CN114591575A - Preparation method of weather-resistant poly (4-methyl-1-pentene) composite material - Google Patents
Preparation method of weather-resistant poly (4-methyl-1-pentene) composite material Download PDFInfo
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Abstract
The invention relates to the technical field of polymer materials, in particular to a preparation method of a weather-resistant poly (4-methyl-1-pentene) composite material.
Description
Technical Field
The invention relates to the technical field of polymer materials, in particular to a preparation method of a weather-resistant poly (4-methyl-1-pentene) composite material.
Background
The poly-4-methyl-1-pentene (PMP) is a novel thermoplastic plastic with an isotactic structure, compared with a common olefin material, the PMP has excellent high-temperature resistance, electrical property and mechanical property, so that the PMP has wide application in the fields of electric appliance lighting equipment, thin film materials and composite materials, the PMP has mechanical property different from that of high temperature at room temperature or below, the property of the PMP is similar to that of PP at normal temperature, but the flexibility is slightly poor; at high temperatures, PMP exhibits better flexibility, elongation at break and impact strength. PMP is the same as other olefin polymers, the weatherability of PMP is general, it is easy to age, in the course of processing, storing and using, because of receiving external factors such as light, heat, oxygen, water, radiation, etc., especially in the ultraviolet band with higher energy, it can make the macromolecular chain of polymer break to produce free radical, under the participation of oxygen, it can make a series of oxidation, degradation and cross-linking reactions, so that the color change of polymer, the physical and mechanical properties can be gradually reduced, and the use value can be lost. PMP polymer aging is largely divided into photo-oxidative aging and thermo-oxidative aging, with photo-oxidative aging being the major factor affecting its performance. The addition of uv resistant adjuvants to PMP polymers is an effective way to do so. At present, the commonly used anti-ultraviolet auxiliary agents mainly comprise four types of ultraviolet absorbers, excited state quenchers, ultraviolet screeners and hindered amine light stabilizers.
The traditional method for preparing the weather-resistant PMP composite material is generally to uniformly mix an anti-ultraviolet auxiliary agent, an antioxidant, a filler and the like with a base material and then extrude the mixture for granulation through an extruder.
Disclosure of Invention
In order to solve the problems, the invention provides a preparation method of a weather-resistant poly-4-methyl-1-pentene composite material, which improves the compatibility of a modified ultraviolet light shielding agent and PMP by modifying an anti-ultraviolet auxiliary agent, reduces the accumulation of inorganic particles, improves the surface tension of the obtained PMP composite material, and greatly improves the weather resistance.
The technical scheme adopted by the invention is as follows:
a preparation method of weather-resistant poly-4-methyl-1-pentene composite material comprises the following preparation steps:
s1, carrying out surface modification on the inorganic ultraviolet light shielding agent by adopting an organosilane coupling agent to obtain a silane-modified ultraviolet light shielding agent;
s2, carrying out free radical polymerization reaction on a C ═ C double bond on the surface of organosilane and a fluorine-containing monomer to obtain a fluorinated modified ultraviolet light shielding agent;
s3, uniformly mixing the poly-4-methyl-1-pentene, the fluorinated modified ultraviolet light shielding agent and other auxiliary agents, and extruding and granulating through a double-screw extruder to obtain the PMP composite material.
Further, the specific steps in S1 are as follows:
adding 80-120ml of toluene solution and 3-7g of inorganic ultraviolet light shielding agent into a reaction container, then ultrasonically dispersing for 10-30min, pouring the mixture into the reaction container after dispersion is finished, placing the reaction container into an oil bath kettle at 60-80 ℃, magnetically stirring for 10-20min, vacuumizing, introducing nitrogen for 3-5 times repeatedly, adding 0-10 wt% of silane coupling agent, immediately adding 0.3-0.5g of triethylamine, condensing and refluxing, reacting for 1-3h, then pouring the solution into a centrifuge tube, centrifuging for 8-12min at the centrifugal speed of 5500-6500r/min, then washing with absolute ethyl alcohol to remove the excessive silane coupling agent, and finally placing the precipitate in an oven for drying to obtain the silane-modified ultraviolet light shielding agent.
Further, the specific steps in S2 are as follows:
adding 3-5g of silane modified ultraviolet light shielding agent into a reaction vessel, then adding 100-150ml of toluene under the protection of nitrogen, stirring for 10-30min, adding 1-2.5g of fluorine-containing monomer, then transferring the fluorine-containing monomer into an oil bath kettle at 70-90 ℃, dissolving 0-3 wt% of free radical initiator in 15-30ml of toluene, transferring the initiator into a separating funnel after the initiator is completely dissolved, slowly dropwise adding the initiator into the solution, continuing to react for 3-5h after the dropwise adding is finished, and centrifuging, washing and drying after the reaction is finished to obtain the fluorinated modified ultraviolet light shielding agent.
Further, the specific steps in S3 are as follows:
according to the weight portion, 85-95 portions of PMP, 0.3-0.5 portion of antioxidant, 0.1-0.3 portion of ultraviolet absorbent, 0.1-0.3 portion of free radical trapping agent and 1-5 portions of fluorinated and modified ultraviolet shielding agent are uniformly mixed and then put into a charging barrel, and a double-screw extruder is utilized to perform extrusion, water cooling, air drying, grain cutting and drying, so as to obtain the PMP composite material.
Further, the silane coupling agent described in S1 is one or more of vinylmethyldimethoxysilane, vinyldimethylmethoxysilane, 3-methacryloxypropyltrimethoxysilane, 3-aminopropyltriethoxysilane, and γ -glycidoxypropyltrimethoxysilane.
Further, the inorganic ultraviolet light-shielding agent described in S1 is zinc oxide and/or titanium dioxide.
Further, the fluorine-containing monomer described in S2 is dodecafluoroheptyl methacrylate and/or trifluoroethyl methacrylate.
Further, the radical initiator described in S2 is azobisisobutyronitrile and/or benzoyl peroxide.
Further, the antioxidant in S3 is one or more of antioxidant 1010, antioxidant 168 and antioxidant 626; the ultraviolet light absorber is UV531 and/or UV 326; the free radical trapping agent is UV770 and/or UV 622.
Further, in S3, the temperature of the feeding section of the twin-screw extruder was 180 ℃, the temperature of the compression section was 240 ℃, the temperature of the homogenization section was 240 ℃, and the screw rotation speed was 400 rpm.
The invention has the following beneficial effects:
according to the preparation method, the ultraviolet light shielding agent is modified by using the organic siloxane, the fluorine-containing monomer is grafted by using a free radical copolymerization method to prepare the fluorinated modified ultraviolet light shielding agent, and then the fluorinated modified ultraviolet light shielding agent is mixed with PMP and other auxiliaries and extruded to prepare the composite material, the compatibility of the modified ultraviolet light shielding agent and PMP is increased, and the accumulation of inorganic particles is reduced, so that the surface tension of the prepared PMP composite material is improved, the weather resistance of the composite material is greatly improved, and the composite material also has excellent ageing resistance in a humidity environment.
Drawings
FIG. 1 is a flow chart of the preparation in examples 1 to 5 of the present invention.
Detailed Description
In order that the invention may be more readily understood, reference will now be made to the following more particular description of the invention, examples of which are set forth below. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. These embodiments are provided so that this disclosure will be thorough and complete. The various starting materials used in the examples are, unless otherwise indicated, conventional commercial products.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
The numerical values set forth in the examples of the present invention are approximations, not necessarily values. All values within the error range may be included without limiting to the specific values disclosed in the embodiments of the present invention, where the error or experimental conditions allow.
The numerical ranges disclosed in the examples of the present invention are intended to indicate the relative amounts of the components in the mixture and the ranges of temperatures or other parameters recited in the other method examples.
It should be noted here that the "total mass of material" referred to in this application is the sum of the masses of the materials in the whole system.
The following are specific examples of the present application
Example 1:
s1, adding 100ml of toluene solution and 5g of titanium dioxide into a 250ml beaker, ultrasonically dispersing for 20min, pouring the mixture into a 250ml three-neck flask after dispersion is finished, then placing the three-neck flask in an oil bath kettle at 70 ℃, magnetically stirring for 10min, vacuumizing, introducing nitrogen for three times repeatedly, then adding 5 wt% of vinylmethyldimethoxysilane, then immediately adding 0.5g of triethylamine, condensing and refluxing, after reaction for 3h, pouring the solution into a centrifugal tube, centrifuging at the centrifugal speed of 6000r/min for 10min, then washing with absolute ethyl alcohol for three times, removing excessive silane coupling agent, and finally drying the precipitate in an oven at 80 ℃ for 12h to obtain titanium dioxide modified by silane;
s2, adding 5g of silane modified titanium dioxide into a 250ml three-neck flask, then adding 100ml of toluene under the protection of nitrogen, stirring for 20min, adding 2g of trifluoroethyl methacrylate, then transferring the obtained product into an 80 ℃ oil bath kettle, dissolving 1 wt% of benzoyl peroxide into 20ml of toluene, after an initiator is completely dissolved, transferring the obtained product into a separating funnel, slowly dropwise adding the obtained product into the solution, continuing to react for 5h after the dropwise adding is finished, and after the reaction is finished, centrifuging, washing and drying to obtain fluorinated modified titanium dioxide;
s3, uniformly mixing 90 parts of PMP, 0.3 part of antioxidant 1010, 0.2 part of antioxidant 168, 0.2 part of ultraviolet light absorber UV326, 0.2 part of free radical scavenger UV770 and 3 parts of fluorinated modified titanium dioxide, putting the mixture into a charging barrel, and extruding, water cooling, air drying, granulating and drying by using a double-screw extruder, wherein the temperatures of a charging section, a compression section and a homogenization section of the double-screw extruder are respectively 180 ℃/240 ℃/240 ℃, and the rotating speed of a screw is 400rpm, so as to obtain the PMP composite material.
Example 2:
s1, adding 100ml of toluene solution and 5g of titanium dioxide into a 250ml beaker, then ultrasonically dispersing for 30min, pouring the mixture into a 250ml three-neck flask after the dispersion is finished, then placing the three-neck flask in an oil bath kettle at 80 ℃, magnetically stirring for 10min, vacuumizing, introducing nitrogen for three times, then adding 5 wt% of 3-methacryloxypropyl trimethoxy silane, then immediately adding 0.5g of triethylamine, condensing and refluxing, after reacting for 3h, pouring the solution into the flask, centrifuging for 10min at the centrifugal speed of 6000r/min, then washing the centrifuge tube for three times by using absolute ethyl alcohol to remove excessive silane coupling agent, and finally drying the precipitate in an oven at 80 ℃ for 12h to obtain silane modified titanium dioxide;
s2, adding 5g of silane modified titanium dioxide into a 250ml three-neck flask, then adding 150ml of toluene under the protection of nitrogen, stirring for 30min, adding 2.5g of dodecafluoroheptyl methacrylate, then transferring the dodecafluoroheptyl methacrylate into an oil bath kettle at 80 ℃, dissolving 2 wt% of azobisisobutyronitrile into 20ml of toluene, transferring the azodiisobutyronitrile into a separating funnel after an initiator is completely dissolved, slowly dropwise adding the azodiisobutyronitrile into the solution, continuing to react for 5h after the dropwise adding is finished, and after the reaction is finished, centrifuging, washing and drying to obtain fluorinated modified titanium dioxide;
s3, uniformly mixing 90 parts by weight of PMP, 0.3 part by weight of antioxidant 1010, 0.2 part by weight of antioxidant 168, 0.1 part by weight of UV531, 0.1 part by weight of UV326 ultraviolet light absorber, 0.2 part by weight of free radical scavenger UV770 and 5 parts by weight of fluorinated modified titanium dioxide, putting the mixture into a charging barrel, extruding, water cooling, air drying, granulating and drying by using a double-screw extruder, wherein the temperatures of a charging section, a compression section and a homogenization section of the double-screw extruder are respectively 180 ℃/240 ℃/240 ℃, and the screw rotating speed is 400rpm, so as to obtain the PMP composite material.
Example 3:
s1, adding 100ml of toluene solution and 5g of zinc oxide into a 250ml beaker, ultrasonically dispersing for 10min, pouring the mixture into a 250ml three-neck flask after dispersion is finished, then placing the three-neck flask in an oil bath kettle at 60 ℃, magnetically stirring for 20min, vacuumizing, introducing nitrogen for three times repeatedly, then adding 10 wt% of gamma-glycidoxypropyltrimethoxysilane, immediately adding 0.4g of triethylamine, condensing and refluxing, after reaction for 2h, pouring the solution into a centrifugal tube, centrifuging for 10min at the centrifugal speed of 6000r/min, then washing for three times with absolute ethyl alcohol to remove excessive silane coupling agent, and finally drying the precipitate in an oven at 80 ℃ for 10h to obtain silane modified zinc oxide;
s2, adding 3g of silane modified zinc oxide into a 250ml three-neck flask, then adding 125ml of toluene under the protection of nitrogen, stirring for 10min, adding 1g of trifluoroethyl methacrylate, then transferring the obtained product into a 70 ℃ oil bath kettle, dissolving 2 wt% of benzoyl peroxide into 15ml of toluene, after an initiator is completely dissolved, transferring the obtained product into a separating funnel, slowly dropwise adding the obtained product into the solution, continuing to react for 3h after the dropwise adding is finished, and after the reaction is finished, centrifuging, washing and drying to obtain fluorinated modified zinc oxide;
s3, uniformly mixing 90 parts by weight of PMP, 0.3 part by weight of antioxidant 1010, 0.1 part by weight of ultraviolet absorber UV531, 0.2 part by weight of free radical scavenger UV622 and 3 parts by weight of fluorinated and modified zinc oxide, putting the mixture into a charging barrel, and extruding, water cooling, air drying, granulating and drying by using a double-screw extruder, wherein the temperatures of a charging section, a compression section and a homogenization section of the double-screw extruder are respectively 180 ℃/240 ℃/240 ℃, and the rotating speed of a screw is 400rpm, so as to obtain the PMP composite material.
Example 4:
s1, adding 100ml of toluene solution and 5g of titanium dioxide into a 250ml beaker, ultrasonically dispersing for 30min, pouring the mixture into a 250ml three-neck flask after dispersion is finished, then placing the flask in an oil bath kettle at 80 ℃, magnetically stirring for 10-20min, vacuumizing, introducing nitrogen for three times repeatedly, then adding 5 wt% of 3-aminopropyltriethoxysilane, immediately adding 0.3g of triethylamine, condensing and refluxing, after reaction for 3h, pouring the solution into a centrifuge tube, centrifuging for 10min at the centrifugal speed of 6000r/min, then washing for three times by using absolute ethyl alcohol to remove excessive silane coupling agent, and finally drying the precipitate in an oven at 80 ℃ for 12h to obtain silane modified titanium dioxide;
s2, adding 5g of silane-modified ultraviolet light shielding agent into a 250ml three-neck flask, then adding 150ml of toluene under the protection of nitrogen, stirring for 20min, adding 2.5g of trifluoroethyl methacrylate, then transferring the mixture into a 90 ℃ oil bath kettle, dissolving 3 wt% of azobisisobutyronitrile into 30ml of toluene, transferring the initiator into a separating funnel after the initiator is completely dissolved, slowly dropwise adding the initiator into the solution, continuing to react for 4h after the dropwise adding is finished, and after the reaction is finished, centrifuging, washing and drying to obtain fluorinated modified titanium dioxide;
s3, uniformly mixing 85 parts of PMP, 0.2 part of antioxidant 1010, 0.1 part of antioxidant 168, 0.1 part of ultraviolet light absorber UV326, 0.1 part of free radical scavenger UV622 and 5 parts of fluorinated modified titanium dioxide, putting the mixture into a charging barrel, and extruding, water cooling, air drying, granulating and drying by using a double-screw extruder, wherein the temperatures of a charging section, a compression section and a homogenization section of the double-screw extruder are respectively 180 ℃/240 ℃/240 ℃, and the rotating speed of a screw is 400rpm, so as to obtain the PMP composite material.
Example 5:
s1, adding 100ml of toluene solution and 5g of zinc oxide into a 250ml beaker, ultrasonically dispersing for 30min, pouring the mixture into a 250ml three-neck flask after dispersion is finished, then placing the three-neck flask in an oil bath kettle at 80 ℃, magnetically stirring for 10min, vacuumizing, introducing nitrogen for three times repeatedly, then adding 10 wt% of vinyl dimethyl methoxysilane, then immediately adding 0.5g of triethylamine, condensing and refluxing, after reaction for 2h, pouring the solution into a centrifuge tube, centrifuging for 10min at 6000r/min, then washing for three times with absolute ethyl alcohol to remove excessive silane coupling agent, and finally drying the precipitate in an oven at 80 ℃ for 8h to obtain the silane-modified ultraviolet light shielding agent;
s2, adding 5g of silane modified zinc oxide into a 250ml three-neck flask, then adding 120ml of toluene under the protection of nitrogen, stirring for 30min, adding 2.5g of dodecafluoroheptyl methacrylate, then transferring the dodecafluoroheptyl methacrylate into an oil bath kettle at 80 ℃, dissolving 1.5 wt% of azobisisobutyronitrile into 20ml of toluene, transferring the initiator into a separating funnel after the initiator is completely dissolved, slowly dropwise adding the initiator into the solution, continuing to react for 5h after the dropwise adding is finished, and centrifuging, washing and drying after the reaction is finished to obtain the fluorinated modified zinc oxide;
s3, uniformly mixing 95 parts of PMP, 0.3 part of antioxidant 1010, 0.2 part of ultraviolet light absorber UV531, 0.3 part of free radical scavenger UV770 and 5 parts of fluorinated modified zinc oxide, putting the mixture into a charging barrel, and extruding, water cooling, air drying, granulating and drying by using a double-screw extruder, wherein the temperatures of a charging section, a compression section and a homogenization section of the double-screw extruder are respectively 180 ℃/240 ℃/240 ℃, and the rotating speed of a screw is 400rpm, so as to obtain the PMP composite material.
PMP composite materials prepared in examples 1 to 5 were dried in an oven at 80 ℃ for 8 hours in vacuum, respectively, and then injection-molded into standard sample strips by an injection molding machine, and then subjected to accelerated aging in a xenon lamp aging box, and the retention of elongation and impact after aging was measured, and the test results are shown in the following table:
as can be seen from the above table, according to the preparation method provided by the present invention, the prepared PMP composite material has significantly improved weather resistance, and can better meet application requirements, and specifically, according to the preparation method of the present invention, the ultraviolet light shielding agent is modified by using the organosiloxane, the fluorine-containing monomer is grafted by using the radical copolymerization method to prepare the fluorinated modified ultraviolet light shielding agent, and then the fluorinated modified ultraviolet light shielding agent is mixed with PMP and other additives to extrude the mixture to prepare the composite material.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is specific and detailed, but not to be understood as limiting the scope of the present invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (10)
1. A preparation method of a weather-resistant poly (4-methyl-1-pentene) composite material is characterized by comprising the following preparation steps:
s1, carrying out surface modification on the inorganic ultraviolet light shielding agent by adopting an organosilane coupling agent to obtain a silane-modified ultraviolet light shielding agent;
s2, carrying out free radical polymerization reaction on a C ═ C double bond on the surface of organosilane and a fluorine-containing monomer to obtain a fluorinated modified ultraviolet light shielding agent;
s3, uniformly mixing the poly-4-methyl-1-pentene, the fluorinated modified ultraviolet light shielding agent and other auxiliary agents, and extruding and granulating through a double-screw extruder to obtain the PMP composite material.
2. The method for preparing the weather-resistant poly-4-methyl-1-pentene composite material according to claim 1, wherein the specific steps in S1 are as follows:
adding 80-120ml of toluene solution and 3-7g of inorganic ultraviolet light shielding agent into a reaction container, then ultrasonically dispersing for 10-30min, pouring the mixture into the reaction container after dispersion is finished, placing the reaction container into an oil bath kettle at 60-80 ℃, magnetically stirring for 10-20min, vacuumizing, introducing nitrogen for 3-5 times repeatedly, adding 0-10 wt% of silane coupling agent, immediately adding 0.3-0.5g of triethylamine, condensing and refluxing, reacting for 1-3h, then pouring the solution into a centrifuge tube, centrifuging for 8-12min at the centrifugal speed of 5500-6500r/min, then washing with absolute ethyl alcohol to remove the excessive silane coupling agent, and finally placing the precipitate in an oven for drying to obtain the silane-modified ultraviolet light shielding agent.
3. The method for preparing the weather-resistant poly-4-methyl-1-pentene composite material according to claim 1, wherein the specific steps in S2 are as follows:
adding 3-5g of silane modified ultraviolet light shielding agent into a reaction vessel, then adding 100-150ml of toluene under the protection of nitrogen, stirring for 10-30min, adding 1-2.5g of fluorine-containing monomer, then transferring the fluorine-containing monomer into an oil bath kettle at 70-90 ℃, dissolving 0-3 wt% of free radical initiator in 15-30ml of toluene, transferring the initiator into a separating funnel after the initiator is completely dissolved, slowly dropwise adding the initiator into the solution, continuing to react for 3-5h after the dropwise adding is finished, and centrifuging, washing and drying after the reaction is finished to obtain the fluorinated modified ultraviolet light shielding agent.
4. The method for preparing the weather-resistant poly-4-methyl-1-pentene composite material according to claim 1, wherein the specific steps in S3 are as follows:
according to the weight portion, 85-95 portions of PMP, 0.3-0.5 portion of antioxidant, 0.1-0.3 portion of ultraviolet absorbent, 0.1-0.3 portion of free radical trapping agent and 1-5 portions of fluorinated and modified ultraviolet shielding agent are uniformly mixed and then put into a charging barrel, and a double-screw extruder is utilized to perform extrusion, water cooling, air drying, grain cutting and drying, so as to obtain the PMP composite material.
5. The method for preparing the weather-resistant poly-4-methyl-1-pentene composite material as claimed in claim 1, wherein the silane coupling agent in S1 is one or more selected from vinylmethyldimethoxysilane, vinyldimethylmethoxysilane, 3-methacryloxypropyltrimethoxysilane, 3-aminopropyltriethoxysilane and gamma-glycidoxypropyltrimethoxysilane.
6. The method for preparing a weather-resistant poly-4-methyl-1-pentene composite material according to claim 1, wherein the inorganic ultraviolet light-shielding agent in S1 is zinc oxide and/or titanium dioxide.
7. The method for preparing the weather-resistant poly-4-methyl-1-pentene composite material as claimed in claim 1, wherein the fluorine-containing monomer in S2 is dodecafluoroheptyl methacrylate and/or trifluoroethyl methacrylate.
8. The method of claim 1, wherein the radical initiator of S2 is azobisisobutyronitrile and/or benzoyl peroxide.
9. The method for preparing the weather-resistant poly-4-methyl-1-pentene composite material as claimed in claim 1, wherein the antioxidant in S3 is one or more of antioxidant 1010, antioxidant 168 and antioxidant 626; the ultraviolet light absorber is UV531 and/or UV 326; the free radical trapping agent is UV770 and/or UV 622.
10. The method for preparing weather-resistant poly-4-methyl-1-pentene composite material according to claim 4, wherein the temperature of the feeding section of the twin-screw extruder in S3 is 180 ℃, the temperature of the compression section is 240 ℃, the temperature of the homogenization section is 240 ℃, and the screw rotation speed is 400 rpm.
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| CN108467532A (en) * | 2018-04-16 | 2018-08-31 | 常州中英科技股份有限公司 | A kind of polyolefin-based antenna house of thermoplastics type's saturation of high wave transmission rate |
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| CN103387645A (en) * | 2013-07-12 | 2013-11-13 | 南京理工大学 | Fluorine-containing copolymer grafted modified nano TiO2 compound particle and preparation method thereof |
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