CN110698829B - Low-temperature-resistant high-toughness composite material - Google Patents
Low-temperature-resistant high-toughness composite material Download PDFInfo
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Abstract
The invention relates to the field of high polymer materials, and discloses a low-temperature-resistant high-toughness composite material and a preparation method thereof, wherein the composite material comprises the following components in parts by weight: 82-94 parts of polycarbonate, 2-6 parts of cold-resistant auxiliary agent, 8-12 parts of toughening agent, 18-26 parts of modified nano clay, 0.4-1.6 parts of antioxidant, 5-12 parts of epoxy resin and 0.5-1.5 parts of curing agent. The preparation method comprises the following steps: sequentially adding the components in parts by weight into a high-speed mixer, and uniformly mixing to obtain a mixed material; putting the mixed material into a double-screw extruder for melt extrusion granulation to obtain granules, wherein the processing temperature is 230-260 ℃, and the rotating speed of a main screw of the double-screw extruder is 700-800 r/min; drying the granules at 100 ℃ for 12h, and carrying out injection molding on the granules by using an injection molding machine to obtain the low-temperature-resistant high-toughness composite material, wherein the injection molding temperature is 230-260 ℃. The low-temperature-resistant high-toughness composite material has high low-temperature toughness retention rate and excellent low-temperature impact performance, and can be suitable for being used in low-temperature extreme environments.
Description
Technical Field
The invention relates to the field of high polymer materials, in particular to a low-temperature-resistant high-toughness composite material.
Background
The polycarbonate is a high-performance engineering plastic, has excellent mechanical properties and good heat resistance, optical and electrical properties, and has important application in the fields of building material industry, automobile manufacturing industry, aerospace and the like. Although the polycarbonate has extremely high impact toughness at room temperature, the toughness is sensitive to temperature, the mechanical property is obviously reduced at low temperature, and the polycarbonate undergoes brittle-tough transition at about 0 ℃, so that the low-temperature toughness of the polycarbonate is still difficult to meet the requirement in certain applications, and the polycarbonate has great limitation in use in low-temperature environments. In order to ensure sufficient toughness of the annealed article and to improve the low temperature impact toughness, some additives are added to improve the properties of the polycarbonate so that the polycarbonate can be used in more occasions. There are two main methods for modifying polycarbonates, namely physical blending and graft modification. In order to improve the low-temperature toughness and processability of polycarbonates, it is more common to incorporate a certain amount of an auxiliary agent into the polycarbonate, which is simple but generally effective. Therefore, it is necessary to develop a method for improving the low temperature toughness of polycarbonate, which is simple in preparation method but has a good toughening effect.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention provides a low-temperature-resistant high-toughness composite material which has high low-temperature toughness retention rate and excellent low-temperature impact performance and can be suitable for being used in a low-temperature extreme environment.
The invention discloses a low-temperature-resistant high-toughness composite material which comprises the following components in parts by weight:
82-94 parts of polycarbonate,
2-6 parts of cold-resistant auxiliary agent,
8-12 parts of toughening agent,
18-26 parts of modified nano clay,
0.4 to 1.6 parts of antioxidant,
5-12 parts of epoxy resin,
0.5-1.5 parts of curing agent.
Preferably, the toughening agent is a mixture of methyl methacrylate-butadiene-styrene copolymer, ethylene propylene diene monomer and methyl methacrylate.
Preferably, the toughening agent is formed by mixing methyl methacrylate-butadiene-styrene copolymer, ethylene propylene diene monomer rubber and methyl methacrylate according to the mass ratio of 3:1.7: 2.6.
Preferably, the cold-resistant auxiliary agent is any one of diethylene glycol monobutyl ether adipate, nylon dioctyl ester and dibutyl phthalate.
Preferably, the preparation method of the modified nanoclay includes the steps of:
2.2-4.6 parts of epoxy resin, 0.4-0.8 part of p-aminobenzoic acid and 20-30 parts of solvent are placed in a stirrer to be stirred and dissolved, then 1.3-1.9 parts of nano-clay is added, and the mixture is stirred until the nano-clay is uniformly dispersed to obtain a mixed solution;
and transferring the mixed solution into a reactor with a condensation reflux device, setting the temperature at 100-110 ℃, stirring at a speed of 400-500 r/min, reacting for 2-5 h, taking out, cooling, performing suction filtration, and drying the particles in an oven to obtain the modified nano clay.
More preferably, the solvent is formed by mixing propylene glycol monomethyl ether propionate and absolute ethyl alcohol according to a volume ratio of 3: 2.
Preferably, the preparation method of the low-temperature-resistant high-toughness composite material comprises the following steps:
according to the weight parts, 82-94 parts of polycarbonate, 2-6 parts of cold-resistant auxiliary agent, 8-12 parts of toughening agent, 18-26 parts of modified nano clay, 0.4-1.6 parts of antioxidant, 5-12 parts of epoxy resin and 0.5-1.5 parts of curing agent are uniformly mixed in a high-speed mixer to obtain a mixed material;
putting the mixed material into a double-screw extruder for melt extrusion granulation to obtain granules, wherein the processing temperature is 230-260 ℃, and the rotating speed of a main screw of the double-screw extruder is 700-800 r/min;
drying the granules at 100 ℃ for 12h, and carrying out injection molding on the granules by using an injection molding machine to obtain the low-temperature-resistant high-toughness composite material, wherein the injection molding temperature is 230-260 ℃.
The invention has the following beneficial effects: the low-temperature-resistant high-toughness composite material has high low-temperature toughness retention rate and excellent low-temperature impact performance, and can be suitable for being used in low-temperature extreme environments. The epoxy resin is adopted to modify the nano clay to obtain the modified nano clay with epoxy groups as the filler, and the epoxy resin is added into the material. In the mixing process, the epoxy group of the outer layer of the modified nano clay and the epoxy resin dispersed in the polycarbonate are jointly crosslinked with the curing agent, so that the modified nano clay particles dispersed in the polycarbonate are connected through an epoxy resin crosslinking network, thereby achieving the aim of further toughening and improving the performance of the material.
In order to make the aforementioned and other objects, features and advantages of the invention more comprehensible, preferred embodiments accompanied with figures are described in detail below.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. 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.
Example 1
Step one, preparing modified nano clay:
placing 4.6 parts of epoxy resin, 0.4 part of p-aminobenzoic acid and 30 parts of solvent into a stirrer, stirring and dissolving, then adding 1.3 parts of nano clay, and stirring until the nano clay is uniformly dispersed to obtain a mixed solution, wherein the solvent is formed by mixing propylene glycol monomethyl ether propionate and absolute ethyl alcohol according to a volume ratio of 3: 2;
and transferring the mixed solution into a reactor with a condensation reflux device, setting the temperature at 110 ℃, stirring at the rotating speed of 400 r/min, reacting for 5 hours, taking out, cooling, filtering, and drying the particles in an oven to obtain the modified nano clay.
Step two, preparing the low-temperature-resistant high-toughness composite material:
according to the weight parts, 82 parts of polycarbonate, 6 parts of diethylene glycol monobutyl ether adipate, 8 parts of toughening agent, 26 parts of modified nano clay, 0.4 part of hindered phenol antioxidant, 5 parts of epoxy resin and 1.5 parts of polyethylene polyamine are uniformly mixed in a high-speed mixer to obtain a mixed material, wherein the toughening agent is formed by mixing methyl methacrylate-butadiene-styrene copolymer, ethylene propylene diene monomer rubber and methyl methacrylate according to the mass ratio of 3:1.7: 2.6;
putting the mixed material into a double-screw extruder for melt extrusion granulation to obtain granules, wherein the processing temperature is 230 ℃, and the rotating speed of a main screw of the double-screw extruder is 800 r/min;
drying the granules at 100 ℃ for 12h, and carrying out injection molding on the granules by using an injection molding machine to obtain the low-temperature-resistant high-toughness composite material, wherein the injection molding temperature is 230 ℃.
Example 2
Step one, preparing modified nano clay:
placing 2.2 parts of epoxy resin, 0.8 part of p-aminobenzoic acid and 20 parts of solvent into a stirrer, stirring and dissolving, then adding 1.9 parts of nano clay, and stirring until the nano clay is uniformly dispersed to obtain a mixed solution, wherein the solvent is formed by mixing propylene glycol monomethyl ether propionate and absolute ethyl alcohol according to a volume ratio of 3: 2;
and transferring the mixed solution into a reactor with a condensation reflux device, setting the temperature at 100 ℃, stirring at the rotating speed of 500 r/min, reacting for 2 hours, taking out, cooling, filtering, and drying the particles in an oven to obtain the modified nano clay.
Step two, preparing the low-temperature-resistant high-toughness composite material:
according to the weight parts, 94 parts of polycarbonate, 2 parts of diethylene glycol monobutyl ether adipate, 12 parts of toughening agent, 18 parts of modified nano clay, 1.6 parts of hindered phenol antioxidant, 12 parts of epoxy resin and 0.5 part of polyethylene polyamine are uniformly mixed in a high-speed mixer to obtain a mixed material, wherein the toughening agent is formed by mixing methyl methacrylate-butadiene-styrene copolymer, ethylene propylene diene monomer rubber and methyl methacrylate according to the mass ratio of 3:1.7: 2.6;
putting the mixed material into a double-screw extruder for melt extrusion granulation to obtain granules, wherein the processing temperature is 260 ℃, and the main screw rotating speed of the double-screw extruder is 700 r/min;
drying the granules at 100 ℃ for 12h, and carrying out injection molding on the granules by using an injection molding machine to obtain the low-temperature-resistant high-toughness composite material, wherein the injection molding temperature is 260 ℃.
Example 3
Step one, preparing modified nano clay:
placing 3.6 parts of epoxy resin, 0.5 part of p-aminobenzoic acid and 28 parts of solvent into a stirrer, stirring and dissolving, then adding 1.4 parts of nano clay, and stirring until the nano clay is uniformly dispersed to obtain a mixed solution, wherein the solvent is formed by mixing propylene glycol monomethyl ether propionate and absolute ethyl alcohol according to a volume ratio of 3: 2;
and transferring the mixed solution into a reactor with a condensation reflux device, setting the temperature at 107 ℃, stirring at the rotating speed of 420 r/min, reacting for 4 hours, taking out, cooling, filtering, and drying the particles in an oven to obtain the modified nano clay.
Step two, preparing the low-temperature-resistant high-toughness composite material:
according to the weight parts, 86 parts of polycarbonate, 5 parts of nylon dioctyl ester, 9 parts of a toughening agent, 24 parts of modified nano clay, 0.6 part of hindered phenol antioxidant, 7 parts of epoxy resin and 1.2 parts of polyethylene polyamine are uniformly mixed in a high-speed mixer to obtain a mixed material, wherein the toughening agent is formed by mixing methyl methacrylate-butadiene-styrene copolymer, ethylene propylene diene monomer rubber and methyl methacrylate according to the mass ratio of 3:1.7: 2.6;
putting the mixed material into a double-screw extruder for melt extrusion granulation to obtain granules, wherein the processing temperature is 240 ℃, and the main screw rotating speed of the double-screw extruder is 770 r/min;
drying the granules at 100 ℃ for 12h, and carrying out injection molding on the granules by using an injection molding machine to obtain the low-temperature-resistant high-toughness composite material, wherein the injection molding temperature is 240 ℃.
Example 4
Step one, preparing modified nano clay:
3.4 parts of epoxy resin, 0.6 part of p-aminobenzoic acid and 26 parts of solvent are placed in a stirrer to be stirred and dissolved, then 1.55 parts of nano-clay is added, and the mixture is stirred until the nano-clay is uniformly dispersed to obtain a mixed solution, wherein the solvent is formed by mixing propylene glycol monomethyl ether propionate and absolute ethyl alcohol according to the volume ratio of 3: 2;
and transferring the mixed solution into a reactor with a condensation reflux device, setting the temperature at 105 ℃, stirring at the rotating speed of 460 r/min, reacting for 4 hours, taking out, cooling, filtering, and drying the particles in an oven to obtain the modified nano clay.
Step two, preparing the low-temperature-resistant high-toughness composite material:
according to the weight parts, 88 parts of polycarbonate, 4 parts of dibutyl phthalate, 9.5 parts of a toughening agent, 22 parts of modified nano clay, 1 part of a hindered phenol antioxidant, 8 parts of epoxy resin and 0.9 part of polyethylene polyamine are uniformly mixed in a high-speed mixer to obtain a mixed material, wherein the toughening agent is formed by mixing methyl methacrylate-butadiene-styrene copolymer, ethylene propylene diene monomer rubber and methyl methacrylate according to the mass ratio of 3:1.7: 2.6;
putting the mixed material into a double-screw extruder for melt extrusion granulation to obtain granules, wherein the processing temperature is 240 ℃, and the rotating speed of a main screw of the double-screw extruder is 760 r/min;
drying the granules at 100 ℃ for 12h, and carrying out injection molding on the granules by using an injection molding machine to obtain the low-temperature-resistant high-toughness composite material, wherein the injection molding temperature is 245 ℃.
Example 5
Step one, preparing modified nano clay:
placing 3.2 parts of epoxy resin, 0.7 part of p-aminobenzoic acid and 22 parts of solvent into a stirrer, stirring and dissolving, then adding 1.7 parts of nano clay, and stirring until the nano clay is uniformly dispersed to obtain a mixed solution, wherein the solvent is formed by mixing propylene glycol monomethyl ether propionate and absolute ethyl alcohol according to a volume ratio of 3: 2;
and transferring the mixed solution into a reactor with a condensation reflux device, setting the temperature at 103 ℃, stirring at the rotating speed of 480 r/min, reacting for 3h, taking out, cooling, filtering, and drying the particles in an oven to obtain the modified nano clay.
Step two, preparing the low-temperature-resistant high-toughness composite material:
according to the weight parts, 90 parts of polycarbonate, 3 parts of nylon dioctyl ester, 10 parts of toughening agent, 20 parts of modified nano clay, 1.4 parts of hindered phenol antioxidant, 10 parts of epoxy resin and 0.8 part of polyethylene polyamine are uniformly mixed in a high-speed mixer to obtain a mixed material, wherein the toughening agent is formed by mixing methyl methacrylate-butadiene-styrene copolymer, ethylene propylene diene monomer rubber and methyl methacrylate according to the mass ratio of 3:1.7: 2.6;
putting the mixed material into a double-screw extruder for melt extrusion granulation to obtain granules, wherein the processing temperature is 250 ℃, and the main screw rotating speed of the double-screw extruder is 730 r/min;
drying the granules at 100 ℃ for 12h, and carrying out injection molding on the granules by using an injection molding machine to obtain the low-temperature-resistant high-toughness composite material, wherein the injection molding temperature is 250 ℃.
Comparative example 1
This comparative example differs from example 4 in that unmodified nanoclay is used.
According to the weight parts, 88 parts of polycarbonate, 4 parts of dibutyl phthalate, 9.5 parts of a toughening agent, 22 parts of nano clay, 1 part of a hindered phenol antioxidant, 8 parts of epoxy resin and 0.9 part of polyethylene polyamine are uniformly mixed in a high-speed mixer to obtain a mixed material, wherein the toughening agent is formed by mixing methyl methacrylate-butadiene-styrene copolymer, ethylene propylene diene monomer rubber and methyl methacrylate according to the mass ratio of 3:1.7: 2.6;
putting the mixed material into a double-screw extruder for melt extrusion granulation to obtain granules, wherein the processing temperature is 240 ℃, and the rotating speed of a main screw of the double-screw extruder is 760 r/min;
drying the granules at 100 ℃ for 12h, and carrying out injection molding on the granules by using an injection molding machine to obtain the low-temperature-resistant high-toughness composite material, wherein the injection molding temperature is 245 ℃.
Comparative example 2
The comparative example differs from example 4 in the composition of the toughening agent.
Step one, preparing modified nano clay:
3.4 parts of epoxy resin, 0.6 part of p-aminobenzoic acid and 26 parts of solvent are placed in a stirrer to be stirred and dissolved, then 1.55 parts of nano-clay is added, and the mixture is stirred until the nano-clay is uniformly dispersed to obtain a mixed solution, wherein the solvent is formed by mixing propylene glycol monomethyl ether propionate and absolute ethyl alcohol according to the volume ratio of 3: 2;
and transferring the mixed solution into a reactor with a condensation reflux device, setting the temperature at 105 ℃, stirring at the rotating speed of 460 r/min, reacting for 4 hours, taking out, cooling, filtering, and drying the particles in an oven to obtain the modified nano clay.
Step two, preparing the low-temperature-resistant high-toughness composite material:
according to the weight parts, 88 parts of polycarbonate, 4 parts of dibutyl phthalate, 9.5 parts of a toughening agent, 22 parts of modified nano clay, 1 part of a hindered phenol antioxidant, 8 parts of epoxy resin and 0.9 part of polyethylene polyamine are uniformly mixed in a high-speed mixer to obtain a mixed material, wherein the toughening agent is formed by mixing methyl methacrylate-butadiene-styrene copolymer, ethylene propylene diene monomer rubber and methyl methacrylate according to the mass ratio of 2:1.5: 2.1;
putting the mixed material into a double-screw extruder for melt extrusion granulation to obtain granules, wherein the processing temperature is 240 ℃, and the rotating speed of a main screw of the double-screw extruder is 760 r/min;
drying the granules at 100 ℃ for 12h, and carrying out injection molding on the granules by using an injection molding machine to obtain the low-temperature-resistant high-toughness composite material, wherein the injection molding temperature is 245 ℃.
The low temperature resistant high toughness composite materials prepared in examples 1-5 and comparative examples 1-2 were subjected to a performance test, and processed into a sample to be tested using a single polycarbonate according to the preparation method of example 4 of the present invention without adding any additives, and also subjected to a performance test:
impact performance testing was performed in accordance with ASTM D256 in different temperature environments using notched Izod impact mode. The specimen size was 127 mm × 12.7 mm × 3.2 mm, the notch angle was 45 °, the notch depth was 2.5 mm, and the radius of curvature was 0.25 mm.
The results of the material toughness testing are shown in the following table:
according to the test result, the toughness of the low-temperature-resistant high-toughness composite material is gradually reduced along with the reduction of the environmental temperature, but compared with polycarbonate, the low-temperature-resistant high-toughness composite material has higher retention rate of low-temperature toughness, has excellent low-temperature impact performance, and can be suitable for being used in low-temperature extreme environments.
The epoxy resin is adopted to modify the nano clay to obtain the modified nano clay with epoxy groups as the filler, and the epoxy resin is added into the material. In the mixing process, the epoxy group of the outer layer of the modified nano clay and the epoxy resin dispersed in the polycarbonate are jointly crosslinked with the curing agent, so that the modified nano clay particles dispersed in the polycarbonate are connected through an epoxy resin crosslinking network, thereby achieving the aim of further toughening and improving the performance of the material.
The principle and the implementation mode of the invention are explained by applying specific embodiments in the invention, and the description of the embodiments is only used for helping to understand the method and the core idea of the invention; meanwhile, for a person skilled in the art, according to the idea of the present invention, there may be variations in the specific embodiments and the application scope, and in summary, the content of the present specification should not be construed as a limitation to the present invention.
Claims (6)
1. The low-temperature-resistant high-toughness composite material is characterized by comprising the following components in parts by weight:
82-94 parts of polycarbonate,
2-6 parts of cold-resistant auxiliary agent,
8-12 parts of toughening agent,
18-26 parts of modified nano clay,
0.4 to 1.6 parts of antioxidant,
5-12 parts of epoxy resin,
0.5-1.5 parts of a curing agent;
wherein, the preparation method of the modified nano clay comprises the following steps:
2.2-4.6 parts of epoxy resin, 0.4-0.8 part of p-aminobenzoic acid and 20-30 parts of solvent are placed in a stirrer to be stirred and dissolved, then 1.3-1.9 parts of nano-clay is added, and the mixture is stirred until the nano-clay is uniformly dispersed to obtain a mixed solution;
and transferring the mixed solution into a reactor with a condensation reflux device, setting the temperature at 100-110 ℃, stirring at a speed of 400-500 r/min, reacting for 2-5 h, taking out, cooling, performing suction filtration, and drying the particles in an oven to obtain the modified nano clay.
2. The low temperature resistant high toughness composite of claim 1, wherein said toughening agent is a mixture of methylmethacrylate-butadiene-styrene copolymer, ethylene propylene diene monomer and methylmethacrylate.
3. The low-temperature-resistant high-toughness composite material as claimed in claim 1 or 2, wherein the toughening agent is formed by mixing methyl methacrylate-butadiene-styrene copolymer, ethylene propylene diene monomer rubber and methyl methacrylate according to a mass ratio of 3:1.7: 2.6.
4. The low temperature resistant high toughness composite material of claim 1, wherein said cold resistant auxiliary agent is any one of diethylene glycol monobutyl ether adipate, nylon dioctyl ester and dibutyl phthalate.
5. The low-temperature-resistant high-toughness composite material as claimed in claim 1, wherein the solvent is propylene glycol monomethyl ether propionate and absolute ethyl alcohol mixed according to a volume ratio of 3: 2.
6. The low temperature resistant high toughness composite material of claim 1, wherein said preparation method of said low temperature resistant high toughness composite material comprises the following steps:
according to the weight parts, 82-94 parts of polycarbonate, 2-6 parts of cold-resistant auxiliary agent, 8-12 parts of toughening agent, 18-26 parts of modified nano clay, 0.4-1.6 parts of antioxidant, 5-12 parts of epoxy resin and 0.5-1.5 parts of curing agent are uniformly mixed in a high-speed mixer to obtain a mixed material;
putting the mixed material into a double-screw extruder for melt extrusion granulation to obtain granules, wherein the processing temperature is 230-260 ℃, and the rotating speed of a main screw of the double-screw extruder is 700-800 r/min;
drying the granules at 100 ℃ for 12h, and carrying out injection molding on the granules by using an injection molding machine to obtain the low-temperature-resistant high-toughness composite material, wherein the injection molding temperature is 230-260 ℃.
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