CN106832824B - Method for preparing high-toughness high-strength PET/glass fiber composite material and product thereof - Google Patents
Method for preparing high-toughness high-strength PET/glass fiber composite material and product thereof Download PDFInfo
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- CN106832824B CN106832824B CN201710166064.2A CN201710166064A CN106832824B CN 106832824 B CN106832824 B CN 106832824B CN 201710166064 A CN201710166064 A CN 201710166064A CN 106832824 B CN106832824 B CN 106832824B
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- C08L67/00—Compositions of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Compositions of derivatives of such polymers
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Abstract
The invention discloses a method for preparing a high-toughness high-strength PET/glass fiber composite material and a product thereof, and aims to solve the defects that the conventional brake resistor valve body prepared from a metal material has large specific gravity of parts and high manufacturing cost, and the problem that the brake resistor valve body prepared from the conventional PET/glass fiber composite material cannot meet the mechanical performance requirement. The invention effectively solves the problems by improving the process, remarkably improves the molecular weight of the fiber-reinforced polyester composite material, further remarkably improves the mechanical properties such as tensile strength, impact strength and the like of the material, and successfully prepares the high-toughness high-strength PET/glass fiber composite material with outstanding mechanical properties and excellent dimensional stability. The composite material prepared by the invention has the advantages of outstanding mechanical property, excellent dimensional stability, high toughness and high strength, can be used for preparing high-performance structural parts such as brake booster valve bodies and the like, and has better application prospect.
Description
Technical Field
The invention relates to the field of materials, in particular to the field of material modification, and specifically relates to a method for preparing a high-toughness high-strength PET/glass fiber composite material and a product thereof. The invention provides a method for preparing a high-toughness high-strength PET/glass fiber composite material by solid-phase tackifying of a vacuum rotary drum and a product thereof.
Background
Polyethylene terephthalate (PET for short) is a special engineering plastic with low price, excellent wear resistance, heat resistance, chemical resistance, electrical insulation and high mechanical strength. It is known that the mechanical properties, such as tensile strength, of polyester can be greatly improved by adding fibers (such as glass fibers, carbon fibers, etc.) into the polyester. Meanwhile, the impact strength of the fiber-reinforced polyester composite material is further improved along with the increase of the molecular weight of the polyester. However, high molecular weight polyesters are not conducive to resin-to-fiber bonding.
At present, most brake resistor valve bodies are made of metal materials (such as aluminum, steel and the like). The parts made of metal materials have large specific gravity and high manufacturing cost. Compared with metal materials, the plastic composite material has the advantages of small specific gravity, convenient processing and low manufacturing cost. The bending strength of the ordinary PET/glass fibre composite material is then lower than 300MPa, which means that the maximum strength to which the valve body made of it (tubular with a thickness of 2mm and a diameter of 70.5mm, as shown in fig. 1 and 2 below) is subjected when it breaks is not within the safety range of the brake caliper valve body (greater than 12 KN). Meanwhile, the unnotched impact of a simple beam of the common PET/glass fiber composite material is lower than 50kJ/m2This means that the valve body (2 mm thick, 70.5mm diameter tube) made of it also has a toughness against falling ball impact that is not within a safe range (357g steel ball does not crack when hit on the valve body from a height of 27.5cm free fall).
Therefore, a new material is urgently needed to solve the above problems.
Disclosure of Invention
The invention aims to: aiming at the defects of large specific gravity of parts and high manufacturing cost of the brake resistor valve body prepared by the existing metal material and the problem that the brake resistor valve body prepared by the existing PET/glass fiber composite material cannot meet the mechanical performance requirement, the method for preparing the high-toughness high-strength PET/glass fiber composite material and the product thereof are provided. The invention effectively solves the problems by improving the process, remarkably improves the molecular weight of the fiber-reinforced polyester composite material, further remarkably improves the mechanical properties such as tensile strength, impact strength and the like of the material, and successfully prepares the high-toughness high-strength PET/glass fiber composite material with outstanding mechanical properties and excellent dimensional stability. The composite material prepared by the invention has the advantages of outstanding mechanical property, excellent dimensional stability, high toughness and high strength, can be used for preparing high-performance structural parts such as brake booster valve bodies and the like, and has better application prospect.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for preparing a high-toughness high-strength PET/glass fiber composite material is prepared from the following raw materials in parts by weight: 50-80 parts of PET resin, 20-50 parts of glass fiber, 0.01-5 parts of toughening agent, 0.1-1 part of nucleating agent and 0.01-0.5 part of antioxidant;
the specific gravity of the PET resin is 1.35-1.41g/cm3The intrinsic viscosity is 0.6-0.8 dl/g;
the method comprises the following steps:
(1) weighing the components according to the proportion, and uniformly mixing the PET resin, the toughening agent and the antioxidant by using a high-speed mixer to obtain a first material;
(2) putting the first material prepared in the step 1 into an extruder for melt extrusion granulation, and adding glass fibers in a side feeding manner to obtain a second material, wherein the extrusion temperature of the extruder is 250-300 ℃, and the rotating speed of the extruder is 350-480 RPM;
(3) and (3) placing the second material prepared in the step (2) into a vacuum rotary drum for solid-phase tackifying for 10-30 h, wherein the tackifying temperature is 160-245 ℃, and the air pressure in the vacuum rotary drum is 1 Pa-10 KPa.
The glass fiber is glass fiber which does not react with the PET resin.
The glass fiber surface has no active groups.
The active group is one or more of epoxy group and amino group.
The toughening agent is one or more of olefin copolymer elastomer containing active groups and methacrylic acid copolymer.
The toughening agent is an olefin copolymer elastomer containing epoxy groups.
The nucleating agent is one or more of inorganic nucleating agent and organic nucleating agent.
The nucleating agent is one or more of superfine talcum powder, superfine attapulgite, sodium montanate, calcium montanate, surlyn resin and metal carboxylate.
The antioxidant is used for polyester materials.
The antioxidant is one or more of tris [2, 4-di-tert-butylphenyl ] phosphite and tetrakis [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid ] pentaerythritol ester.
In the step 3, the tackifying temperature is 200-240 ℃, and the air pressure in the vacuum rotary drum is 1 Pa-1 KPa.
In the step 3, the tackifying temperature is 200-240 ℃, and the air pressure in the vacuum rotary drum is 1-500 Pa.
The product prepared by the method.
In order to solve the problems, the invention provides a method for preparing a high-toughness high-strength PET/glass fiber composite material and a product thereof. The method adopts the following raw materials in parts by weight: 50-80 parts of PET resin, 20-50 parts of glass fiber, 0.001-5 parts of toughening agent, 0.1-1 part of nucleating agent and 0.01-0.5 part of antioxidant. The method comprises the following specific steps: weighing the components according to the proportion, and uniformly mixing the PET resin, the toughening agent and the antioxidant by using a high-speed mixer to obtain a first material. And then, putting the prepared first material into an extruder for melt extrusion granulation, and adding glass fibers in a side feeding manner to obtain a second material. Wherein the extrusion temperature of the extruder is 250-300 ℃, and the rotating speed of the extruder is 350-480 RPM. Further, a twin-screw extruder may be used, and the length to diameter ratio is preferably 40: 1. Finally, placing the second into a vacuum rotary drum for solid-phase tackifying for 10-30 h; the tackifying temperature is preferably close to but necessarily lower than the melting point of PET, and can be 160-245 ℃, preferably set at 170-240 ℃, and most preferably set at 200-240 ℃; the pressure in the vacuum drum is 1Pa to 10KPa, preferably less than 1KPa, and more preferably less than 500 Pa.
The glass fiber is non-reactive with polyester, and no active groups such as epoxy groups or amino groups are on the surface of the glass fiber. The nucleating agent is well known, such as inorganic nucleating agents including ultrafine talc powder and ultrafine attapulgite, and organic nucleating agents including sodium montanate (Nav101), calcium montanate (Cav102), surly 8920, and metal carboxylate. The toughening agent is olefin copolymer elastomer with active groups (such as epoxy groups), methacrylic acid copolymer and the like. The antioxidant used is an antioxidant commonly used for polyester materials, such as a compound of tris [2, 4-di-tert-butylphenyl ] phosphite and pentaerythrityl tetrakis [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ].
Meanwhile, the invention claims the product prepared by the method.
According to the invention, through the improvement of the process, the molecular weight of the fiber-reinforced polyester composite material is remarkably improved, so that the mechanical properties such as tensile strength, impact strength and the like of the material are remarkably improved, and the high-toughness high-strength PET/glass fiber composite material with outstanding mechanical properties and excellent dimensional stability is successfully prepared.
Through determination, the bending strength of the high-toughness high-strength PET/glass fiber composite material is more than 300MPa, and the unnotched impact of a simply supported beam is more than 70kJ/m2The brake resistor valve body (the thickness is 2mm, the diameter is 70.5 mm) made of the steel ball can bear the pressure of more than 15KN, and the steel ball can completely bear 357g of steel balls and cannot crack when being hit on the valve body from a free falling body with the height of 27.5cm, so that the requirements of strength and toughness of the brake resistor valve body can be effectively met. The invention provides the high-toughness high-strength PET/glass fiber composite material with outstanding mechanical properties and excellent dimensional stability, which can be used for preparing high-performance structural parts such as brake booster valve bodies and the like, has better application prospect, and is worthy of large-scale popularization and application.
Drawings
The invention will now be described, by way of example, with reference to the accompanying drawings, in which:
FIG. 1 is a cross-sectional view of a brake caliper valve body.
FIG. 2 is a side view of a brake caliper valve body.
Detailed Description
All of the features disclosed in this specification, or all of the steps in any method or process so disclosed, may be combined in any combination, except combinations of features and/or steps that are mutually exclusive.
Any feature disclosed in this specification may be replaced by alternative features serving equivalent or similar purposes, unless expressly stated otherwise. That is, unless expressly stated otherwise, each feature is only an example of a generic series of equivalent or similar features.
Example 1
Weighing the following components in percentage by mass:
example 2
Weighing the following components in percentage by mass:
in the above-described embodiments 1 and 2:
the PET resin is homopolymerized PET with the intrinsic viscosity of 0.8 dl/g;
the chopped fiber without active groups is obtained by treating commercial chopped fiber at a high temperature of 400 ℃ for 1 hour and removing a surface active treating agent;
the chopped fiber containing active groups is glass fiber which is produced by Chongqing International composite Material Co.Ltd and has the trade name of ECS 303W, and the surface of the chopped fiber contains active epoxy groups;
the toughening agent is EMA LOTADER AX8900 resin produced by Arkema France, which is a random terpolymer of ethylene-methyl acrylate-glycidyl methacrylate and is prepared by a high-pressure free radical polymerization process;
the nucleating agent is sodium benzoate E221 produced by Univar Benelux company;
compound antioxidant: a 2:1 mixture of tris [ 2.4-di-tert-butylphenyl ] phosphite and tetrakis [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propanoic acid ] pentaerythritol ester.
In the above examples 1 and 2, after weighing the components, the weighed components are respectively subjected to blending granulation by a twin-screw extruder with a length-diameter ratio of 40: 1: the extrusion temperature is set to be 250-300 ℃, and the rotating speed is 400 RPM.
Example 3
The granules obtained in example 1 were placed in a vacuum drum and solid-tackified for 20 hours. Wherein the solid phase tackifying temperature is 220 ℃, and the air pressure in the vacuum rotary drum is 480 Pa.
Example 4
The granules obtained in example 2 were placed in a vacuum drum and solid-tackified for 20 hours. Wherein the solid phase tackifying temperature is 220 ℃, and the air pressure in the vacuum rotary drum is 480 Pa.
Drying the products obtained in the embodiments 1-4 in a dehumidifying dryer at 120 ℃ for 4h, then injection molding to obtain standard sample strips, adjusting the state of the standard sample strips according to GB/T2918, testing tensile strength according to GB/T1040, testing bending strength and bending modulus according to GB/T9341, testing unnotched impact strength of a simply supported beam according to GB/T1043, testing intrinsic viscosity value of a composite material according to GB/T14190, and testing molecular weight and molecular weight distribution by gel chromatography. The test results are shown in table 1 below.
TABLE 1 comparison of Properties
As can be seen from the comparison of the 4 examples, the tensile strength and the unnotched impact strength of the simply supported beam of the PET/glass fiber composite material can be greatly improved by adopting the invention. It should be noted that the active groups on the surface of the glass fiber can affect the mechanical properties of the production process, especially the improvement of the unnotched impact strength of the simply supported beam. The active groups on the surface of the glass fiber react with ester groups in polyethylene terephthalate (PET), so that the molecular weight is increased and the molecular weight distribution is wider in the solid-phase tackifying of the vacuum rotary drum, and the wider molecular weight distribution reduces the improvement range of the unnotched impact strength of the simply supported beam.
Example 5
Weighing the following components in percentage by mass:
the preparation steps are as follows:
(1) weighing the components according to the proportion, and uniformly mixing the PET resin, the toughening agent and the antioxidant by using a high-speed mixer to obtain a first material;
(2) putting the first material prepared in the step 1 into an extruder for melt extrusion granulation, and adding glass fibers in a side feeding manner to obtain a second material, wherein the extrusion temperature of the extruder is 260-280 ℃, and the rotating speed of the extruder is 440 RPM;
(3) and (3) placing the second material prepared in the step (2) in a vacuum rotary drum for solid phase tackifying for 15h, wherein the tackifying temperature is 230 ℃, and the air pressure in the vacuum rotary drum is 300 Pa.
The tensile strength of the product prepared in the example is measured to be 201 MPa; the bending strength is 298 MPa; the flexural modulus is 11011 MPa; the unnotched impact strength of the simply supported beam is 77KJ/m2(ii) a The maximum pressure when the valve body is broken is 13.2 KN; 357g of steel ball breaks on the valve body from a free falling body with the height of 27.5 cm: no cracking; intrinsic viscosity: 1.13; Mw/Mn: 2.5.
example 6
Weighing the following components in percentage by mass:
in the present embodiment, the first and second electrodes are,
the preparation steps are as follows: the PET resin, the chopped fiber without active groups, the toughening agent, the nucleating agent and the antioxidant are the same as those in the example 1.
(1) Weighing the components according to the proportion, and uniformly mixing the PET resin, the toughening agent and the antioxidant by using a high-speed mixer to obtain a first material;
(2) putting the first material prepared in the step 1 into an extruder for melt extrusion granulation, and adding glass fibers in a side feeding manner to obtain a second material, wherein the extrusion temperature of the extruder is 270-290 ℃, and the rotating speed of the extruder is 430 RPM;
(3) and (3) placing the second material prepared in the step (2) in a vacuum rotary drum for solid phase tackifying for 25h, wherein the tackifying temperature is 200 ℃, and the air pressure in the vacuum rotary drum is 1 kPa.
The tensile strength of the product prepared in the example is determined to be 203 MPa; the bending strength is 296 MPa; the flexural modulus is 110107 MPa; the unnotched impact strength of the simply supported beam is 79KJ/m2(ii) a The maximum pressure when the valve body is broken is 13.3 KN; 357g of steel ball breaks on the valve body from a free falling body with the height of 27.5 cm: no cracking; intrinsic viscosity: 1.14; Mw/Mn: 2.6.
the above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
All features disclosed in this specification may be combined in any combination, except features that are mutually exclusive.
Any feature disclosed in this specification (including any accompanying claims, abstract and drawings), may be replaced by alternative features serving equivalent or similar purposes, unless expressly stated otherwise. That is, unless expressly stated otherwise, each feature is only an example of a generic series of equivalent or similar features.
Claims (7)
1. The method for preparing the high-toughness high-strength PET/glass fiber composite material is characterized by comprising the following raw materials in parts by weight: 50-80 parts of PET resin, 20-50 parts of glass fiber, 0.001-5 parts of toughening agent, 0.1-1 part of nucleating agent and 0.01-0.5 part of antioxidant;
the specific gravity of the PET resin is 1.35-1.41g/cm3The intrinsic viscosity is 0.6-0.8 dl/g;
the method comprises the following steps:
(1) weighing the components according to the proportion, and uniformly mixing the PET resin, the toughening agent and the antioxidant by using a high-speed mixer to obtain a first material;
(2) putting the first material prepared in the step (1) into an extruder for melt extrusion granulation, and adding glass fibers in a side feeding manner to obtain a second material, wherein the extrusion temperature of the extruder is 250-300 ℃, and the rotating speed of the extruder is 350-480 RPM;
(3) placing the second material prepared in the step (2) into a vacuum rotary drum for solid-phase tackifying for 10-30 h, wherein the tackifying temperature is 160-245 ℃, and the air pressure in the vacuum rotary drum is 1 Pa-10 KPa;
the glass fiber is glass fiber which does not react with the PET resin;
the surface of the glass fiber has no active groups;
the toughening agent is one or more of olefin copolymer elastomer containing active groups and methacrylic acid copolymer.
2. The method for preparing the high-toughness high-strength PET/glass fiber composite material according to claim 1, wherein the toughening agent is an olefin copolymer elastomer containing epoxy groups.
3. The method for preparing the high-toughness high-strength PET/glass fiber composite material according to claim 1, wherein the nucleating agent is one or more of an inorganic nucleating agent and an organic nucleating agent.
4. The method for preparing the high-toughness high-strength PET/glass fiber composite material according to claim 1, wherein the antioxidant is an antioxidant for polyester materials.
5. The method for preparing the high-toughness high-strength PET/glass fiber composite material according to any one of claims 1 to 4, wherein in the step (3), the tackifying temperature is 200-240 ℃, and the air pressure in a vacuum rotary drum is 1 Pa-1 KPa.
6. The method for preparing the high-toughness high-strength PET/glass fiber composite material according to claim 5, wherein in the step (3), the tackifying temperature is 200-240 ℃, and the air pressure in a vacuum rotary drum is 1-500 Pa.
7. A product prepared by the method of any one of claims 1 to 6.
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Citations (3)
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| CN101787184A (en) * | 2009-12-30 | 2010-07-28 | 中国石油化工股份有限公司 | Quickly crystallized polyester engineering plastic and preparation method thereof |
| CN102807743A (en) * | 2012-07-27 | 2012-12-05 | 广东联塑科技实业有限公司 | Foamed PET (polyethylene glycol terephthalate) plate slice, and preparation method thereof |
| CN103232685A (en) * | 2013-04-27 | 2013-08-07 | 上海锦湖日丽塑料有限公司 | Low-mold-deposit high-surface-quality high-content glass fiber reinforced material and preparation method thereof |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101787184A (en) * | 2009-12-30 | 2010-07-28 | 中国石油化工股份有限公司 | Quickly crystallized polyester engineering plastic and preparation method thereof |
| CN102807743A (en) * | 2012-07-27 | 2012-12-05 | 广东联塑科技实业有限公司 | Foamed PET (polyethylene glycol terephthalate) plate slice, and preparation method thereof |
| CN103232685A (en) * | 2013-04-27 | 2013-08-07 | 上海锦湖日丽塑料有限公司 | Low-mold-deposit high-surface-quality high-content glass fiber reinforced material and preparation method thereof |
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| Title |
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| "PET增粘技术的发展和应用";朱小莺;《燕山油化》;19920401(第1期);第53-57页 * |
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