CN114716792A - Low-odor PET composite material with good physical properties and preparation method thereof - Google Patents

Low-odor PET composite material with good physical properties and preparation method thereof Download PDF

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CN114716792A
CN114716792A CN202110012844.8A CN202110012844A CN114716792A CN 114716792 A CN114716792 A CN 114716792A CN 202110012844 A CN202110012844 A CN 202110012844A CN 114716792 A CN114716792 A CN 114716792A
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pet
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CN114716792B (en
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杨桂生
何璟
姚晨光
邹冲
李术
杨莺
李枭
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Hefei Genius New Materials Co Ltd
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Hefei Genius New Materials Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L67/00—Compositions of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Compositions of derivatives of such polymers
    • C08L67/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
    • C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
    • C08F220/10—Esters
    • C08F220/26—Esters containing oxygen in addition to the carboxy oxygen
    • C08F220/32—Esters containing oxygen in addition to the carboxy oxygen containing epoxy radicals
    • C08F220/325—Esters containing oxygen in addition to the carboxy oxygen containing epoxy radicals containing glycidyl radical, e.g. glycidyl (meth)acrylate
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F8/00—Chemical modification by after-treatment
    • C08F8/42—Introducing metal atoms or metal-containing groups
    • 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
    • C08J3/005—Processes for mixing polymers
    • 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
    • C08J2367/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
    • C08J2367/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
    • 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
    • C08J2433/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
    • C08J2433/04—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers esters
    • C08J2433/14—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers esters of esters containing halogen, nitrogen, sulfur, or oxygen atoms in addition to the carboxy oxygen
    • 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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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Silicon Polymers (AREA)

Abstract

The invention discloses a low-odor polyethylene terephthalate (PET) composite material with good physical properties, which is prepared from the following components in parts by weight: 80-100 parts of PET, 8-12 parts of modifier poly glycidyl methacrylate-styrene-dimethyl siloxane and 0.1-0.5 part of antioxidant. The invention also discloses a preparation method of the PET composite material. The modifier P (GMA-St-DMS) in the PET composite material prepared by the invention can well improve the physical property of the PET material; supercritical carbon dioxide is introduced into the PET composite material, and volatile micromolecules in fluid are adsorbed through the powerful permeation and dissolution capacity of the supercritical carbon dioxide, so that the odor of the PET composite material is improved. The PET composite material prepared by the invention has excellent application prospect in the field of automobile materials.

Description

Low-odor PET composite material with good physical properties and preparation method thereof
Technical Field
The invention belongs to the field of high polymer materials, and particularly relates to a low-odor PET composite material with good physical properties and a preparation method thereof.
Background
Polyethylene terephthalate (PET) is a widely used high molecular polyester resin, and PET has the advantages of good fatigue resistance, good heat resistance, excellent dimensional stability and the like, but in some specific automobile material fields, the requirements on the odor property and the physical property of PET are high, and the common PET material cannot meet the requirements, so that the application of the PET composite material in some automobile material fields is limited.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a PET composite material with low odor and good physical properties and a preparation method thereof.
The purpose of the invention is realized by the following technical scheme:
a low-odor PET composite material with good physical properties is prepared from the following components in parts by weight:
80 to 100 portions of PET, and the mixture,
8 to 12 portions of modifier of poly glycidyl methacrylate-styrene-dimethyl siloxane,
0.1 to 0.5 portion of antioxidant.
As a preferable technical scheme, the modifier of poly glycidyl methacrylate-styrene-dimethyl siloxane is abbreviated as modifier P (GMA-St-DMS), and the preparation steps are as follows:
(1) adding emulsifier sodium dodecyl benzene sulfonate, initiator sodium persulfate, glycidyl methacrylate, styrene, cross-linking agent ethylene glycol dimethacrylate and deionized water into a reaction vessel, and stirring and reacting at 60-80 ℃ for 10-16h to obtain solution A; further preferably, the mass ratio of the emulsifier sodium dodecyl benzene sulfonate, the initiator sodium persulfate, the glycidyl methacrylate, the styrene, the cross-linking agent ethylene glycol dimethacrylate and the deionized water is (0.2-0.4): (0.1-0.3): (30-40): (20-30): (0.1-0.3): (160-200).
(2) Weighing the solution A, initiator sodium persulfate and dimethyldichlorosilane, adding the solution A, initiator sodium persulfate and dimethyldichlorosilane into a reaction vessel, and stirring at 70-90 ℃ for reaction for 8-12 hours to obtain solution B, wherein the solution A, the initiator sodium persulfate and the dimethyldichlorosilane are preferably mixed according to a mass ratio of (60-80): (0.1-0.3): (10-16).
(3) Weighing the solution B and a magnesium sulfate solution, adding the solution B and the magnesium sulfate solution into a reaction vessel, and stirring and reacting for 6-8h at 50-70 ℃ to obtain a solution C; more preferably, the mass ratio of the solution B to the magnesium sulfate solution is (70-90): (20-30).
(4) And carrying out suction filtration, washing and drying on the solution C to obtain a modifier P (GMA-St-DMS).
Preferably, the antioxidant is at least one of antioxidant 168, antioxidant 1010 and antioxidant 1330.
The invention also aims to provide a preparation method of the PET composite material, which comprises the following steps:
(1) weighing PET, a modifier P (GMA-St-DMS) and an antioxidant according to a certain proportion, putting the PET, the modifier P and the antioxidant into an autoclave in a supercritical carbon dioxide environment, and uniformly mixing to obtain a mixture;
(2) and (2) adding the mixture obtained in the step (1) into a double-screw extruder for extrusion granulation to obtain the PET composite material.
Preferably, the temperature of the autoclave is 30-40 ℃ and the pressure is 6-8 MPa.
Further preferably, the twin-screw extruder comprises six temperature zones arranged in sequence, and the temperature of each zone is respectively as follows: the temperature of the first zone is 240-260 ℃, the temperature of the second zone is 280-300 ℃, the temperature of the third zone is 280-300 ℃, the temperature of the fourth zone is 280-300 ℃, the temperature of the fifth zone is 280-300 ℃, the temperature of the sixth zone is 280-300 ℃, the temperature of the machine head is 280-300 ℃, and the rotating speed of the screw is 200-280 r/min.
Compared with the prior art, the invention has the beneficial effects that:
(1) the invention prepares a novel modifier P (GMA-St-DMS), which can well improve the physical properties of PET materials, and has important significance.
(2) The invention introduces supercritical carbon dioxide, and has important significance in adsorbing volatile micromolecules in PET and improving the odor of the PET composite material through strong penetrating and dissolving capacities.
Detailed Description
The present invention will be further described with reference to the following examples. It is to be understood that the embodiments described are only a few embodiments of the present invention, and not all embodiments. All other embodiments, which can be obtained by a person skilled in the art without inventive step based on the embodiments of the present invention, are within the scope of protection of the present invention.
The types and suppliers of reagents used in the following examples and comparative examples are merely illustrative of the sources and components of reagents used in the experiments of the present invention and are fully disclosed, and do not indicate that the present invention cannot be practiced using other reagents of the same type or other suppliers.
The raw materials used in the following examples are as follows:
PET (model 008L), Aclo, canada; sodium dodecyl benzene sulfonate, chemical ltd, denamantan; sodium persulfate, guangzhou puss chemical ltd; styrene, denming chemical limited, denna; glycidyl methacrylate, Nanjing Rongan chemical technology, Inc.; ethylene glycol dimethacrylate, Shandong Yukang chemical Co., Ltd; dimethyldichlorosilane, north huichi permanent broad science and technology ltd; deionized water, Shanghai Jing pure Water treatment technologies, Inc.; antioxidant 168, antioxidant 1010, antioxidant 1330, basf corporation.
Preparation example 1
(1) Weighing 2g of emulsifier sodium dodecyl benzene sulfonate, 1g of initiator sodium persulfate, 300g of glycidyl methacrylate, 200g of styrene, 1g of cross-linking agent ethylene glycol dimethacrylate and 1.6kg of deionized water, adding into a reaction vessel, and stirring and reacting for 10 hours at the temperature of 60 ℃ to obtain a solution A.
(2) 600g of the solution A, 1g of initiator sodium persulfate and 100g of dimethyldichlorosilane are weighed and added into a reaction vessel, and stirred and reacted for 8 hours at 70 ℃ to obtain a solution B.
(3) Weighing 700g of the solution B and 200g of the magnesium sulfate solution, adding the solution B and the magnesium sulfate solution into a reaction vessel, and stirring and reacting for 6 hours at 50 ℃ to obtain a solution C.
(4) And carrying out suction filtration, washing and drying on the solution C to obtain a modifier P (GMA-St-DMS) X1.
Example 1
(1) Weighing 80 parts of PET, 8 parts of modifier P (GMA-St-DMS) X1 and 0.1 part of Irganox1010, and uniformly mixing in an autoclave in a supercritical carbon dioxide environment to obtain a mixture;
(2) and (3) extruding and granulating the mixture obtained in the step (1) from an extruder to obtain the PET composite material P1.
Wherein the temperature of the high-pressure kettle is 30 ℃, the pressure intensity is 6MPa, and the temperature and the screw rotating speed of each area of the double-screw extruder are respectively as follows: the temperature of the first zone is 240 ℃, the temperature of the second zone is 280 ℃, the temperature of the third zone is 280 ℃, the temperature of the fourth zone is 280 ℃, the temperature of the fifth zone is 280 ℃, the temperature of the sixth zone is 280 ℃, the temperature of a machine head is 280 ℃ and the rotating speed of a screw is 200 r/min.
Preparation example 2
(1) Weighing 4g of emulsifier sodium dodecyl benzene sulfonate, 3g of initiator sodium persulfate, 400g of glycidyl methacrylate, 300g of styrene, 3g of cross-linking agent ethylene glycol dimethacrylate and 2.0kg of deionized water, adding into a reaction vessel, and stirring and reacting for 16h at 80 ℃ to obtain a solution A.
(2) 800g of the solution A, 3g of initiator sodium persulfate and 160g of dimethyldichlorosilane are weighed and added into a reaction vessel, and the mixture is stirred and reacted for 12 hours at 90 ℃ to obtain a solution B.
(3) And weighing 900g of the solution B and 300g of the magnesium sulfate solution, adding the solution B and the magnesium sulfate solution into a reaction vessel, and stirring and reacting for 8 hours at 70 ℃ to obtain a solution C.
(4) And carrying out suction filtration, washing and drying on the solution C to obtain a modifier P (GMA-St-DMS) X2.
Example 2
(1) Weighing 100 parts of PET, 12 parts of modifier P (GMA-St-DMS) X2, 0.1 part of Irganox1010, 0.2 part of Irganox168 and 0.2 part of Irganox1330, and uniformly mixing in an autoclave in a supercritical carbon dioxide environment to obtain a mixture;
(2) and (3) extruding and granulating the mixture obtained in the step (1) from an extruder to obtain the PET composite material P2.
Wherein the temperature of the high-pressure kettle is 40 ℃, the pressure intensity is 8MPa, and the temperature and the screw rotating speed of each area of the double-screw extruder are respectively as follows: the temperature of the first zone is 260 ℃, the temperature of the second zone is 300 ℃, the temperature of the third zone is 300 ℃, the temperature of the fourth zone is 300 ℃, the temperature of the fifth zone is 300 ℃, the temperature of the sixth zone is 300 ℃, the temperature of the machine head is 300 ℃ and the screw rotation speed is 280 r/min.
Preparation example 3
(1) 3g of emulsifier sodium dodecyl benzene sulfonate, 2g of initiator sodium persulfate, 350g of glycidyl methacrylate, 250g of styrene, 2g of cross-linking agent ethylene glycol dimethacrylate and 1.8kg of deionized water are weighed and added into a reaction vessel, and stirred and reacted for 13 hours at the temperature of 70 ℃ to obtain a solution A.
(2) Weighing 700g of the solution A, 2g of initiator sodium persulfate and 130g of dimethyldichlorosilane, adding into a reaction vessel, and stirring and reacting at 80 ℃ for 10 hours to obtain a solution B.
(3) Weighing 800g of the solution B and 250g of the magnesium sulfate solution, adding the solution B and the magnesium sulfate solution into a reaction vessel, and stirring and reacting for 7 hours at 60 ℃ to obtain a solution C.
(4) And carrying out suction filtration, washing and drying on the solution C to obtain a modifier P (GMA-St-DMS) X3.
Example 3
(1) Weighing 90 parts of PET, 10 parts of modifier P (GMA-St-DMS) X3, 0.1 part of Irganox168 and 0.2 part of Irganox1010, and uniformly mixing in an autoclave in a supercritical carbon dioxide environment to obtain a mixture;
(2) and (2) extruding and granulating the mixture obtained in the step (1) from an extruder to obtain the PET composite material P3.
Wherein the temperature of the high-pressure kettle is 35 ℃, the pressure intensity is 7MPa, and the temperature and the screw rotating speed of each area of the double-screw extruder are respectively as follows: the temperature of the first zone is 250 ℃, the temperature of the second zone is 290 ℃, the temperature of the third zone is 290 ℃, the temperature of the fourth zone is 290 ℃, the temperature of the fifth zone is 290 ℃, the temperature of the sixth zone is 290 ℃, the temperature of the machine head is 290 ℃ and the rotating speed of the screw is 240 r/min.
Preparation example 4
(1) Weighing 2g of emulsifier sodium dodecyl benzene sulfonate, 3g of initiator sodium persulfate, 380g of glycidyl methacrylate, 220g of styrene, 1g of cross-linking agent ethylene glycol dimethacrylate and 1.9kg of deionized water, adding into a reaction vessel, and stirring and reacting for 11 hours at 65 ℃ to obtain a solution A.
(2) 710g of the solution A, 3g of initiator sodium persulfate and 120g of dimethyldichlorosilane are weighed and added into a reaction vessel, and the mixture is stirred and reacted for 11 hours at the temperature of 75 ℃ to obtain a solution B.
(3) 780g of the solution B and 210g of the magnesium sulfate solution are weighed and added into a reaction vessel, and the mixture is stirred and reacted for 7 hours at the temperature of 55 ℃ to obtain a solution C.
(4) And carrying out suction filtration, washing and drying on the solution C to obtain a modifier P (GMA-St-DMS) X4.
Example 4
(1) Weighing 85 parts of PET, 9 parts of modifier P (GMA-St-DMS) X4, 16 parts of supercritical carbon dioxide, 0.1 part of Irganox1010 and 0.2 part of Irganox1330, and uniformly mixing in an autoclave in a supercritical carbon dioxide environment to obtain a mixture;
(2) and (2) extruding and granulating the mixture obtained in the step (1) from an extruder to obtain the PET composite material P4.
Wherein the temperature of the high-pressure kettle is 40 ℃, the pressure intensity is 6MPa, and the temperature and the screw rotating speed of each area of the double-screw extruder are respectively as follows: the temperature of the first zone is 245 ℃, the temperature of the second zone is 285 ℃, the temperature of the third zone is 285 ℃, the temperature of the fourth zone is 285 ℃, the temperature of the fifth zone is 285 ℃, the temperature of the sixth zone is 285 ℃, the temperature of a machine head is 285 ℃, and the rotating speed of a screw is 255 r/min.
Preparation example 5
(1) 3g of emulsifier sodium dodecyl benzene sulfonate, 3g of initiator sodium persulfate, 380g of glycidyl methacrylate, 210g of styrene, 1g of cross-linking agent ethylene glycol dimethacrylate and 1.9kg of deionized water are weighed and added into a reaction vessel, and the mixture is stirred and reacted for 14 hours at the temperature of 65 ℃ to obtain a solution A.
(2) 690g of the solution A, 2g of initiator sodium persulfate and 140g of dimethyldichlorosilane are weighed and added into a reaction vessel, and the mixture is stirred and reacted for 11 hours at the temperature of 75 ℃ to obtain a solution B.
(3) 780g of the solution B and 240g of the magnesium sulfate solution are weighed and added into a reaction vessel, and the mixture is stirred and reacted for 8 hours at 55 ℃ to obtain a solution C.
(4) And carrying out suction filtration, washing and drying on the solution C to obtain a modifier P (GMA-St-DMS) X5.
Example 5
(1) Weighing 95 parts of PET, 11 parts of modifier P (GMA-St-DMS) X5, 0.1 part of Irganox1010 and 0.1 part of Irganox168, and uniformly mixing in an autoclave in a supercritical carbon dioxide environment to obtain a mixture;
(2) and (3) extruding and granulating the mixture obtained in the step (1) from an extruder to obtain the PET composite material P5.
Wherein the temperature of the high-pressure kettle is 35 ℃, the pressure intensity is 7MPa, and the temperature and the screw rotating speed of each area of the double-screw extruder are respectively as follows: the temperature of the first zone is 250 ℃, the temperature of the second zone is 295 ℃, the temperature of the third zone is 295 ℃, the temperature of the fourth zone is 295 ℃, the temperature of the fifth zone is 295 ℃, the temperature of the sixth zone is 295 ℃, the temperature of the machine head is 295 ℃ and the rotating speed of the screw is 270 r/min.
Comparative example 1
(1) Weighing 100 parts of PET, 0.1 part of Irganox1010 and 0.2 part of Irganox168, mixing and uniformly stirring to obtain a mixture;
(2) and (3) extruding and granulating the mixture obtained in the step (1) from an extruder to obtain the PET composite material D1.
Wherein the temperature and the screw rotating speed of each area of the double-screw extruder are respectively as follows: the temperature of the first zone is 250 ℃, the temperature of the second zone is 295 ℃, the temperature of the third zone is 295 ℃, the temperature of the fourth zone is 295 ℃, the temperature of the fifth zone is 295 ℃, the temperature of the sixth zone is 295 ℃, the temperature of a machine head is 295 ℃, and the rotating speed of a screw is 270 r/min.
Comparative example 2
(1) Weighing 80 parts of PET and 0.1 part of Irganox1010, putting into an autoclave in a supercritical carbon dioxide environment, and uniformly mixing to obtain a mixture;
(2) and (3) extruding and granulating the mixture obtained in the step (1) from an extruder to obtain the PET composite material D2.
Wherein the temperature of the high-pressure kettle is 30 ℃, the pressure intensity is 6MPa, and the temperature and the screw rotating speed of each area of the double-screw extruder are respectively as follows: the temperature of the first zone is 240 ℃, the temperature of the second zone is 280 ℃, the temperature of the third zone is 280 ℃, the temperature of the fourth zone is 280 ℃, the temperature of the fifth zone is 280 ℃, the temperature of the sixth zone is 280 ℃, the temperature of a machine head is 280 ℃ and the rotating speed of a screw is 200 r/min.
Comparative example 3
(1) Weighing 80 parts of PET, 8 parts of modifier P (GMA-St-DMS) X1 and 0.1 part of Irganox1010, and uniformly mixing to obtain a mixture;
(2) and (3) extruding and granulating the mixture obtained in the step (1) from an extruder to obtain the PET composite material D3.
Wherein the temperature of the high-pressure kettle is 30 ℃, the pressure intensity is 6MPa, and the temperature and the screw rotating speed of each area of the double-screw extruder are respectively as follows: the temperature of the first zone is 240 ℃, the temperature of the second zone is 280 ℃, the temperature of the third zone is 280 ℃, the temperature of the fourth zone is 280 ℃, the temperature of the fifth zone is 280 ℃, the temperature of the sixth zone is 280 ℃, the temperature of a machine head is 280 ℃ and the rotating speed of a screw is 200 r/min.
The PET composite materials prepared in the above examples 1-5 and comparative examples 1-3 are made into sample bars by an injection molding machine for relevant performance detection, and the test data are as follows in the following table 1:
TABLE 1 Performance test results
Figure BDA0002885632830000071
Note: in table 1, the spline types and the relevant conditions used for the correlation test are as follows:
the tensile sample bar model is (170.0 + -5.0) mm (13.0 + -0.5) mm (3.2 + -0.2) mm, and the tensile rate is 50 mm/min; the cantilever beam notch impact strength sample bars used are of the type: (125.0 +/-5.0) mm (13.0 +/-0.5) mm (3.2 +/-0.2) mm, machining the notch, and cutting to obtain notch depth (2.6 +/-0.2) mm. The odor detection standard employs VDA270, which is divided into 6 grades: 1 is odorless; 2-slightly odorous; 3-tasted but not irritating; 4, pungent smell; 5 ═ strong pungent odor; 6-intolerable taste, the test procedure was to take 30g of the sample into a 1L container, seal it with the lid, and place it in a high temperature oven at 40 ℃ for 24 h.
As can be seen from Table 1 above, examples 1-5 are superior to comparative example 1 in both physical properties and odor properties, examples 1-5 are superior to comparative example 2 in physical properties, and examples 1-5 are superior to comparative example 3 in odor properties. This shows that the PET composite material of the patent has excellent physical properties and good odor. The application field of the PET composite material is greatly expanded, and the method has very important significance.
The invention is not limited to the embodiments described, and those skilled in the art can make various equivalent modifications or substitutions without departing from the spirit of the invention, and these equivalent modifications or substitutions are included in the scope defined by the claims of the present application.

Claims (9)

1. A low-odor PET composite material with good physical properties is characterized in that: the composition is prepared from the following components in parts by weight:
80 to 100 portions of PET, and the mixture,
8 to 12 portions of modifier of poly glycidyl methacrylate-styrene-dimethyl siloxane,
0.1 to 0.5 portion of antioxidant.
2. The PET composite material according to claim 1, characterized in that: the preparation method of the modifier of poly glycidyl methacrylate-styrene-dimethyl siloxane comprises the following steps:
(1) adding emulsifier sodium dodecyl benzene sulfonate, initiator sodium persulfate, glycidyl methacrylate, styrene, cross-linking agent ethylene glycol dimethacrylate and deionized water into a reaction vessel, and stirring and reacting at 60-80 ℃ for 10-16h to obtain solution A;
(2) weighing the solution A, initiator sodium persulfate and dimethyl dichlorosilane, adding into a reaction vessel, and stirring at 70-90 ℃ for reacting for 8-12h to obtain solution B;
(3) weighing the solution B and a magnesium sulfate solution, adding the solution B and the magnesium sulfate solution into a reaction vessel, and stirring and reacting for 6-8h at 50-70 ℃ to obtain a solution C;
(4) and carrying out suction filtration, washing and drying on the solution C to obtain the modifier of poly glycidyl methacrylate-styrene-dimethyl siloxane.
3. The PET composite of claim 2, characterized in that: in the step (1), the mass ratio of the emulsifier sodium dodecyl benzene sulfonate, the initiator sodium persulfate, the glycidyl methacrylate, the styrene, the cross-linking agent ethylene glycol dimethacrylate and the deionized water is (0.2-0.4): (0.1-0.3): (30-40): (20-30): (0.1-0.3): (160-200).
4. The PET composite of claim 2, characterized in that: in the step (2), the mass ratio of the solution A, the initiator sodium persulfate and the dimethyldichlorosilane is (60-80): (0.1-0.3): (10-16).
5. The PET composite of claim 2, characterized in that: in the step (3), the mass ratio of the solution B to the magnesium sulfate solution is (70-90): (20-30).
6. The PET composite of claim 1, characterized in that: the antioxidant is at least one of antioxidant 168, antioxidant 1010 and antioxidant 1330.
7. A process for the preparation of a PET composite material as claimed in any one of claims 1 to 6, characterized in that: the method comprises the following steps:
(1) weighing PET, modifier poly glycidyl methacrylate-styrene-dimethyl siloxane and antioxidant according to a proportion, putting into an autoclave in a supercritical carbon dioxide environment, and uniformly mixing to obtain a mixture;
(2) and (2) adding the mixture obtained in the step (1) into a double-screw extruder for extrusion granulation to obtain the PET composite material.
8. The method of claim 7, wherein: the temperature of the high-pressure autoclave in the step (1) is 30-40 ℃, and the pressure is 6-8 MPa.
9. The method of claim 7, wherein: in the step (2), the twin-screw extruder comprises six temperature zones which are sequentially arranged, and the temperature of each zone is as follows: the temperature of the first zone is 240-260 ℃, the temperature of the second zone is 280-300 ℃, the temperature of the third zone is 280-300 ℃, the temperature of the fourth zone is 280-300 ℃, the temperature of the fifth zone is 280-300 ℃, the temperature of the sixth zone is 280-300 ℃, the temperature of the machine head is 280-300 ℃, and the rotating speed of the screw is 200-280 r/min.
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