CN111825802B - Ethylene oxide-octene copolymer composition and preparation method thereof - Google Patents

Ethylene oxide-octene copolymer composition and preparation method thereof Download PDF

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CN111825802B
CN111825802B CN201910330534.3A CN201910330534A CN111825802B CN 111825802 B CN111825802 B CN 111825802B CN 201910330534 A CN201910330534 A CN 201910330534A CN 111825802 B CN111825802 B CN 111825802B
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octene copolymer
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ethylene
copolymer composition
poe
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李坤泉
柴生勇
李积德
陈林
刘勤
李岩
刘振峰
汪廷洪
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Kingfa Science and Technology Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F255/00Macromolecular compounds obtained by polymerising monomers on to polymers of hydrocarbons as defined in group C08F10/00
    • C08F255/02Macromolecular compounds obtained by polymerising monomers on to polymers of hydrocarbons as defined in group C08F10/00 on to polymers of olefins having two or three carbon atoms
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F2/00Processes of polymerisation
    • C08F2/44Polymerisation in the presence of compounding ingredients, e.g. plasticisers, dyestuffs, fillers
    • 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
    • C08K3/34Silicon-containing compounds

Abstract

The invention provides an ethylene oxide-octene copolymer composition, which comprises, by weight, 0.2% -10.0% of styrene monomers, 0.5% -10.0% of glycidyl methacrylate monomers and/or glycidyl methacrylate derivative monomers, 70.0% -99.0% of ethylene-octene copolymers and 0.2% -10.0% of talcum powder. According to the invention, the talcum powder is added, so that the grafting rate of the epoxidized ethylene-octene copolymer is ensured, and the crosslinking degree is reduced; the melting point of the initiator is further preferred, further reducing the degree of crosslinking.

Description

Ethylene oxide-octene copolymer composition and preparation method thereof
Technical Field
The invention relates to the technical field of high polymer materials, in particular to an ethylene oxide-octene copolymer composition and a preparation method thereof.
Background
Ethylene-octene copolymer (POE) is a new type of thermoplastic elastomer developed by metallocene, and has plasticity of plastics and elasticity of rubber. The POE mainly comprises a polyethylene crystallization area and a polyoctene amorphous area, and the special structure endows the POE with excellent mechanical property, rheological property and ultraviolet resistance. In addition, POE has good low-temperature toughness, good compatibility with polyolefin and low price, so that the POE is widely applied to toughening modification of plastics.
The method is the simplest and most effective method for carrying out melt grafting modification on POE by taking Glycidyl Methacrylate (GMA) as a monomer and adopting a double screw. However, in the melt grafting process, on one hand, the liquid GMA monomer is unevenly dispersed in the resin and is easily self-polymerized at high temperature, so that the grafting efficiency is low; on the other hand, in the presence of an initiator, a free radical chain segment generated in the POE resin is easy to crosslink, the melt index is greatly reduced, the flowability of the product is poor, and the toughening efficiency is reduced. Therefore, the preparation of GMA grafted POE with high grafting ratio and low crosslinking degree is the focus of research and development.
In order to improve the melt fluidity of POE and reduce the crosslinking degree of the POE, the Chinese patent (CN 101747600B) adds a crosslinking inhibitor triphenyl phosphite or dimethylformamide to capture and quench free radicals generated in a molecular chain of the POE, so that the crosslinking degree of the POE is reduced, but the method hinders the grafting reaction, so that the grafting rate of the obtained product is lower. Chinese patent (CN 102391432B) discloses a high-fluidity ethylene-alpha-octene graft copolymer and a preparation method thereof, which inhibit the POE crosslinking phenomenon in the extrusion process by selecting high-fluidity POE resin and adding various additives such as a lubricant, an antioxidant, a liquid additive and the like into the system, but the added additives are more, the reaction system is more complex and the reaction is difficult to control. In order to improve the dispersion of the monomer and the initiator in the resin, the chinese patent (CN 106674432 a) starts from an extrusion reaction device, and they adopt a sectional feeding manner to feed the reaction monomer and the initiator in the second or fifth section of a twin-screw, so as to reduce the generation of cross-linking by-products in the melt grafting process of the polymer, but the preparation method is cumbersome. Chinese patent (CN 104479078A) also adopts a method of compounding a casting film forming device and a double-screw extrusion device, and reduces the phenomenon of uneven monomer dispersion and the occurrence of cross-linking side reaction in the reaction process by spraying a monomer and an initiator after polymer casting film forming and then carrying out double-screw reactive extrusion, but the operations are more complicated, and need to be carried out for a plurality of times, and special equipment is also needed.
Disclosure of Invention
The present invention has been made to overcome the above technical problems, and an object of the present invention is to provide an epoxidized ethylene-octene copolymer composition in which the degree of crosslinking is improved while the graft ratio is ensured.
Another object of the present invention is to provide a process for producing an epoxidized ethylene-octene copolymer composition, which is simple in process, can suppress the self-polymerization of GMA and the progress of POE crosslinking reaction during grafting, and can further produce an epoxidized ethylene-octene copolymer having a low degree of crosslinking.
The invention is realized by the following technical scheme:
an ethylene oxide-octene copolymer composition comprises, by weight, 0.2% -10.0% of styrene monomers, 0.5% -10.0% of glycidyl methacrylate monomers and/or glycidyl methacrylate derivative monomers, 70.0% -99.0% of ethylene-octene copolymers, and 0.2% -10.0% of talcum powder.
Before and after the grafting reaction, the talcum powder plays a role in promoting the reaction and reducing crosslinking, and the talcum powder is not consumed. Other monomers, and ethylene-octene copolymers, are consumed during the reaction, but are generally not completely reacted, leaving some unreacted monomer or ethylene-octene copolymer in the final product.
The epoxidized ethylene-octene copolymer composition also comprises an initiator.
During the reaction, most of the initiator is decomposed, most of the initiator exists in other compound forms in the product, and the initiator used can be deduced according to the reaction mechanism by detecting the corresponding compound.
Customary initiators, such as dicumyl peroxide, having a melting point of 42 ℃ (abbreviated to DCP in English); cumene hydroperoxide, melting point 53 ℃; dibenzoyl peroxide, melting point 103-; n-butyl 4, 4-di (t-butylperoxy) valerate, mp 146 ℃; diacetyl peroxide, melting point 30 ℃; succinic peroxide, melting point 125 ℃; dicumyl peroxide, melting point 40 ℃.
Preferably, said initiator is selected from initiators having a melting point below 10 ℃;
the initiator with the melting point lower than 10 ℃ is at least one selected from tert-amyl peroxyacetate, tert-amyl peroxybenzoate, 2-di (tert-butylperoxy) butane, tert-butyl peroxyisopropylcarbonate, tert-butyl peroxybenzoate, di-tert-amyl peroxide, 2, 5-di-tert-butyl peroxy-2, 5-dimethyl hexane, tert-butyl cumyl peroxide, di-tert-butyl peroxide, diisopropylbenzene hydroperoxide and 1,1,3, 3-tetramethylbutyl hydroperoxide.
It has been found that initiators having a melting point below 10 ℃ reduce the occurrence of local excessive crosslinking reactions and also promote grafting compared to initiators having a melting point above 10 ℃.
The density of the ethylene-octene copolymer is 0.860-0.880 g/cm -3 And a melt index of 0.5 to 18g/10min (190 ℃, 2.16 kg).
The glycidyl methacrylate derivative monomer is selected from allyl glycidyl ether or at least one of derivatives thereof.
The styrene monomer is at least one selected from styrene, alpha-methyl styrene, alpha-ethyl styrene and derivatives thereof.
Preferably, the particle size of the talcum powder is D90=2-15 microns.
The preparation method of the epoxidized ethylene-octene copolymer composition comprises the following steps: uniformly mixing a styrene monomer, a glycidyl methacrylate monomer and/or a glycidyl methacrylate derivative monomer, an ethylene-octene copolymer, talcum powder and an initiator, and then putting the mixture into a screw extruder for melting plasticization, extrusion, drying and grain cutting to obtain an epoxidized ethylene-octene copolymer composition; wherein the length-diameter ratio L/D of the screw extruder is = 30-60, the rotating speed is 150-500 rpm, and the temperature of each section of screw is 60-215 ℃.
Compared with the prior art, the invention has the following beneficial effects:
the invention provides a preparation method of an epoxidized ethylene-octene copolymer composition, and surprisingly discovers that the talcum powder can effectively inhibit the self-polymerization of GMA and the POE crosslinking reaction in the grafting process in the reactive extrusion process of a screw extruder, so that the epoxidized ethylene-octene copolymer has good fluidity. Furthermore, the invention finds that the melting point of the initiator is lower than 10 ℃, and the degree of crosslinking can be further reduced to improve the grafting rate. On the one hand, the phenomenon that the product grafting rate is lower due to the fact that a cross-inhibiting agent is introduced to capture free radicals is avoided, on the other hand, raw materials can be subjected to reactive extrusion after being uniformly mixed at one time, and the method is simple and convenient and does not need to use special equipment.
Detailed Description
The present invention will be further illustrated by the following specific embodiments, and the following examples are illustrative of the present invention and are not intended to limit the present invention.
Example 1
94.0% POE resin (density 0.870 g/cm) -3 The melt index is 5g/10 min), 3.0% GMA, 1.5% styrene, 0.3%2, 5-di-tert-butyl peroxy-2, 5-dimethyl hexane (melting point is lower than 8 ℃) and 1.2% talcum powder (particle size is D90=5 microns) are mixed uniformly in a high-speed mixer, and then the mixture is added into a double-screw extruder through a feeding hopper for reactive extrusion, the length-diameter ratio L/D =36 of the double-screw extruder is used, and the extrusion temperatures of the first section to the ninth section are respectively: the E-POE-1 can be obtained by melting, plasticizing, extruding, drying and granulating the materials at 60 ℃, 100 ℃, 190 ℃, 190 ℃, 190 ℃, 190 ℃, 200 ℃, 210 ℃ and 170 ℃ and at the screw rotating speed of 250 revolutions per minute.
Example 2
94.0% POE resin (density 0.870 g/cm) -3 After the melt index is 5g/10 min), 3.0% GMA, 1.5% styrene, 0.3% dicumyl peroxide (DCP, melting point 42 ℃) and 1.2% talcum powder (particle size is D90=5 microns) are uniformly mixed in a high-speed mixer, the mixture is added into a double-screw extruder through a feeding hopper for reactive extrusion, the length-diameter ratio L/D =36 of the double-screw extruder is used, and the extrusion temperatures of the first section to the ninth section are respectively: the E-POE-2 can be obtained by melting, plasticizing, extruding, drying and granulating the materials at 60 ℃, 100 ℃, 190 ℃, 190 ℃, 190 ℃, 200 ℃, 210 ℃, 170 ℃ and the screw rotating speed of 250 revolutions per minute.
Example 3
94.0% POE resin (density 0.870 g/cm) -3 Melt index of 5g/10 min), 3.0% GMA, 1.5% styrene, 0.3%2, 5-di-tert-butylperoxy-2, 5Dimethylhexane (melting point lower than 8 ℃) and 1.2% talc (particle size D90=20 μm) were mixed homogeneously in a high-speed mixer and then fed via a hopper into a twin-screw extruder for reactive extrusion, the twin-screw extruder having a length-to-diameter ratio L/D =36, the extrusion temperatures in the first to ninth stages were: the E-POE-3 can be obtained by melting, plasticizing, extruding, drying and granulating the materials at 60 ℃, 100 ℃, 190 ℃, 190 ℃, 190 ℃, 200 ℃, 210 ℃, 170 ℃ and the screw rotating speed of 250 revolutions per minute.
Example 4
90.0% POE resin (density 0.863 g/cm) -3 The melt index is 13g/10 min), 4.0% GMA, 3.0% styrene, 0.5% tert-amyl peroxyacetate (melting point is lower than 0 ℃) and 2.5% talcum powder (particle size is D90=2 microns) are mixed uniformly in a high-speed mixer, and then added into a double-screw extruder through a feeding hopper for reactive extrusion, the length-diameter ratio L/D =48 of the double-screw extruder is used, and the extrusion temperatures of the first section to the ninth section are respectively: the E-POE-4 can be obtained by melting, plasticizing, extruding, drying and granulating the materials at 60 ℃, 120 ℃, 190 ℃, 190 ℃, 190 ℃, 200 ℃, 210 ℃, 170 ℃ and the screw rotating speed of 350 r/min.
Example 5
68.0% of POE resin (density of 0.880 g/cm) -3 The melt index is 18g/10 min), 10.0% GMA, 10.0% alpha-ethyl styrene, 2.0% ditert amyl peroxide (melting point is lower than 0 ℃) and 10.0% talcum powder (particle size is D90=10 microns) are mixed uniformly in a high-speed mixer, and then the mixture is added into a double-screw extruder through a feeding hopper for reactive extrusion, the length-diameter ratio L/D =60 of the double-screw extruder is used, and the extrusion temperatures of the first section to the ninth section are respectively: the E-POE-5 can be obtained by melting, plasticizing, extruding, drying and granulating the materials at 60 ℃, 120 ℃, 190 ℃, 190 ℃, 190 ℃, 190 ℃, 200 ℃, 210 ℃ and 170 ℃ at a screw rotating speed of 200 revolutions per minute.
Example 6
99.0% POE resin (density 0.868 g/cm) -3 Melt index 0.5g/10 min), 0.5% allyl glycidyl ether, 0.2% styrene, 0.1%1,1,3, 3-tetramethylbutylhydroperoxide (melting point below 0 ℃ C.) and 0.2% of talcum powder (the particle size is D90=12 microns) is uniformly mixed in a high-speed mixer, and then is added into a double-screw extruder through a feeding hopper for reactive extrusion, the length-diameter ratio L/D =60 of the double-screw extruder is used, and the extrusion temperatures of the first section to the ninth section are respectively: the E-POE-6 can be obtained by melting, plasticizing, extruding, drying and granulating the materials at 60 ℃, 100 ℃, 190 ℃, 190 ℃, 210 ℃, 210 ℃, 210 ℃, 170 ℃ and the screw rotating speed of 500 revolutions per minute.
Example 7
78.0% POE resin (density 0.873 g/cm) -3 The melt index is 11g/10 min), 8.0% GMA, 6.0% alpha-methyl styrene, 1.2% tert-butyl peroxybenzoate (melting point is lower than 0 ℃) and 6.8% talcum powder (particle size is D90=8 microns) are mixed uniformly in a high-speed mixer, and then the mixture is added into a double-screw extruder through a feeding hopper for reactive extrusion, the length-diameter ratio L/D =48 of the double-screw extruder is used, and the extrusion temperatures of the first section to the ninth section are respectively: the E-POE-7 can be obtained by melting, plasticizing, extruding, drying and granulating the materials at 60 ℃, 100 ℃, 190 ℃, 190 ℃, 190 ℃, 200 ℃, 210 ℃, 170 ℃ and the screw rotating speed of 400 r/min.
Example 8
88.0% POE resin (density 0.875 g/cm) -3 After the melt index is 3g/10 min), 6.0% GMA, 2.0% styrene, 0.4% tert-butyl cumyl peroxide (melting point is lower than 0 ℃) and 3.6% talcum powder (particle size is D90=15 microns) are uniformly mixed in a high-speed mixer, the mixture is added into a double-screw extruder through a feeding hopper for reactive extrusion, the length-diameter ratio L/D =30 of the double-screw extruder is used, and the extrusion temperatures of the first section to the ninth section are respectively: the E-POE-8 can be obtained by melting, plasticizing, extruding, drying and granulating the materials at 60 ℃, 100 ℃, 190 ℃, 190 ℃, 190 ℃, 200 ℃, 210 ℃, 170 ℃ and the screw rotating speed of 150 revolutions per minute.
Example 9
90.0 percent of POE resin (the density is 0.875 g/cm) -3 Melt index 6g/10 min), 4.0% allyl glycidyl ether, 1.0% styrene, 1.5% diisopropylbenzene hydroperoxide (melting point below 0 ℃) and 3.5% talc (particle size D90=9 μm) were mixed in a high-speed mixerAfter uniform mixing, adding the mixture into a double-screw extruder through a feeding hopper for reactive extrusion, wherein the length-diameter ratio L/D =48 of the double-screw extruder, and the extrusion temperatures of the first section to the ninth section are respectively as follows: the E-POE-9 can be obtained by melting, plasticizing, extruding, drying and granulating the materials at 60 ℃, 100 ℃, 190 ℃, 190 ℃, 190 ℃, 210 ℃, 210 ℃, 170 ℃ and the screw rotating speed of 360 revolutions per minute.
Comparative example 1
94.0% POE resin (density 0.870 g/cm) -3 The melt index is 5g/10 min), 3.0% GMA, 1.5% styrene, 0.3%2, 5-di-tert-butyl peroxy-2, 5-dimethyl hexane (melting point is lower than 8 ℃) and 1.2% calcium carbonate (particle size is D90=5 microns) are mixed uniformly in a high-speed mixer, and then the mixture is added into a double-screw extruder through a feeding hopper for reactive extrusion, the length-diameter ratio L/D =36 of the double-screw extruder is used, and the extrusion temperatures of the first section to the ninth section are respectively: the E-POE-10 can be obtained by melting, plasticizing, extruding, drying and granulating the materials at 60 ℃, 100 ℃, 190 ℃, 190 ℃, 190 ℃, 190 ℃, 200 ℃, 210 ℃ and 170 ℃ and at the screw rotating speed of 250 revolutions per minute.
Comparative example 2
94.0% POE resin (density 0.870 g/cm) -3 After the melt index is 5g/10 min), 3.0% GMA, 1.5% styrene, 0.3%2, 5-di-tert-butyl peroxy-2, 5-dimethyl hexane (melting point is lower than 8 ℃) and 1.2% titanium dioxide (particle size is D90=5 microns) are mixed uniformly in a high-speed mixer, the mixture is added into a double-screw extruder through a feeding hopper for reactive extrusion, the length-diameter ratio L/D =36 of the double-screw extruder is used, and the extrusion temperatures of the first section to the ninth section are respectively: the E-POE-11 can be obtained by melting, plasticizing, extruding, drying and granulating the materials at 60 ℃, 100 ℃, 190 ℃, 190 ℃, 190 ℃, 200 ℃, 210 ℃, 170 ℃ and the screw rotating speed of 250 revolutions per minute.
Comparative example 3
95.2% POE resin (density 0.870 g/cm) -3 Melt index of 5g/10 min), 3.0 percent of GMA, 1.5 percent of styrene and 0.3 percent of 2, 5-di-tert-butyl peroxy-2, 5-dimethyl hexane (melting point is lower than 8 ℃) are mixed evenly in a high-speed mixer and added into a double-screw extruder through a feeding hopper for reactionSexual extrusion, the length-diameter ratio L/D of a double-screw extruder is =36, and the extrusion temperatures of the first section to the ninth section are respectively as follows: the E-POE-12 can be obtained by melting, plasticizing, extruding, drying and granulating the materials at 60 ℃, 100 ℃, 190 ℃, 190 ℃, 190 ℃, 200 ℃, 210 ℃, 170 ℃ and the screw rotating speed of 250 revolutions per minute.
Comparative example 4
95.0% POE resin (density 0.870 g/cm) -3 The melt index is 5g/10 min), 3.0 percent of GMA, 1.5 percent of styrene, 0.3 percent of 2, 5-di-tert-butyl peroxy-2, 5-dimethyl hexane (the melting point is lower than 8 ℃) and 0.2 percent of cross-linking inhibiting agent triphenyl phosphite are uniformly mixed in a high-speed mixer, and then added into a double-screw extruder through a feeding hopper for reactive extrusion, the length-diameter ratio L/D =36 of the double-screw extruder is used, and the extrusion temperatures from the first section to the ninth section are respectively: the E-POE-13 can be obtained by melting, plasticizing, extruding, drying and granulating the materials at 60 ℃, 100 ℃, 190 ℃, 190 ℃, 190 ℃, 190 ℃, 200 ℃, 210 ℃ and 170 ℃ and at the screw rotating speed of 250 revolutions per minute.
Comparative example 5
95.2% POE resin (density 0.870 g/cm) -3 After the melt index is 5g/10 min), 3.0% GMA, 1.5% styrene and 0.3% dicumyl peroxide (DCP, the melting point is 42 ℃) are uniformly mixed in a high-speed mixer, the mixture is added into a double-screw extruder through a feeding hopper for reactive extrusion, the length-diameter ratio L/D =36 of the double-screw extruder is used, and the extrusion temperatures of the first section to the ninth section are respectively as follows: the E-POE-14 can be obtained by melting, plasticizing, extruding, drying and granulating the materials at 60 ℃, 100 ℃, 190 ℃, 190 ℃, 190 ℃, 200 ℃, 210 ℃, 170 ℃ and the screw rotating speed of 250 revolutions per minute.
Method for testing various performances
(1) Test of graft ratio
Adding the obtained epoxidized ethylene-octene copolymer composition (hereinafter referred to as E-POE) into toluene, dissolving, heating and refluxing for 30min, then precipitating and washing with acetone, repeating the operation for 3 times, and finally drying to obtain the purified E-POE.
Weighing purified E-POE, adding the E-POE into dimethylbenzene, dropwise adding 1.00G of trichloroacetic acid-dimethylbenzene solution, heating to 120-130 ℃, refluxing for 30min until the polymer is completely dissolved, adding two drops of 10G/L phenolphthalein ethanol solution, maintaining the system at 80-100 ℃, titrating to the phenolphthalein end point by using potassium hydroxide/ethanol solution with certain concentration, simultaneously carrying out blank test, and calculating the grafting rate G (%):
Figure DEST_PATH_IMAGE001
(1-1)
in the formula, V 0 Titration of the volume of potassium hydroxide/ethanol solution consumed without grafting of POE, mL;
v-volume of potassium hydroxide/ethanol solution consumed in E-POE titration, mL;
c-the quantity concentration of potassium hydroxide substance, mol/L;
m-mass of graft, g;
relative molecular mass of the M-epoxy group-containing graft monomer, g/mol.
(2) Mechanical Property test
The notched impact strength of the cantilever beam is tested according to ISO 180-93;
the flexural properties were tested according to ISO 178-93.
(3) Melt index test
Epoxidized ethylene-octene copolymer: melt index was measured according to ASTM D1238 at 190 ℃ and a weight of 2.16 kg.
PBT flame-retardant reinforced material: melt index was measured according to ASTM D1238 at 250 ℃ and a weight of 2.16 kg.
(4) Degree of crosslinking test
The melt index of POE and E-POE before and after grafting were measured, respectively, and the degree of crosslinking C (%) was calculated using the formula (1-2):
Figure 138531DEST_PATH_IMAGE002
(1-2)
wherein w is the melt index of the ungrafted POE, and g/10 min;
and q is the melt index of the grafted E-POE, g/10 min.
The preparation method of the flame-retardant reinforced material comprises the following steps:
the E-POE obtained in comparative examples 1-5 and examples 1-9 was used as a toughening agent in the preparation of PBT flame-retardant reinforced material containing 30% glass fiber and 15% aluminum diethylhypophosphite flame retardant. The PBT flame-retardant reinforced material comprises 30 parts of glass fiber, 50 parts of PBT (grade 1100-211M), 15 parts of diethyl aluminum hypophosphite flame retardant and 5 parts of toughening agent. And drying the PBT in an oven at 120 ℃ for 4 hours for later use. Uniformly mixing all materials, adding the materials into a feeding port of a double-screw extruder, extruding and granulating, feeding glass fibers in a side feeding mode, feeding extruded strips into a granulator for granulation after water cooling and blow drying through a water tank to obtain a PBT flame-retardant reinforced material, drying the obtained plastic particles for 4 hours at 120 ℃, adding the plastic particles into a hopper of an injection molding machine, setting a corresponding injection molding process, and performing injection molding and film pressing to obtain a standard sample strip for testing.
Table 1: results of various performance tests of examples and comparative examples
Figure DEST_PATH_IMAGE003
Table 2 results of performance tests of examples and comparative examples
Figure 383567DEST_PATH_IMAGE004
From the example 1 and the example 2, it can be seen that the initiator with the melting point lower than 10 ℃ can improve the grafting ratio and reduce the crosslinking degree, and the prepared epoxidized ethylene-octene copolymer composition has good toughening effect.
As can be seen from example 1/2 and comparative examples 1 to 5, the degree of crosslinking/grafting was lower when a certain amount of talc was added during the reaction. The crosslinking degree/grafting ratio of the obtained product is high by using other inorganic fillers or crosslinking inhibiting agents.
It can be seen from examples 3 and 1 that the particle size of talc affects the progress of the grafting reaction and the crosslinking reaction, and the effect of increasing the grafting ratio and decreasing the degree of crosslinking is reduced when the particle size exceeds D90=15 μm.

Claims (6)

1. An ethylene oxide-octene copolymer composition is characterized by comprising, by weight, 0.2% -10.0% of styrene monomers, 0.5% -10.0% of glycidyl methacrylate monomers and/or glycidyl methacrylate derivative monomers, 70.0% -99.0% of ethylene-octene copolymers and 0.2% -10.0% of talcum powder;
the epoxidized ethylene-octene copolymer composition further comprises an initiator having a melting point of less than 10 ℃;
the particle size of the talcum powder is D90=2-15 microns.
2. The epoxidized ethylene-octene copolymer composition according to claim 1, wherein said initiator having a melting point lower than 10 ℃ is selected from at least one of the group consisting of tert-amyl peroxyacetate, tert-amyl peroxybenzoate, 2-di (tert-butylperoxy) butane, tert-butyl peroxyisopropylcarbonate, tert-butyl peroxybenzoate, di-tert-amyl peroxide, 2, 5-di-tert-butylperoxy-2, 5-dimethylhexane, tert-butyl cumyl peroxide, di-tert-butyl peroxide, dicumyl hydroperoxide, 1,3, 3-tetramethylbutyl hydroperoxide.
3. The epoxidized ethylene-octene copolymer composition according to claim 1, wherein said ethylene-octene copolymer has a density of 0.860 to 0.880 g/cm -3 And a melt index of 0.5 to 18g/10min (190 ℃, 2.16 kg).
4. The epoxidized ethylene-octene copolymer composition according to claim 1, wherein said glycidyl methacrylate derivative monomer is selected from at least one of allyl glycidyl ether or its derivatives.
5. The epoxidized ethylene-octene copolymer composition according to claim 1, wherein said styrenic monomer is selected from at least one of styrene, α -methylstyrene, α -ethylstyrene and derivatives thereof.
6. The method for producing an epoxidized ethylene-octene copolymer composition according to claim 1, characterized by comprising the steps of: uniformly mixing a styrene monomer, a glycidyl methacrylate monomer and/or a glycidyl methacrylate derivative monomer, an ethylene-octene copolymer, talcum powder and an initiator, and then putting the mixture into a screw extruder for melting plasticization, extrusion, drying and grain cutting to obtain an epoxidized ethylene-octene copolymer composition; wherein the length-diameter ratio L/D of the screw extruder is = 30-60, the rotating speed is 150-500 rpm, and the temperature of each section of screw is 60-215 ℃.
CN201910330534.3A 2019-04-23 2019-04-23 Ethylene oxide-octene copolymer composition and preparation method thereof Active CN111825802B (en)

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