CN110903486A - Compatilizer, preparation method thereof and PET/inorganic filler composite material - Google Patents

Compatilizer, preparation method thereof and PET/inorganic filler composite material Download PDF

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CN110903486A
CN110903486A CN201911210439.6A CN201911210439A CN110903486A CN 110903486 A CN110903486 A CN 110903486A CN 201911210439 A CN201911210439 A CN 201911210439A CN 110903486 A CN110903486 A CN 110903486A
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pet
compatilizer
inorganic filler
composite material
sample
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CN110903486B (en
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刘凯
包翰
张龙
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Anhui Jianghuai Automobile Group Corp
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Anhui Jianghuai Automobile Group Corp
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G81/00Macromolecular compounds obtained by interreacting polymers in the absence of monomers, e.g. block polymers
    • C08G81/02Macromolecular compounds obtained by interreacting polymers in the absence of monomers, e.g. block polymers at least one of the polymers being obtained by reactions involving only carbon-to-carbon unsaturated bonds
    • C08G81/024Block or graft polymers containing sequences of polymers of C08C or C08F and of polymers of C08G
    • C08G81/027Block or graft polymers containing sequences of polymers of C08C or C08F and of polymers of C08G containing polyester or polycarbonate sequences
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L67/00Compositions of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Compositions of derivatives of such polymers
    • C08L67/02Polyesters derived from dicarboxylic acids and dihydroxy compounds
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/24Acids; Salts thereof
    • C08K3/26Carbonates; Bicarbonates
    • C08K2003/265Calcium, strontium or barium carbonate
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/30Sulfur-, selenium- or tellurium-containing compounds
    • C08K2003/3045Sulfates
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00Polymer mixtures characterised by other features
    • C08L2205/08Polymer mixtures characterised by other features containing additives to improve the compatibility between two polymers

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Abstract

The invention discloses a compatilizer, a preparation method thereof and a PET/inorganic filler composite material, and relates to the technical field of compatilizers. The preparation method of the compatilizer comprises the following steps: PET, ethylene-octene front-segment copolymer, FeCl3Adding diisopropyl peroxydicarbonate and deionized water into a reaction kettle, keeping the pressure in the kettle at 10-12 MPa, and reacting for 16-20 h; after the reaction in the reaction kettle is finished, the reaction kettle is arranged in the jacketIntroducing cooling water and releasing pressure, cooling to 25-30 ℃, filtering, and taking out a sample A; and (3) soaking the sample A in N, N-dimethylformamide, carrying out suction filtration, and drying to obtain the compatilizer. The compatilizer prepared by the invention can improve the compatibility between PET and inorganic filler in the PET/inorganic filler composite material, thereby improving the physical property of the PET/inorganic filler composite material.

Description

Compatilizer, preparation method thereof and PET/inorganic filler composite material
Technical Field
The invention relates to the technical field of compatilizers, in particular to a compatilizer, a preparation method thereof and a PET/inorganic filler composite material.
Background
Polyolefins (e.g., PP, PS, PET, etc.) are widely used thermoplastics that have many advantageous properties, but have poor impact toughness and low dimensional stability, particularly at room and low temperatures, which limits their utility. CaCO addition to polyolefin plastics3The inorganic fillers such as talcum powder, wollastonite, mica and the like can not only reduce the cost and improve the rigidity, hardness and heat resistance of the material, but also improve the dimensional stability, creep resistance and the like of a product, and can also endow the material with special properties such as flame retardance, conductive function and the like. However, the polyolefin and the inorganic filler have large polarity difference and poor compatibility, so that the inorganic filler is difficult to uniformly disperse in the polyolefin, the interface adhesive force is low, and the physical properties of the material, such as impact strength, tensile strength, flexural modulus and the like, are reduced. At present, for the surface treatment of the filler, a traditional surfactant or an organic coupling agent (such as stearic acid, silane, aluminate and the like) is mainly adopted, although the dispersibility and the interfacial adhesion of the filler can be improved, the improvement of the physical properties of the composite material is limited because the organic chain segment of the organic coupling agent is short and has small effect with a matrix.
In recent years, scholars at home and abroad research the macromolecular compatilizer filled plastic, and find that the macromolecular compatilizer can promote the dispersion of the filler in the matrix, improve the interface adhesion between the filler and the matrix and between the matrix and the coupling agent, and overcome the defect of weak action between the traditional coupling agent and the matrix, thereby improving the comprehensive performance of the composite material. The commonly used compatibilizer for modifying the compatibility between the inorganic filler and the polyolefin in the market at present is SEBS-g-MAH, and the application of the SEBS-g-MAH to the composite material of the polyolefin/inorganic filler can improve the physical properties of the composite material of the polyolefin/inorganic filler to a certain extent, but the SEBS-g-MAH has an effect on various composite materials of the polyolefin/inorganic filler (such as a PP/inorganic filler composite material, a PE/inorganic filler composite material and a PA 6/inorganic filler composite material) although the SEBS-g-MAH is widely applied, but has no pertinence, and has an unsatisfactory effect on improving the compatibility between PET and the inorganic filler in the composite material of the PET/inorganic filler.
Disclosure of Invention
The invention mainly aims to provide a compatilizer, a preparation method thereof and a PET/inorganic filler composite material, and aims to solve the problem that the compatibility between PET and inorganic filler in the PET/inorganic filler composite material improved by the conventional compatilizer is not ideal.
In order to achieve the above object, the present invention provides a method for preparing a compatibilizer, which comprises the following steps:
PET, ethylene-octene front-segment copolymer, FeCl3Adding diisopropyl peroxydicarbonate and deionized water into a reaction kettle, keeping the pressure in the kettle at 10-12 MPa, and reacting for 16-20 h;
after the reaction in the reaction kettle is finished, introducing cooling water into the reaction kettle jacket, releasing the pressure, cooling to 25-30 ℃, filtering, and taking out a sample A;
and (3) soaking the sample A in N, N-dimethylformamide, carrying out suction filtration, and drying to obtain the compatilizer.
Optionally, the PET, ethylene-octene front-end copolymer, FeCl3The mass ratio of the diisopropyl peroxydicarbonate to the deionized water is (60-70): (12-16): (0.4-0.8): (0.2-0.6): (280-320).
Optionally, the step of soaking the sample a in N, N-dimethylformamide, filtering, and drying to obtain the compatibilizer comprises: the soaking time is 6-8 h.
Optionally, the step of soaking the sample a in N, N-dimethylformamide, filtering, and drying to obtain the compatibilizer comprises: the drying temperature is 30-60 ℃, and the drying time is 4-7 h.
In addition, the invention also provides a compatilizer, and the compatilizer is prepared by the preparation method of the compatilizer.
In addition, the invention also provides a PET/inorganic filler composite material, which comprises PET, a compatilizer and an inorganic filler, wherein the compatilizer is the compatilizer.
Optionally, the inorganic filler comprises any one of talc powder, calcium carbonate, barium sulfate, mica powder and wollastonite.
In the preparation method of the compatilizer, FeCl is utilized firstly3Lewis acid capable of absorbing molecules or atomic groups of electron cloud is formed to be used as a catalyst for alkylation reaction of a blending system, meanwhile, a benzene ring on PET can be used as an active site and has coupling reaction with free radicals in an ethylene-octene front-stage copolymer (OBC), and then the free radicals after chain scission of the PET can be grafted onto the benzene ring through the free radical reaction under the catalysis of the Lewis acid, so that the grafted copolymer of the PET-g-OBC, namely a compatilizer, is generated. Compared with the prior SEBS-g-MAH applied to the PET/inorganic filler composite material, the PET-g-OBC has higher surface grafting rate, so that the compatilizer prepared by the invention can improve the compatibility between PET and the inorganic filler in the PET/inorganic filler composite material, thereby improving the physical property of the PET/inorganic filler composite material.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other related drawings can be obtained according to the drawings without creative efforts.
Fig. 1 is a schematic flow chart of an embodiment of a method for preparing a compatibilizer according to the present invention.
The implementation, functional features and advantages of the objects of the present invention will be further explained with reference to the accompanying drawings.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. It is to be understood that the described embodiments are merely a few embodiments of the invention, and not all embodiments.
It should be noted that those whose specific conditions are not specified in the examples were performed according to the conventional conditions or the conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially. In addition, technical solutions between various embodiments may be combined with each other, but must be realized by a person skilled in the art, and when the technical solutions are contradictory or cannot be realized, such a combination should not be considered to exist, and is not within the protection scope of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The commonly used compatilizer SEBS-g-MAH in the market at present has an unsatisfactory effect of improving the compatibility between PET and an inorganic filler in a PET/inorganic filler composite material, so that the invention provides a preparation method of the compatilizer, and the prepared compatilizer can improve the compatibility between PET and the inorganic filler in the PET/inorganic filler composite material, thereby improving the physical property of the PET/inorganic filler composite material. With reference to the schematic flow chart of an embodiment of the method for preparing the compatibilizer provided in fig. 1, the method for preparing the compatibilizer comprises the following steps:
step S10, mixing PET, ethylene-octene front-segment copolymer, FeCl3Adding diisopropyl peroxydicarbonate and deionized water into a reaction kettle, keeping the pressure in the kettle at 10-12 MPa, and reacting for 16-20 h.
Wherein the PET, the ethylene-octene front-segment copolymer and the FeCl3The mass ratio of the diisopropyl peroxydicarbonate to the deionized water is (60-70): (12-16): (0.4-0.8): (0.2-0.6): (280-320).
And S20, after the reaction in the reaction kettle is finished, introducing cooling water into the reaction kettle jacket, releasing the pressure, cooling to 25-30 ℃, filtering, and taking out the sample A.
And step S30, soaking the sample A in N, N-dimethylformamide, filtering, and drying to obtain the compatilizer.
In order to fully dissolve the reacted impurities, the sample A is soaked for 6-8 h. In addition, in order to ensure that the drying effect is better, the drying temperature is 30-60 ℃, and the drying time is 4-7 h.
In the preparation method of the compatilizer, FeCl is utilized firstly3Lewis acid capable of absorbing molecules or atomic groups of electron cloud is formed to be used as a catalyst for alkylation reaction of a blending system, meanwhile, a benzene ring on PET can be used as an active site and has coupling reaction with free radicals in an ethylene-octene front-stage copolymer (OBC), and then the free radicals after chain scission of the PET can be grafted onto the benzene ring through the free radical reaction under the catalysis of the Lewis acid, so that the grafted copolymer of the PET-g-OBC, namely a compatilizer, is generated. Compared with the PET/inorganic filler composite material applied with SEBS-g-MAH, the PET-g-OBC has higher surface grafting rate, so that the compatilizer prepared by the invention can improve the compatibility between PET and the inorganic filler in the PET/inorganic filler composite material, thereby improving the physical property of the PET/inorganic filler composite material.
In addition, the invention also provides a compatilizer, and the compatilizer is prepared by the preparation method of the compatilizer.
Further, the invention also provides a PET/inorganic filler composite material, which comprises PET, a compatilizer and an inorganic filler, wherein the compatilizer is the compatilizer.
Wherein the inorganic filler comprises any one of talcum powder, calcium carbonate, barium sulfate, mica powder and wollastonite. It should be noted that the inorganic filler of the present invention is not limited to these examples, and other inorganic fillers blended with PET to prepare the composite material are also within the protection scope of the present invention, such as kaolin and coal gangue powder, which can be used as inorganic fillers, and any one of talc powder, calcium carbonate, barium sulfate, mica powder and wollastonite is used as the inorganic filler, so that the compatibilizer provided by the present invention has a better effect of improving the compatibility between PET and the inorganic filler.
The technical solutions of the present invention are further described in detail below with reference to specific examples and drawings, it should be understood that the following examples are merely illustrative of the present invention and are not intended to limit the present invention.
In the following examples, the source information of the raw materials used is as follows: PET (model 008L), Aclo, canada; OBC, dow group of america; FeCl3Chemical engineering of denn guren; diisopropyl peroxydicarbonate, a company of limited liability of industrial Haoyanhua, Jinan; n, N-Dimethylformamide (DMF), chemical ltd, denn century todda; talc, laizhou sunward talc, ltd; mica powder, Chuzhou Wanqiao sericite factory; calcium carbonate, Jiangxi Fenglii chemical Co., Ltd; barium sulfate, Shenzhen Jiaxin chemical Limited liability company; wollastonite, Jiangxi Ke extra fine powder Co., Ltd; SEBS-g-MAH, Deba, Nanjing, high molecular materials, Inc.; antioxidants (type Irganox168, Irganox1010, Irganox1330), from Bassfer.
The following examples used the following test instrument types: model ZSK30 twin-screw extruder, W & P, Germany; JL-1000 type tensile testing machine, produced by Guangzhou Youcai laboratory instruments; HTL900-T-5B injection molding machine, manufactured by Haita plastics machinery, Inc.; XCJ-500 impact tester, manufactured by Chengde tester; QT-1196 tensile tester, Gaotai detection instruments, Inc. of Dongguan; QD-GJS-B12K model high-speed mixer, HengOde instruments, Beijing.
Example 1
(1) 600g of PET, 120g of an ethylene-octene front-end copolymer (OBC), and 4g of FeCl were weighed32g of diisopropyl peroxydicarbonate and 2.8kg of deionized water are put into a reaction kettle, the pressure in the kettle is kept at 10MPa, and the reaction lasts for 16 hours.
(2) And after the reaction is finished, introducing cooling water into the reaction kettle jacket, releasing the pressure, cooling to 25 ℃, filtering, and taking out the sample A.
(3) And (3) soaking the sample A in N, N-Dimethylformamide (DMF) for 6h, carrying out suction filtration, and drying (the drying temperature is 30 ℃, and the drying time is 7h) to obtain the compatilizer P1.
Application example 1
15 parts of talcum powder and 5 parts of the compatilizer P1 prepared in example 1 are added into 80 parts of PET, stirred for 10min by a high-speed mixer, and then added into a double-screw extruder (the temperature and the screw rotation speed of each zone of the double-screw extruder are respectively 240 ℃ in the first zone, 280 ℃ in the second zone, 280 ℃ in the third zone, 280 ℃ in the fourth zone, 280 ℃ in the fifth zone, 280 ℃ in the sixth zone, 280 ℃ in the head and 200r/min of the screw) for blending and extrusion, so that the PET/talcum powder composite material X1 is obtained.
Comparative example 1
The procedure was the same as in application example 1, except that: a PET/talc composite D1 was prepared by replacing 5 parts of the compatibilizer P1 prepared in example 1 with 5 parts of commercially available SEBS-g-MAH.
The PET/talc composite X1 prepared in comparative example 1 and the PET/talc composite D1 prepared in comparative example 1 were molded into specimens by an injection molding machine, and the physical property data of the specimens are shown in Table 1:
TABLE 1 results of physical Properties measurements
Test items Test standard Unit of X1 D1
Tensile strength ASTM D638 MPa 65 60
Flexural modulus ASTM D790 MPa 3180 2800
Impact strength of cantilever beam ASTM D256 kJ/m2 4.8 3.2
As can be seen from Table 1, the tensile strength, bending strength and Izod impact strength of X1 are all higher than those of D1, which shows that the compatibility and physical properties of the PET-talcum powder modified by the compatibilizer P1 prepared in example 1 are better than those of the SEBS-g-MAH sold on the market.
Example 2
(1) 700g of PET, 160g of an ethylene-octene front-end copolymer (OBC), and 8g of FeCl were weighed36g of diisopropyl peroxydicarbonate and 3.2kg of deionized water are put into a reaction kettle, the pressure in the kettle is kept at 12MPa, and the reaction is carried out for 20 hours.
(2) And after the reaction is finished, introducing cooling water into the reaction kettle jacket, releasing the pressure, cooling to 28 ℃, filtering, and taking out the sample A.
(3) And (3) soaking the sample A in N, N-Dimethylformamide (DMF) for 8 hours, carrying out suction filtration, and drying (the drying temperature is 60 ℃, and the drying time is 4 hours), thus obtaining the compatilizer P2.
Application example 2
15 parts of calcium carbonate and 5 parts of the compatibilizer P2 prepared in example 2 are added into 80 parts of PET, stirred for 10min by a high-speed mixer, and then added into a double-screw extruder (the temperature and the screw rotation speed of each zone of the double-screw extruder are respectively 260 ℃ in the first zone, 300 ℃ in the second zone, 300 ℃ in the third zone, 300 ℃ in the fourth zone, 300 ℃ in the fifth zone, 300 ℃ in the sixth zone, 300 ℃ at the head and 280r/min in the screw) to be blended and extruded, so that the PET/calcium carbonate composite material X2 is obtained.
Comparative example 2
The procedure was the same as in application example 2, except that: a PET/calcium carbonate composite D2 was prepared by replacing 5 parts of the compatibilizer P2 prepared in example 2 with 5 parts of a commercially available SEBS-g-MAH.
The PET/calcium carbonate composite material X2 prepared in comparative example 2 and the PET/calcium carbonate composite material D2 prepared in comparative example 2 were molded into bars by an injection molding machine, and the physical property data of the product are shown in Table 1:
TABLE 2 results of physical Properties measurements
Test items Test standard Unit of X2 D2
Tensile strength ASTM D638 MPa 62 58
Flexural modulus ASTM D790 MPa 3120 2650
Impact strength of cantilever beam ASTM D256 kJ/m2 4.8 3.1
As can be seen from Table 2, the tensile strength, flexural strength and Izod impact strength of X2 are all higher than those of D1, which shows that the compatibility and physical properties of the modified PET-calcium carbonate modified by the compatibilizer P2 prepared in example 2 are better than those of the commercially available SEBS-g-MAH.
Example 3
(1) 650g of PET, 140g of ethylene-octene front-end copolymer (OBC), 6g of FeCl3, 4g of diisopropyl peroxydicarbonate and 3.0kg of deionized water are weighed and put into a reaction kettle, the pressure in the kettle is kept at 11MPa, and the reaction lasts for 18 hours.
(2) And after the reaction is finished, introducing cooling water into the reaction kettle jacket, releasing the pressure, cooling to 30 ℃, filtering, and taking out the sample A.
(3) And (3) soaking the sample A in N, N-Dimethylformamide (DMF) for 7h, carrying out suction filtration, and drying (the drying temperature is 40 ℃, and the drying time is 6h) to obtain the compatilizer P3.
Application example 3
15 parts of barium sulfate and 5 parts of the compatibilizer P3 prepared in example 3 are added into 80 parts of PET, stirred for 10min by a high-speed mixer, and then added into a double-screw extruder (the temperature and the screw rotation speed of each zone of the double-screw extruder are respectively 250 ℃ in the first zone, 290 ℃ in the second zone, 290 ℃ in the third zone, 290 ℃ in the fourth zone, 290 ℃ in the fifth zone, 290 ℃ in the sixth zone, 290 ℃ in the head and 240r/min in the screw) to be blended and extruded, so that the PET/barium sulfate composite material X3 is obtained.
Comparative example 3
The procedure was the same as in application example 3, except that: a PET/barium sulfate composite D3 was prepared by replacing 5 parts of the compatibilizer P3 prepared in example 3 with 5 parts of a commercially available SEBS-g-MAH.
The PET/barium sulfate composite material X3 prepared in comparative example 3 and the PET/barium sulfate composite material D3 prepared in comparative example 3 were molded into bars by an injection molding machine, and the physical property data of the product are shown in Table 3:
TABLE 3 results of physical Properties measurements
Test items Test standard Unit of X3 D3
Tensile strength ASTM D638 MPa 69 63
Flexural modulus ASTM D790 MPa 3350 2920
Impact strength of cantilever beam ASTM D256 kJ/m2 5.2 3.5
As can be seen from Table 3, the tensile strength, flexural strength and Izod impact strength of X3 are all higher than those of D3, which shows that the compatibility and physical properties of the modified PET-barium sulfate prepared by adding the compatibilizer P3 prepared in example 3 are better than those of the commercially available SEBS-g-MAH.
Example 4
(1) 640g of PET, 150g of ethylene-octene front-end copolymer (OBC), 7g of FeCl3, 5g of diisopropyl peroxydicarbonate and 3.1kg of deionized water are weighed and put into a reaction kettle, the pressure in the kettle is kept at 10MPa, and the reaction is carried out for 20 hours.
(2) And after the reaction is finished, introducing cooling water into the reaction kettle jacket, releasing the pressure, cooling to 29 ℃, filtering, and taking out the sample A.
(3) And (3) soaking the sample A in N, N-Dimethylformamide (DMF) for 6h, carrying out suction filtration, and drying (the drying temperature is 50 ℃, and the drying time is 5h) to obtain the compatilizer P4.
Application example 4
15 parts of mica powder and 5 parts of the compatilizer P4 prepared in the embodiment 4 are added into 80 parts of PET, stirred for 10min by a high-speed mixer, and then added into a double-screw extruder (the temperature and the screw rotation speed of each zone of the double-screw extruder are respectively 245 ℃ in the first zone, 285 ℃ in the second zone, 285 ℃ in the third zone, 285 ℃ in the fourth zone, 285 ℃ in the fifth zone, 285 ℃ in the sixth zone, 285 ℃ in a machine head and 255r/min in the screw) for blending and extrusion, so that the PET/mica composite material X4 is obtained.
Comparative example 4
The procedure was the same as in application example 4, except that: 5 parts of the compatibilizer P4 obtained in example 4 were replaced by 5 parts of a commercially available SEBS-g-MAH, giving a composite D4 of PET/mica powder.
The PET/mica powder composite material X4 prepared by the application comparative example 4 and the PET/mica powder composite material D4 prepared by the comparative example 4 are made into sample bars by an injection molding machine, and the physical property data of the product are shown in Table 4:
TABLE 4 results of physical Properties measurements
Test items Test standard Unit of X4 D4
Tensile strength ASTM D638 MPa 65 61
Flexural modulus ASTM D790 MPa 3380 2850
Impact strength of cantilever beam ASTM D256 kJ/m2 5.2 3.3
As can be seen from Table 4, the tensile strength, flexural strength and Izod impact strength of X4 are all higher than those of D4, which shows that the compatibility and physical properties of the P4 modified PET-mica powder prepared by adding the compatilizer prepared in example 4 are better than those of the SEBS-g-MAH powder sold on the market.
Example 5
(1) 620g of PET, 150g of ethylene-octene front-end copolymer (OBC), 5g of FeCl3, 3g of diisopropyl peroxydicarbonate and 2.9kg of deionized water are weighed and put into a reaction kettle, the pressure in the kettle is kept at 10MPa, and the reaction is carried out for 20 hours.
(2) And after the reaction is finished, introducing cooling water into the reaction kettle jacket, releasing the pressure, cooling to 27 ℃, filtering, and taking out the sample A.
(3) And (3) soaking the sample A in N, N-Dimethylformamide (DMF) for 7h, carrying out suction filtration, and drying (the drying temperature is 40 ℃, and the drying time is 6h) to obtain the compatilizer P5.
Application example 5
15 parts of wollastonite and 5 parts of the compatibilizer P5 prepared in example 5 are added into 80 parts of PET, stirred for 10min by a high-speed mixer, and then added into a double-screw extruder (the temperature and the screw rotation speed of each zone of the double-screw extruder are respectively 250 ℃ in the first zone, 295 ℃ in the second zone, 295 ℃ in the third zone, 295 ℃ in the fourth zone, 295 ℃ in the fifth zone, 295 ℃ in the sixth zone, 295 ℃ in the head and 270r/min in the screw) to be blended and extruded, so that the PET/wollastonite composite material X5 is obtained.
Comparative example 5
The procedure was the same as in application example 5, except that: a composite D5 of PET/wollastonite was prepared by replacing 5 parts of the compatibilizer P5 prepared in example 1 with 5 parts of a commercially available SEBS-g-MAH.
The PET/wollastonite composite material X5 prepared in comparative example 5 and the PET/wollastonite composite material D5 prepared in comparative example 5 were molded into specimens by an injection molding machine, and the physical property data of the products are shown in Table 5:
TABLE 5 results of physical Properties measurements
Test items Test standard Unit of X5 D5
Tensile strength ASTM D638 MPa 65 61
Flexural modulus ASTM D790 MPa 3290 2850
Impact strength of cantilever beam ASTM D256 kJ/m2 5.3 3.3
As can be seen from Table 5, the tensile strength, flexural strength and Izod impact strength of X5 are all higher than those of D5, which shows that the compatibility of the P5 modified PET-wollastonite prepared by adding the compatilizer prepared in example 5 is better than that of the SEBS-g-MAH sold on the market, and the physical properties are also better.
In conclusion, compared with the conventional commonly used compatilizer, the compatilizer prepared by the preparation method of the compatilizer provided by the invention is applied to the PET/inorganic filler composite material, and has more excellent physical properties, namely, the effect of improving the compatibility between PET and the inorganic filler is better. Therefore, the compatilizer of the invention can improve the compatibility between PET and the inorganic filler in the PET/inorganic filler composite material, thereby improving the physical properties of the PET/inorganic filler composite material.
The above is only a preferred embodiment of the present invention, and it is not intended to limit the scope of the invention, and various modifications and changes will occur to those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention shall be included in the scope of the present invention.

Claims (7)

1. A preparation method of a compatilizer is characterized by comprising the following steps:
PET, ethylene-octene front-segment copolymer, FeCl3Adding diisopropyl peroxydicarbonate and deionized water into a reaction kettle, keeping the pressure in the kettle at 10-12 MPa, and reacting for 16-20 h;
after the reaction in the reaction kettle is finished, introducing cooling water into the reaction kettle jacket, releasing the pressure, cooling to 25-30 ℃, filtering, and taking out a sample A;
and (3) soaking the sample A in N, N-dimethylformamide, carrying out suction filtration, and drying to obtain the compatilizer.
2. The method of claim 1, wherein the PET, the ethylene-octene front-end copolymer, the FeCl3The mass ratio of the diisopropyl peroxydicarbonate to the deionized water is (60-70): (12-16): (0.4-0.8): (0.2-0.6): (280-320).
3. The method for preparing the compatilizer according to claim 1, wherein the step of obtaining the compatilizer by soaking the sample A in N, N-dimethylformamide, performing suction filtration and drying comprises the following steps: the soaking time is 6-8 h.
4. The method for preparing the compatilizer according to claim 1, wherein the step of obtaining the compatilizer by soaking the sample A in N, N-dimethylformamide, performing suction filtration and drying comprises the following steps: the drying temperature is 30-60 ℃, and the drying time is 4-7 h.
5. A compatibilizer, which is produced by the method for producing a compatibilizer according to any one of claims 1 to 4.
6. A PET/inorganic filler composite comprising PET, a compatibilizer and an inorganic filler, wherein the compatibilizer is the compatibilizer defined in claim 5.
7. The PET/inorganic filler composite according to claim 6, wherein the inorganic filler comprises any one of talc, calcium carbonate, barium sulfate, mica powder and wollastonite.
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