supercritical fluid foaming agent into the extruder, and uniformly mixing; extruding through a mouth die, granulating by a rotary blade, filling bead foam into a die, and performing hot-press molding and cooling to obtain a single-polyester composite foam plate;
Mode four: and (3) mould pressing preparation of the single-polyester reinforced foaming composite lightweight material:
Uniformly mixing 70-100 parts of polyester resin, 0-10 parts of polyester fiber, 0.1-2 parts of chain extender, 0.1-1.5 parts of antioxidant and 0.1-1.5 parts of nucleating agent, and then adding the mixture from a main feed inlet of an injection molding machine; adding 0.5-5 parts (weight ratio) of supercritical fluid foaming agent into the extruder, and uniformly mixing with the melt; placing 0-30 parts of polyester fibers in a mold, injecting the mixed and plasticized melt containing the foaming agent into the mold, and cooling and shaping to obtain the single-polyester composite foam board;
Mode five:
Uniformly mixing 70-100 parts of polyester resin, 0-10 parts of polyester fiber, 0.1-2 parts of chain extender, 0.1-1.5 parts of antioxidant and 0.1-1.5 parts of nucleating agent, and then adding the mixture from a main feed inlet of an extruder; adding 0.5-5 parts (weight ratio) of supercritical fluid foaming agent into the extruder, and uniformly mixing; and drawing 1-30 parts of polyester fiber into the machine head to be in situ compounded with the foamed PET, and carrying out molding and cooling to obtain the single-polyester composite foam board.
In the first to third modes, the preferable polyester resin is 70 to 95 parts and the polyester fiber is 5 to 30 parts;
in the fourth to fifth modes, the polyester resin is preferably 70 to 95 parts and the total amount of the polyester fiber is preferably 5 to 30 parts.
The invention also provides the single polyester reinforced foaming composite lightweight material prepared by the method. The foaming multiplying power of the lightweight polyester-polyester composite material is 3-30 times, and the average diameter of the foam cells is 10-500 mu m.
In the invention, the following components are added:
Under the plasticization and viscosity reduction effects of supercritical carbon dioxide and entrainer thereof, hydroxyl or carboxyl at the end of a polyester molecular chain is reacted with a multifunctional chain extender to obtain long-chain branched polyester, and the dispersibility of fibers in molten resin is improved. On the other hand, the processing temperature can be properly reduced, the main chain degradation of the polyester resin is reduced, and the processing window for keeping the melting of the polyester resin and the existence of the polyester fiber is widened. And then directly extruding and foaming after branching reaction, and using the carbon dioxide and entrainer thereof as physical foaming agent, thereby realizing continuous, stable, energy-saving and efficient preparation of the reinforced foaming polyester material integrating reactive extrusion/injection foaming.
The invention relates to a single-polyester reinforced foaming composite lightweight material which consists of six parts, namely polyester resin, polyester fiber, chain extender, antioxidant, nucleating agent and foaming agent. Wherein the polyester resin is low-melting resin, and the polyester fiber is short fiber. And (3) mixing polyester resin, polyester fiber, a chain extender, an antioxidant and a nucleating agent according to a certain temperature and a certain proportion, and then mixing with a foaming agent according to a certain proportion to obtain the single-polyester reinforced foaming composite lightweight material.
The invention aims at solving the problems that the conventional polyester resin has the defects of poor melt strength, slow crystallization rate, easy degradation, difficult foam molding and the like due to the characteristics of linear molecular structure and low molecular weight in the polyester foaming process, and cannot be directly applied to the preparation of polyester foaming materials, and provides a single-polyester reinforced composite material. The invention is a single polymer composite material prepared by taking polyester materials with different forms as a matrix and a reinforcing phase, not only can strengthen the melt strength of the polyester material, but also can obtain an interface with good combination.
The invention combines two light weight technologies of fiber reinforcement and supercritical foaming, uses polyester fiber reinforcement polyester resin, and uses a supercritical fluid assisted continuous reaction extrusion foaming integrated process to prepare a light weight single polyester composite material. The method can solve the problems of high recovery difficulty, complex foaming process of the polyester material, low foaming multiplying power of the product, poor mechanical property and the like of the traditional composite material at present.
The single polyester reinforced foaming composite lightweight material and the preparation method thereof have the following technical advantages:
(1) The preparation process is simple, continuous and stable reaction modification can be realized, the reinforced foaming single polyester foam can be prepared integrally, and the production energy consumption is low;
(2) The single-polyester foam has higher foaming multiplying power and smaller pore diameter, and has better mechanical property;
(3) The green physical foaming agent is adopted for foaming, so that the environment friendliness is achieved;
(4) The used single polyester foam is easy to recycle and meets the requirement of green sustainable development.
Drawings
The following describes the embodiments of the present invention in further detail with reference to the accompanying drawings.
FIG. 1 is an SEM image of a polyester-composite foam sheet (29.7 times magnification) obtained in example 1;
FIG. 2 is an SEM image of a polyester-composite foam sheet (expansion ratio: 26.9) obtained in example 5;
FIG. 3 is an SEM image of a polyester composite foam sheet (expansion ratio: 18.1) obtained in example 6;
FIG. 4 is an SEM image of a polyester foam sheet (expansion ratio: 3.2) obtained in comparative example 2.
Detailed Description
The invention will be further described with reference to the following specific examples, but the scope of the invention is not limited thereto:
the PET resin and the polyester used in the invention are dried in a conventional manner (vacuum drying for 12 hours at 80 ℃).
The raw materials of the single-polyester reinforced foaming composite lightweight material consist of main materials, auxiliary materials and foaming agents; the main material consists of polyester resin and polyester fiber, and the auxiliary material consists of a chain extender, an antioxidant and a nucleating agent.
In the present invention,
Examples 1 to 8, twin screw extruders of comparative examples 1 to 2 were of the type d=20 mm in diameter; the length-diameter ratio L/D=48, the extruder 1-6 area is a melting reaction area, the 4 area is a CO 2 injection area, the 7-9 area is a cooling and extrusion area, and the material feeding amount is 1.0-2.0Kg/h;
Examples 9 to 12, the injection molding machine model of comparative example 3 was diameter d=25 mm; the length-diameter ratio L/D=30 is divided into 5 zones, the zones 1-5 of the extruder are melt reaction zones, the zone 3 is CO 2 injection zone, and the material feeding amount is 1.0-2.0Kg/h.
1. The preparation examples of the single polyester reinforced foaming composite lightweight material of the invention are as follows:
Example 1
90 Parts of dried PET resin (melting point 210 ℃), 10 parts of polyester fiber (melting point 260 ℃), 1.5 parts of triglycidyl isocyanurate (TGIC), 0.5 part of antioxidant 1010 and 0.5 part of nano silicon dioxide are mixed in a high-speed mixer for 5min. The mixed material was fed into a feeding hopper of a twin screw extruder at a feed rate of 1.0Kg/h, 5 parts of supercritical CO 2 (i.e., 5wt% of the main material of the foaming agent) was injected into the extruder by a metering pump, and 2% by mass of hexane was contained in the supercritical CO 2 as an entrainer. Controlling the rotation speed of a screw to 200rpm, controlling the temperature of a machine head to 220 ℃, extruding and foaming through a mouth die, and obtaining the single-polyester composite foam board with the thickness of 20mm after molding and cooling. The extruder was divided into 9 zones, i.e., zone i through zone ix, each of which had a working temperature and other process parameters as set forth in table 1 below.
The apparent density of the lightweight mono-polyester composite material was measured according to the ISO 845:2006 standard, and the foaming ratio Rv was calculated to be 29.7 times. The obtained composite material is quenched by liquid nitrogen, the section of the composite material is subjected to metal spraying, the section of the composite material is observed by a scanning electron microscope, and the average diameter of cells is counted to be 18 mu m. The tensile strength of the composite material was tested according to GB/T1040-2006, the compressive strength of the composite material was tested according to GB/T8813-2008, the flexural strength and flexural modulus of the composite material were tested according to GB/T9341-2000, and the notched impact strength of the composite material was tested according to GB/T1043-1993. The results of performance testing of the light-weight monoester composite are shown in table 3.
Example 2:
90 parts of dried PET resin (melting point 220 ℃), 10 parts of polyester fiber (melting point 260 ℃), 1.0 part of glycerol, 168.5 parts of antioxidant and 1.5 parts of talcum powder are mixed in a high-speed mixer for 5min. The mixed materials are added into a feeding hopper of a double-screw extruder, the feeding amount is 1Kg/h, 3 parts of supercritical CO 2 (namely, 3wt% of the foaming agent is the main material) is injected into the extruder through a metering pump, and 3 percent (mass%) of isopentane is contained in the supercritical CO 2 to serve as an entrainer. Controlling the rotating speed of the screw to 150rpm, controlling the temperature of the machine head to 215 ℃, extruding and foaming through a mouth die, and obtaining the single-polyester composite foam board with the thickness of 20mm after molding and cooling. The extruder was divided into 9 zones, i.e., zone i through zone ix, each of which had a working temperature and other process parameters as set forth in table 1 below.
Example 3:
80 parts of dried PET resin (melting point 220 ℃), 20 parts of polyester fiber (melting point 250 ℃), 0.5 part of pyromellitic anhydride (PMDA), 0.25 part of antioxidant 1010 and 0.5 part of titanium dioxide are mixed in a high-speed mixer for 5 minutes. The mixed materials are added into a feeding hopper of a double-screw extruder, the feeding amount is 2Kg/h, 3 parts of supercritical CO 2 (namely, 3wt% of the foaming agent is the main material) is injected into the extruder through a metering pump, and 2 percent (mass%) of cyclopentane is contained in the supercritical CO 2 to serve as an entrainer. Controlling the rotation speed of the screw to 100rpm, controlling the temperature of the machine head to 220 ℃, extruding and foaming through a mouth die, and obtaining the single-polyester composite foam board with the thickness of 20mm after molding and cooling. The extruder was divided into 9 zones, i.e., zone i through zone ix, each of which had a working temperature and other process parameters as set forth in table 1 below.
Example 4:
95 parts of dried PET resin (melting point 220 ℃), 5 parts of polyester fiber (melting point 260 ℃), 0.5 part of triethanolamine hydrochloride (TEAH), 1425.25 parts of antioxidant and 2 parts of nano calcium carbonate are mixed in a high-speed mixer for 5 minutes. The mixed material was fed into a feeding hopper of a twin screw extruder at a feed rate of 1.5Kg/h, and 2 parts of supercritical CO 2 (i.e., 2wt% of the main material of the foaming agent) containing 2% by mass of isopentane as an entrainer was injected into the extruder by a metering pump. Controlling the rotating speed of the screw to 150rpm, controlling the temperature of the machine head to 210 ℃, extruding and foaming through a mouth die, and obtaining the single-polyester composite foam board with the thickness of 20mm after molding and cooling. The extruder was divided into 9 zones, i.e., zone i through zone ix, each of which had a working temperature and other process parameters as set forth in table 1 below.
Example 5:
90 parts of dried PET resin (melting point 220 ℃), 10 parts of polyester fiber (melting point 260 ℃), 1.0 part of pyromellitic anhydride (PMDA), 0.5 part of antioxidant 1098 and 1.5 parts of talcum powder are mixed in a high-speed mixer for 5 minutes. The mixed material was fed into a feeding hopper of a twin screw extruder at a feed rate of 1.5Kg/h, 3 parts of supercritical CO 2 (i.e., 3wt% of the main material of the foaming agent) containing 3% of cyclopentane as an entrainer was injected into the extruder by a metering pump. The rotating speed of the screw is controlled to be 150rpm, the temperature of the machine head is 215 ℃, and the die opening speed is controlled to be 300rpm, so that the beaded mono-polyester composite foam is obtained. Then filling the bead foam into a mould, and obtaining the single polyester composite foam board with the thickness of 20mm after heating, forming and cooling. The extruder was divided into 9 zones, i.e., zone i through zone ix, each of which had a working temperature and other process parameters as set forth in table 1 below.
Example 6:
90 parts of dried PET resin (melting point 240 ℃), 5 parts of polyester fiber (melting point 265 ℃), 1.0 part of pyromellitic anhydride (PMDA), 0.5 part of antioxidant 168 and 1.5 parts of montmorillonite are mixed in a high-speed mixer for 5 minutes. The mixed materials are added into a feeding hopper of a double-screw extruder, the feeding amount is 1Kg/h, 2 parts of supercritical CO 2 (namely, 2wt% of the foaming agent is the main material) is injected into the extruder through a metering pump, and 2 percent (mass%) of isopentane is contained in the supercritical CO 2 to serve as an entrainer. Controlling the rotation speed of a screw to 150rpm, controlling the temperature of a machine head to 215 ℃, extruding and foaming through a mouth die, pulling 5 parts of polyester fibers (melting point 265 ℃) into the machine head to be in-situ compounded with the foamed PET, and obtaining the single-polyester composite foam board with the thickness of 20mm after molding and cooling. The extruder was divided into 9 zones, i.e., zone i through zone ix, each of which had a working temperature and other process parameters as set forth in table 1 below.
Example 7:
90 parts of dried PET resin (melting point 250 ℃), 1.0 part of pyromellitic anhydride (PMDA), 14250.5 parts of antioxidant and 1.5 parts of montmorillonite are mixed in a high-speed mixer for 5 minutes. The mixed material was fed into a feeding hopper of a twin screw extruder at a feed rate of 1Kg/h, and 4 parts of supercritical CO 2 (i.e., a blowing agent of 4wt% based on the main material) containing 2% by mass of isopentane as an entrainer was injected into the extruder by a metering pump. Controlling the rotation speed of a screw to 150rpm, controlling the temperature of a machine head to 220 ℃, extruding and foaming through a mouth die, drawing 10 parts of polyester fibers (with the melting point of 260 ℃) at the machine head, compounding with the foaming PET in situ, and obtaining the single-polyester composite foam board with the thickness of 20mm after molding and cooling. The extruder was divided into 9 zones, i.e., zone i through zone ix, each of which had a working temperature and other process parameters as set forth in table 1 below.
Example 8:
70 parts of dried PET resin (melting point 250 ℃), 1.0 part of pyromellitic anhydride (PMDA), 10100.5 parts of antioxidant and 1.5 parts of talcum powder are mixed in a high-speed mixer for 5 minutes. The mixed materials are added into a feeding hopper of a double-screw extruder, the feeding amount is 1Kg/h, 2 parts of supercritical CO 2 (namely, 2wt% of the foaming agent is the main material) is injected into the extruder through a metering pump, and 2 percent (mass%) of isopentane is contained in the supercritical CO 2 to serve as an entrainer. Controlling the rotation speed of a screw at 200rpm, controlling the temperature of a machine head at 220 ℃, extruding and foaming through a mouth die, drawing 30 parts of polyester fibers (melting point 265 ℃) at the machine head, compounding with the foaming PET in situ, and obtaining the single-polyester composite foam board with the thickness of 20mm after molding and cooling. The extruder was divided into 9 zones, i.e., zone i through zone ix, each of which had a working temperature and other process parameters as set forth in table 1 below.
Example 9:
85 parts of dried PET resin (melting point 220 ℃), 15 parts of polyester fiber (melting point 260 ℃), 0.5 part of triglycidyl isocyanurate (TGIC), 1425.25 parts of antioxidant and 2.0 parts of talcum powder are mixed in a high-speed mixer for 5min. The mixed material was fed into a rotary injection molding machine (screw diameter of the injection molding machine: 25mm, length-diameter ratio: 30), the feed amount was 1.0Kg/h, and 4 parts of supercritical CO 2 (i.e., blowing agent: 4wt% of main material) containing 2% by mass of isopentane as an entrainer was injected into the extruder by a metering pump. Controlling the back pressure of the injection molding machine to be 20MPa, controlling the temperature of a melt in the injection molding machine to be 230 ℃, dividing the injection molding machine into 5 sections, wherein the technological parameters of each section are shown in table 2, injecting a melt mixture containing a foaming agent into a mold through an injection nozzle, and cooling and shaping to obtain the single-polyester composite foam board with the thickness of 20 mm.
Example 10:
80 parts of dried PET resin (melting point 240 ℃), 20 parts of polyester fiber (melting point 260 ℃), 0.5 part of ethylenediamine, 1425.25 parts of antioxidant and 1.5 parts of nano silicon dioxide are mixed in a high-speed mixer for 5min. The mixed material was fed into a rotary injection molding machine (screw diameter of the injection molding machine: 25mm, aspect ratio: 30), the feed amount was 1.5Kg/h, and 3 parts of supercritical CO 2 (i.e., 3wt% of blowing agent as main material) containing 2% by mass of cyclopentane as an entrainer was injected into the extruder by a metering pump. Controlling the back pressure of the injection molding machine to be 18MPa, controlling the temperature of a melt in the injection molding machine to be 215 ℃, dividing the injection molding machine into 5 sections, wherein the technological parameters of each section are shown in table 2, injecting a melt mixture containing a foaming agent into a mold through an injection nozzle, and cooling and shaping to obtain the single-polyester composite foam board with the thickness of 20 mm.
Example 11:
90 parts of dried PET resin (melting point 250 ℃), 1.0 part of pyromellitic anhydride (PMDA), 10100.5 parts of antioxidant and 1.5 parts of talcum powder are mixed in a high-speed mixer for 5 minutes. The mixed material was fed into a rotating injection molding machine (screw diameter of the injection molding machine is 25mm, length-diameter ratio is 30), feeding amount is 2.0Kg/h, 4 parts of supercritical CO 2 (i.e. 4wt% of foaming agent as main material) is injected into the extruder by a metering pump, and the supercritical CO 2 contains no entrainer. Controlling the back pressure of the injection molding machine to 18MPa, controlling the temperature of a melt in the injection molding machine to 240 ℃, dividing the injection molding machine into 5 sections, wherein the technological parameters of each section are shown in table 2, placing 10 parts of polyester fibers (the single side content is 5 parts, and the melting point is 265 ℃), injecting the mixed and plasticized melt containing the foaming agent into the mold, and cooling and shaping to obtain the single-polyester composite foam board with the thickness of 20 mm.
Example 12:
90 parts of dried PET resin (melting point 260 ℃), 1.0 part of pyromellitic anhydride (PMDA), 10100.5 parts of antioxidant and 1.5 parts of talcum powder are mixed in a high-speed mixer for 5 minutes. The mixed materials are added into a feeding hopper of a double-screw extruder, the feeding amount is 1Kg/h, 2 parts of supercritical CO 2 (namely, 2wt% of the foaming agent is the main material) is injected into the extruder through a metering pump, and 2 percent (mass%) of isopentane is contained in the supercritical CO 2 to serve as an entrainer. Controlling the back pressure of the injection molding machine to be 18MPa, controlling the temperature of a melt in the injection molding machine to be 250 ℃, dividing the injection molding machine into 5 sections, wherein the technological parameters of each section are shown in table 2, placing 10 parts of polyester fibers in a mold (the fiber filaments at the two ends of the mold are fixed by silica gel, and the melting point is 260 ℃), injecting the mixed and plasticized melt containing the foaming agent into the mold, and cooling and shaping to obtain the single-polyester composite foam board with the thickness of 20 mm.
Comparative example 1:
100 parts of dried PET resin (melting point 220 ℃ C.), 0.5 part of triglycidyl isocyanurate (TGIC), 0.25 part of antioxidant 1010 and 1.5 parts of talcum powder are mixed in a high-speed mixer for 5min. The mixed material was fed into a feeding hopper of a twin screw extruder at a feed rate of 1.0Kg/h, and 2 parts of supercritical CO 2 (i.e., 2wt% of the main material of the foaming agent) containing 2% by mass of isopentane as an entrainer was injected into the extruder by a metering pump. Controlling the rotating speed of the screw to 150rpm, controlling the temperature of the machine head to 210 ℃, extruding and foaming through a mouth die, and obtaining the polyester foam board with the thickness of 20mm after molding and cooling. The extruder was divided into 9 zones, i.e., zone i through zone ix, each with the operating temperature and other process parameters as set forth in table 1.
Comparative example 2:
100 parts of dried PET resin (melting point 220 ℃ C.), 0.5 part of triglycidyl isocyanurate (TGIC), 0.25 part of antioxidant 1010 and 1.5 parts of talcum powder are mixed in a high-speed mixer for 5min. The mixed materials are added into a feeding hopper of a double-screw extruder, the feeding amount is 2.0Kg/h, 2 parts of supercritical CO 2 (namely, the foaming agent is 2wt% of the main material) is injected into the extruder through a metering pump, and the supercritical CO 2 does not contain entrainer. The rotational speed of the screw is controlled to be 150rpm, the temperature of the machine head is 210 ℃, and the die opening speed is 200rpm, so that the beaded mono-polyester composite foam is obtained. Then filling the bead foam into a mould, and obtaining the single polyester composite foam board with the thickness of 20mm after molding and cooling. The extruder was divided into 9 zones, i.e., zone i through zone ix, each with the operating temperature and other process parameters as set forth in table 1.
Comparative example 3:
100 parts of dried PET resin (melting point 220 ℃ C.), 0.5 part of triglycidyl isocyanurate (TGIC), 0.25 part of antioxidant 1010 and 2.0 parts of talcum powder are mixed in a high-speed mixer for 5min. The mixed material was fed into a rotary injection molding machine (screw diameter of the injection molding machine: 25mm, length-diameter ratio: 30), the feed amount was 1.5Kg/h, and 2 parts of supercritical CO 2 (i.e., blowing agent: 2wt% of main material) containing 4% by mass of isopentane as an entrainer was injected into the extruder by a metering pump. Controlling the back pressure of the injection molding machine to be 20MPa, controlling the temperature of the melt in the injection molding machine to be 210 ℃, enabling technological parameters of each section of the injection molding machine to be shown in table 2, injecting the melt mixture containing the foaming agent into a mold through an injection nozzle, and cooling and shaping to obtain the polyester foam board with the thickness of 20 mm.
Table 1, examples 1 to 8, and comparative examples 1 to 2, the extruder process parameters for each stage of sample preparation
Table 2, examples 9 to 12, and comparative example 3 sample preparation of injection molding machine section process parameters
And (II) testing the performance of the light-weight polyester composite material:
1. apparent density experiment:
The samples of examples 1 to 12 and comparative examples 1 to 3 were subjected to the following experiments. Apparent density ρ f(g/cm3) of the foamed sample is measured according to ASTM D792-00 standard using a drainage method, the calculation formula of the apparent density: Wherein m 1 (g) is the apparent mass of the foamed sample; m 2 (g) is the apparent mass of the foamed sample and the load after complete immersion in water; m 3 (g) is the mass of the load after complete immersion in water.
Foaming multiplying power of foaming sample is changed fromCalculated, where ρ 0(g/cm3) is the density of the sample before foaming.
The obtained composite material is quenched by liquid nitrogen, the section of the composite material is subjected to metal spraying, the section of the composite material is observed by a Scanning Electron Microscope (SEM), and an electron microscope photograph is analyzed by Nano Measurer software to obtain the cell diameter and the cell density. Average cell diameter of the foam sample was determined fromCalculated, where n is the number of cells in the statistical region of the SEM photograph and d is the diameter of a single cell. Cell density N (cm -3) is defined as the number of cells per unit volume of the foamed material, defined byCalculated, where A (cm 2) is the SEM photo area.
2. Mechanical property experiment:
the compressive strength of the samples obtained in examples 1 to 12 and comparative examples 1 to 3 above were tested according to GB/T8813-2008, the tensile strength of the composite material was tested according to GB/T1040-2006, the flexural strength and flexural modulus were tested according to GB/T9341-2000, and the notched impact strength was tested according to GB/T1043-1993.
The results obtained are as follows:
table 3, examples 1-8, and comparative examples 1-2 sample Performance comparisons
As can be seen from table 3: the products obtained in examples 1 to 8 had better properties than those obtained in comparative examples 1 and 2.
Table 4, examples 9-12 and comparative example 3 sample Performance comparison
From table 4, it can be seen that: the products obtained in examples 9 to 12 have better properties than comparative example 3.
From fig. 1 to 4, it can be seen that: the polyester fiber and the PET resin have better fusion, and the polyester material with the polyester fiber has more uniform cell structure than polyester fiber without or glass fiber, smaller pore diameter, high foaming multiplying power and high regularity.
Finally, it should also be noted that the above list is merely a few specific embodiments of the present invention. Obviously, the invention is not limited to the above embodiments, but many variations are possible. All modifications directly derived or suggested to one skilled in the art from the present disclosure should be considered as being within the scope of the present invention.
Claims (5)
1. A preparation method of a single polyester reinforced foaming composite lightweight material is characterized by comprising the following steps:
90 parts of dried PET resin with the melting point of 210 ℃,10 parts of polyester fiber with the melting point of 260 ℃,1.5 parts of triglycidyl isocyanurate, 0.5 part of antioxidant 1010 and 0.5 part of nano silicon dioxide are mixed in a high-speed mixer for 5min; adding the mixed materials into a feeding hopper of a double-screw extruder, wherein the feeding amount is 1.0 Kg/h, and injecting 5 parts of supercritical CO 2 into the extruder through a metering pump, wherein the supercritical CO 2 contains 2% of hexane as an entrainer; % is mass%, parts are parts by weight; controlling the rotation speed of a screw to 200rpm, controlling the temperature of a machine head to 220 ℃, extruding and foaming through a mouth die, and obtaining the single-polyester composite foam board with the thickness of 20 mm after molding and cooling; the extruder is divided into 9 areas, namely an I area to an IX area, and the working temperature of each area is respectively and sequentially as follows: 220 ℃, 240 ℃, 250 ℃, 240 ℃, 230 ℃, 220 ℃, 200 ℃.
2. A preparation method of a single polyester reinforced foaming composite lightweight material is characterized by comprising the following steps:
90 parts of dried PET resin with the melting point of 220 ℃,10 parts of polyester fiber with the melting point of 260 ℃, 1.0 part of pyromellitic anhydride, 0.5 part of antioxidant 1098 and 1.5 parts of talcum powder are mixed in a high-speed mixer for 5min; adding the mixed materials into a feeding hopper of a double-screw extruder, wherein the feeding amount is 1.5 Kg/h, and injecting 3 parts of supercritical CO 2 into the extruder through a metering pump, wherein the supercritical CO 2 contains 3% cyclopentane as an entrainer; % is mass%, parts are parts by weight; controlling the rotating speed of a screw to 150rpm, the temperature of a machine head to 215 ℃ and the speed of a die orifice to 300rpm to obtain beaded mono-polyester composite material foam; filling the bead foam into a mould, and heating, forming and cooling to obtain a single-polyester composite foam board with the thickness of 20 mm; the extruder is divided into 9 areas, namely an I area to an IX area, and the working temperature of each area is respectively and sequentially as follows: 240 ℃, 250 ℃, 255 ℃, 260 ℃, 240 ℃, 235 ℃, 230 ℃, 150 ℃.
3. A preparation method of a single polyester reinforced foaming composite lightweight material is characterized by comprising the following steps:
Mixing 90 parts of dried PET resin with the melting point of 250 ℃, 1.0 part of pyromellitic anhydride, 1420.5 part of antioxidant and 1.5 parts of montmorillonite in a high-speed mixer for 5min; adding the mixed materials into a feeding hopper of a double-screw extruder, wherein the feeding amount is 1 Kg/h, and injecting 4 parts of supercritical CO 2 into the extruder through a metering pump, wherein the supercritical CO 2 contains 2% isopentane as an entrainer; controlling the rotating speed of a screw to 150rpm, controlling the temperature of a machine head to 220 ℃, extruding and foaming through a mouth die, pulling 10 parts of polyester fiber with the melting point of 260 ℃ into the machine head to be in-situ compounded with the foamed PET, and obtaining the single-polyester composite foam board with the thickness of 20 mm after molding and cooling; % is mass%, parts are parts by weight; the extruder is divided into 9 areas, namely an I area to an IX area, and the working temperature of each area is respectively and sequentially as follows: 270 ℃, 275 ℃, 280 ℃, 260 ℃, 240 ℃, 230 ℃, 150 ℃.
4. A preparation method of a single polyester reinforced foaming composite lightweight material is characterized by comprising the following steps:
Mixing 90 parts of dried PET resin with the melting point of 250 ℃, 1.0 part of pyromellitic anhydride, 0.5 part of antioxidant 1010 and 1.5 parts of talcum powder in a high-speed mixer for 5min; adding the mixed materials into a rotary injection molding machine, wherein the diameter of a screw of the injection molding machine is 25mm, the length-diameter ratio is 30, the feeding amount is 2.0 Kg/h, 4 parts of supercritical CO 2 is injected into the extruder through a metering pump, and the supercritical CO 2 does not contain entrainer; controlling the back pressure of the injection molding machine to be 18MPa, wherein the temperature of a melt in the injection molding machine is 240 ℃, the injection molding machine is divided into 5 sections, and the temperatures of the first region temperature and the fifth region temperature are 240 ℃, 245 ℃, 250 ℃, 245 ℃ and 240 ℃ respectively in sequence; placing 5 parts of single-sided polyester fibers with a melting point of 265 ℃ in a mold, wherein the total of the polyester fibers is 10 parts; parts by weight; and (3) injecting the mixed and plasticized melt containing the foaming agent into a mould, and cooling and shaping to obtain the single-polyester composite foam board with the thickness of 20 mm.
5. The method for preparing the single-polyester reinforced foam composite lightweight material according to any one of claims 1 to 4, which is characterized by comprising the following steps: the drying was carried out under vacuum at a temperature of 80℃for 12 hours.
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| CN112679921A (en) * | 2021-03-18 | 2021-04-20 | 中广核高新核材科技（苏州）有限公司 | Ionomer composite nucleating agent for PET extrusion foaming and preparation method and application thereof |
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