CN112920595A - Nano potassium titanate whisker reinforced high-temperature-resistant nylon composite material and preparation method thereof - Google Patents
Nano potassium titanate whisker reinforced high-temperature-resistant nylon composite material and preparation method thereof Download PDFInfo
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- 239000004677 Nylon Substances 0.000 title claims abstract description 115
- 229920001778 nylon Polymers 0.000 title claims abstract description 115
- NJLLQSBAHIKGKF-UHFFFAOYSA-N dipotassium dioxido(oxo)titanium Chemical compound [K+].[K+].[O-][Ti]([O-])=O NJLLQSBAHIKGKF-UHFFFAOYSA-N 0.000 title claims abstract description 107
- 239000002131 composite material Substances 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title abstract description 16
- 239000000203 mixture Substances 0.000 claims abstract description 28
- 239000003963 antioxidant agent Substances 0.000 claims abstract description 23
- 230000003078 antioxidant effect Effects 0.000 claims abstract description 23
- 239000012760 heat stabilizer Substances 0.000 claims abstract description 20
- 238000002156 mixing Methods 0.000 claims abstract description 11
- 239000002994 raw material Substances 0.000 claims abstract description 3
- 238000000034 method Methods 0.000 claims abstract 3
- 229920003189 Nylon 4,6 Polymers 0.000 claims description 31
- 229920006111 poly(hexamethylene terephthalamide) Polymers 0.000 claims description 14
- 238000001035 drying Methods 0.000 claims description 10
- 238000001125 extrusion Methods 0.000 claims description 10
- 229920003023 plastic Polymers 0.000 claims description 9
- 239000004033 plastic Substances 0.000 claims description 9
- HQKMJHAJHXVSDF-UHFFFAOYSA-L magnesium stearate Chemical compound [Mg+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O HQKMJHAJHXVSDF-UHFFFAOYSA-L 0.000 claims description 8
- 239000002245 particle Substances 0.000 claims description 8
- 229920006115 poly(dodecamethylene terephthalamide) Polymers 0.000 claims description 5
- OKOBUGCCXMIKDM-UHFFFAOYSA-N Irganox 1098 Chemical compound CC(C)(C)C1=C(O)C(C(C)(C)C)=CC(CCC(=O)NCCCCCCNC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)=C1 OKOBUGCCXMIKDM-UHFFFAOYSA-N 0.000 claims description 4
- UTGQNNCQYDRXCH-UHFFFAOYSA-N N,N'-diphenyl-1,4-phenylenediamine Chemical compound C=1C=C(NC=2C=CC=CC=2)C=CC=1NC1=CC=CC=C1 UTGQNNCQYDRXCH-UHFFFAOYSA-N 0.000 claims description 4
- 235000019359 magnesium stearate Nutrition 0.000 claims description 4
- 229940114930 potassium stearate Drugs 0.000 claims description 4
- ANBFRLKBEIFNQU-UHFFFAOYSA-M potassium;octadecanoate Chemical compound [K+].CCCCCCCCCCCCCCCCCC([O-])=O ANBFRLKBEIFNQU-UHFFFAOYSA-M 0.000 claims description 4
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical group [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 3
- 239000011701 zinc Substances 0.000 claims description 3
- 229910052725 zinc Inorganic materials 0.000 claims description 3
- DMBHHRLKUKUOEG-UHFFFAOYSA-N N-phenyl aniline Natural products C=1C=CC=CC=1NC1=CC=CC=C1 DMBHHRLKUKUOEG-UHFFFAOYSA-N 0.000 claims description 2
- 239000006185 dispersion Substances 0.000 abstract description 3
- 229920005989 resin Polymers 0.000 abstract description 2
- 239000011347 resin Substances 0.000 abstract description 2
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 12
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 9
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 9
- 238000002441 X-ray diffraction Methods 0.000 description 7
- 238000002329 infrared spectrum Methods 0.000 description 7
- 238000001228 spectrum Methods 0.000 description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 6
- 239000013078 crystal Substances 0.000 description 6
- 238000002425 crystallisation Methods 0.000 description 6
- 230000008025 crystallization Effects 0.000 description 6
- 125000000524 functional group Chemical group 0.000 description 6
- 238000001000 micrograph Methods 0.000 description 6
- 239000011259 mixed solution Substances 0.000 description 6
- 238000012545 processing Methods 0.000 description 6
- 239000002070 nanowire Substances 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- 239000004952 Polyamide Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 229920002647 polyamide Polymers 0.000 description 4
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 description 4
- 238000011160 research Methods 0.000 description 4
- 238000001878 scanning electron micrograph Methods 0.000 description 4
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 3
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 description 3
- 239000004202 carbamide Substances 0.000 description 3
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 230000007935 neutral effect Effects 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 239000002243 precursor Substances 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- MFNFHZVOHDNCDN-UHFFFAOYSA-N 4,6-bis[(2,2,6,6-tetramethylpiperidin-3-yl)amino]benzene-1,3-dicarboxamide Chemical group CC1(NC(CCC1NC1=CC(=C(C=C1C(=O)N)C(=O)N)NC1C(NC(CC1)(C)C)(C)C)(C)C)C MFNFHZVOHDNCDN-UHFFFAOYSA-N 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 229920006351 engineering plastic Polymers 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 229910000027 potassium carbonate Inorganic materials 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- QAPVYZRWKDXNDK-UHFFFAOYSA-N P,P-Dioctyldiphenylamine Chemical compound C1=CC(CCCCCCCC)=CC=C1NC1=CC=C(CCCCCCCC)C=C1 QAPVYZRWKDXNDK-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 125000003368 amide group Chemical group 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000002657 fibrous material Substances 0.000 description 1
- 238000005469 granulation Methods 0.000 description 1
- 230000003179 granulation Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 239000011208 reinforced composite material Substances 0.000 description 1
- 239000002990 reinforced plastic Substances 0.000 description 1
- 239000012744 reinforcing agent Substances 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 229920001169 thermoplastic Polymers 0.000 description 1
- 239000004416 thermosoftening plastic Substances 0.000 description 1
- 239000012745 toughening agent Substances 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/04—Reinforcing macromolecular compounds with loose or coherent fibrous material
- C08J5/06—Reinforcing macromolecular compounds with loose or coherent fibrous material using pretreated fibrous materials
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2377/00—Characterised by the use of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Derivatives of such polymers
- C08J2377/06—Polyamides derived from polyamines and polycarboxylic acids
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/003—Additives being defined by their diameter
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/02—Fibres or whiskers
- C08K7/04—Fibres or whiskers inorganic
- C08K7/08—Oxygen-containing compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
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- Manufacturing & Machinery (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Reinforced Plastic Materials (AREA)
Abstract
The invention discloses a nano potassium titanate whisker reinforced high-temperature-resistant nylon composite material which is prepared from the following raw materials in parts by weight: 45-60 parts of high-temperature nylon, 20-35 parts of modified nano potassium titanate whiskers, 1-5 parts of an antioxidant and 0.5-2 parts of a heat stabilizer. The invention also discloses a method for preparing the nano potassium titanate whisker reinforced high-temperature-resistant nylon composite material, which comprises the following specific steps: 1) uniformly mixing high-temperature nylon, the modified nano potassium titanate whisker, the antioxidant and the heat stabilizer in proportion, and pouring the mixture into a double-screw extruder; 2) and obtaining the nano potassium titanate whisker reinforced high-temperature resistant nylon composite material by a double-screw extruder and a granulator. The nano potassium titanate whisker reinforced high-temperature-resistant nylon composite material obtained by the invention has the advantages of simple preparation process, low cost and high productivity. In addition, the modified nano potassium titanate whisker has good dispersion and good compatibility in nylon resin, so that the nylon composite material has excellent comprehensive performance.
Description
Technical Field
The invention relates to a high-molecular composite material, in particular to a nano potassium titanate whisker reinforced high-temperature-resistant nylon composite material and a preparation method thereof.
Background
Nylon, also known as Polyamide (PA), is a thermoplastic engineering plastic, has been used for a long time in human history, has good temperature resistance, toughness, rigidity and wear resistance due to the presence of repeated amide groups in the molecular chain, is widely applied to industries such as electronics, electricity, construction, machinery, aerospace and the like, and has become the focus of research personnel to replace steel and wood with plastic. Due to excellent performance of nylon, the demand of the nylon in five engineering plastics is in the first place all the time, and the high-temperature nylon has more unique advantages in the high-end application field of nylon, so that the development of the reinforced and toughened high-temperature resistant nylon has very important significance.
In recent years, more and more scientific researches are carried out on whisker reinforced composite materials, the research depth is continuously increased, remarkable results are achieved, and whisker modified polymers become hot spots of modification researches on polymer-based composite materials at present. The crystal whisker is a high-purity acicular fiber material which grows in a single crystal structure form and is small in size under the condition of manual control, has a uniform structure, almost has no defect in the interior, and has strength and modulus close to the theoretical values of crystal materials, so that the crystal whisker is a novel composite material reinforcing and toughening agent with very excellent mechanical properties. Whisker reinforced plastics appear as early as 60 years, but are subject to multiple limitations of factors such as whisker manufacturing technology, cost and the like, and the application of the whiskers in high polymer materials cannot be popularized until cheap nano potassium titanate whiskers appear, wherein the whiskers mainly play roles in strengthening, toughening, improving heat resistance, wear resistance, corrosion resistance, dimensional stability and the like.
Disclosure of Invention
The invention aims to provide a nano potassium titanate whisker reinforced high-temperature-resistant nylon composite material aiming at overcoming the defects in the prior art, and the invention also aims to provide a preparation method of the material. The nanometer potassium titanate whisker after modification treatment is combined with the reasonably improved double-screw extruder module, so that the problem of uniform dispersion of the nanometer potassium titanate whisker in high-temperature resistant nylon is solved, and the high-temperature nylon is reinforced and toughened by the nanometer potassium carbonate whisker.
In order to achieve the purpose, the technical scheme provided by the invention is as follows: the nano potassium titanate whisker reinforced high-temperature-resistant nylon composite material is characterized by being prepared from the following raw materials in parts by weight: 45-60 parts of high-temperature nylon, 20-35 parts of modified nano potassium titanate whiskers, 1-5 parts of an antioxidant and 0.5-2 parts of a heat stabilizer.
Preferably, the high temperature nylon is PA46, PA6T, PA12T or PA 5T.
Preferably, the diameter of the modified nano potassium titanate whisker is 5-15 nm. The preparation method of the nano potassium titanate whisker refers to a document of Li Ice professor of mechanical and dynamic engineering college of eastern university (Catal.Sci.Technol.,2018,8, 6180-containing material 6195), the invention carries out modification treatment on the nano potassium carbonate whisker to obtain the modified nano potassium titanate whisker, and the specific steps are detailed in the examples.
Preferably, the antioxidant is zinc dialkyl dithiophosphate, N', N-diphenyl p-phenylenediamine, antioxidant 1001 or antioxidant 1098.
Preferably, the heat stabilizer is bis (2,2,6, 6-tetramethyl-3-piperidylamino) -isophthalamide, 4' -dioctyl diphenylamine, magnesium stearate or potassium stearate.
The invention also provides a preparation method of the nano potassium titanate whisker reinforced high-temperature-resistant nylon composite material, which comprises the following specific steps of drying the high-temperature nylon and the modified nano potassium titanate whisker, uniformly mixing the dried high-temperature nylon and the modified nano potassium titanate whisker with an antioxidant and a heat stabilizer, pouring the mixture into a hopper of a double-screw extruder, extruding the mixture by the double-screw extruder at a certain extrusion temperature and a certain rotation speed, and then granulating the mixture in a granulator to obtain the nano potassium titanate whisker reinforced high-temperature-resistant nylon plastic particles.
Preferably, the extrusion temperature of the double-screw extruder is 320-360 ℃, and the rotating speed of the double-screw extruder is 200-300 r/min.
Has the advantages that:
the nano potassium titanate whisker reinforced high-temperature-resistant nylon composite material prepared by the invention has the advantages of simple preparation process, low material cost and high productivity. In addition, the modified nano potassium titanate whisker has good dispersion and compatibility in nylon resin, so that the nylon composite material has excellent comprehensive performance, and the application field of the nylon composite material is greatly widened.
Drawings
FIG. 1 is a Scanning Electron Micrograph (SEM) of a nano potassium titanate whisker (SEM) in example 1 of the invention;
FIG. 2 is a scanning electron microscope image of modified nano potassium titanate whiskers (SEM) in example 1 of the invention;
FIG. 3 is an infrared spectrum of the nano potassium titanate whisker reinforced high temperature resistant nylon PA46 in example 1 of the present invention;
FIG. 4 is the X-ray diffraction spectrum of the nano potassium titanate whisker reinforced high temperature resistant nylon PA46 in example 1 of the present invention;
FIG. 5 is the stress-strain curve of the nano potassium titanate whisker reinforced high temperature resistant nylon PA46 in example 1 of the invention.
Detailed Description
The present invention will be described below with reference to specific examples, but the present invention is not limited to the following examples.
Example 1
A nanometer potassium titanate whisker reinforced high temperature resistant nylon composite material and a preparation method thereof are disclosed: 45 parts of high-temperature nylon PA46, 8g of potassium hydroxide nano-titanate whisker (with the diameter of 10nm, the preparation steps of dissolving 8g of potassium hydroxide in 40mL of water, dissolving 1.36g of tetrabutyl titanate in 10mL of ethylene glycol, uniformly mixing the two precursor solutions, weighing 5.29 g of urea and 3.38 g of citric acid, dissolving in a mixed solution, uniformly stirring, pouring into a hydrothermal kettle for reaction at 200 ℃ for 14 hours, naturally cooling the product, adding a deionized water/ethanol mixed solution, centrifugally washing for a plurality of times until the pH value is neutral, drying, grinding into powder, wherein the scanning electron microscope image of the modified nano-potassium titanate whisker shown in figure 2 shows that the average diameter of the whisker is 10nm, and compared with the unmodified nano-potassium titanate whisker shown in figure 1, the modified nano-potassium titanate whisker has a good superfine nanowire structure and the antioxidant (zinc dialkyl dithiophosphate) is 1 part, 0.5 part of heat stabilizer (bis (2,2,6, 6-tetramethyl-3-piperidylamino) -isophthalamide) and 1kg of total processing weight.
Fully drying the high-temperature nylon PA46 and the modified nano potassium titanate whisker to remove water in the high-temperature nylon PA46 and the modified nano potassium titanate whisker; and (2) fully and uniformly mixing the high-temperature-resistant nylon PA46, the modified nano potassium titanate whisker, the antioxidant and the heat stabilizer, pouring the mixture into a hopper of a double-screw extruder, starting the extruder, starting a vacuum pump, extruding the mixture by the double-screw extruder, and then granulating the mixture in a granulator at the extrusion temperature of 320 ℃ and the rotation speed of 200r/min to obtain the nano potassium titanate whisker reinforced high-temperature-resistant nylon PA46 plastic particles. FIG. 3 is an infrared spectrum of nano potassium titanate whisker reinforced high temperature resistant nylon PA46, and it can be seen that the modified potassium titanate whisker is stably distributed in nylon, and the content of functional groups in nylon is increased. FIG. 4 is an X-ray diffraction spectrum of the high temperature resistant nylon PA46 reinforced by nano potassium titanate whiskers, and the diffraction peak becomes stronger and sharper, which can show that the modified nano potassium titanate whiskers improve the crystallization property and strength of PA 46. From the stress-strain curve of the potassium titanate whisker reinforced high temperature resistant nylon PA46 in FIG. 5, it can be seen that the elongation at break (e) of the modified nylon is 42.7%, and the tensile strength (sigma.). sup.b) The elongation at break and tensile strength of 88.6MPa are much higher than those of pure PA46 (e is 38 percent, sigma)b＝57.7MPa)。
Example 2
A nanometer potassium titanate whisker reinforced high temperature resistant nylon composite material and a preparation method thereof are disclosed: 50 parts of high-temperature nylon PA6T, modified nano potassium titanate whisker (the diameter is 5nm, the preparation steps are that 8g of potassium hydroxide is dissolved in 40mL of water, 0.7g of tetrabutyl titanate is dissolved in 10mL of ethylene glycol, the two parts of precursor solutions are uniformly mixed, then 2.65 g of urea and 1.65 g of citric acid are weighed and dissolved in a mixed solution to be uniformly stirred, then the mixture is poured into a hydrothermal kettle to react for 14 hours at 200 ℃, after the product is naturally cooled, deionized water/ethanol mixed solution is added to centrifugally wash for a plurality of times until the pH value is neutral, then the product is dried and ground into powder, the scanning electron microscope image of the modified nano potassium titanate whisker shows that the average diameter of the whisker is 5nm, compared with the unmodified nano potassium titanate whisker electron microscope image, the product has a good superfine nanowire structure) of 25 parts, and an antioxidant (N', N-diphenyl-p-phenylenediamine) of 3 parts, 1 part of heat stabilizer (4,4' -dioctyl diphenylamine) and 1kg of total processing weight.
Fully drying the high-temperature nylon PA6T and the modified nano potassium titanate whisker to remove water in the crystal whisker; and (2) fully and uniformly mixing the high-temperature-resistant nylon PA6T, the modified nano potassium titanate whisker, the antioxidant and the heat stabilizer, pouring the mixture into a hopper of a double-screw extruder, starting the extruder, starting a vacuum pump, extruding the mixture by the double-screw extruder, and then granulating the mixture in a granulator at the extrusion temperature of 325 ℃ and the rotation speed of 250r/min to obtain the nano potassium titanate whisker reinforced high-temperature-resistant nylon plastic particles. The infrared spectrum of the high-temperature-resistant nylon PA6T reinforced by the nano potassium titanate whiskers shows that the modified potassium titanate whiskers are stably distributed in the nylon, and the content of functional groups of the nylon is improved. As seen from the X-ray diffraction spectrum of the nano potassium titanate whisker reinforced high-temperature-resistant nylon PA6T, the diffraction peak becomes stronger and sharper, which can indicate that the modified potassium titanate whisker improves the crystallization property and strength of PA 6T. The elongation at break (e) of the nylon PA6T is 42 percent and the tensile strength (sigma) is obtained by the tensile stress test of the nano potassium titanate whisker reinforced high-temperature resistant nylon PA6Tb) Reaches 83 MPa.
Example 3
A nanometer potassium titanate whisker reinforced high temperature resistant nylon composite material and a preparation method thereof are disclosed: 55 parts of high-temperature nylon PA12T, 8g of potassium hydroxide in 40mL of water, 2.05g of tetrabutyl titanate in 15mL of ethylene glycol, uniformly mixing the two parts of precursor solutions, weighing 7.8 g of urea and 5.05 g of citric acid, uniformly stirring the mixture in a mixed solution, pouring the mixture into a hydrothermal kettle for reaction at 200 ℃ for 14 hours, naturally cooling the product, adding a deionized water/ethanol mixed solution for multiple times of centrifugal washing until the pH value is neutral, drying and grinding the product into powder, wherein the average diameter of the whisker is 15 nanometers, and compared with the unmodified potassium titanate nanowire electron microscope image, the whisker has a good superfine nanowire structure) and 30 parts of antioxidant (antioxidant 1001) and heat stabilizer (magnesium stearate) from a scanning electron microscope image of the modified potassium titanate nanowire whisker, the total weight of the processing was 1 kg.
Fully drying the high-temperature nylon PA6T and the modified nano potassium titanate whisker to remove water in the crystal whisker; and (2) fully and uniformly mixing the high-temperature-resistant nylon PA12T, the modified nano potassium titanate whisker, the antioxidant and the heat stabilizer, pouring the mixture into a hopper of a double-screw extruder, starting the extruder, starting a vacuum pump, extruding the mixture by the double-screw extruder, and then feeding the mixture into a granulator for granulation, wherein the extrusion temperature is 320 ℃, and the rotation speed is 300r/min, so as to obtain the nano potassium titanate whisker reinforced high-temperature-resistant nylon plastic particles. The infrared spectrum of the high-temperature-resistant nylon PA6T reinforced by the nano potassium titanate whiskers shows that the modified potassium titanate whiskers are stably distributed in the nylon, and the content of functional groups of the nylon is improved. As seen from the X-ray diffraction spectrum of the nano potassium titanate whisker reinforced high-temperature-resistant nylon PA6T, the diffraction peak becomes stronger and sharper, which can indicate that the modified potassium titanate whisker improves the crystallization property and strength of PA 6T. The elongation at break (e) of the nylon PA6T is 45 percent and the tensile strength (sigma) is obtained by the tensile stress test of the nano potassium titanate whisker reinforced high-temperature resistant nylon PA6Tb) Reaches 89 MPa.
Example 4
A nanometer potassium titanate whisker reinforced high temperature resistant nylon composite material and a preparation method thereof are disclosed: 60 parts of high-temperature nylon PA5T, 35 parts of modified nano potassium titanate whisker (same as example 1), 5 parts of antioxidant (antioxidant 1098), 1.5 parts of heat stabilizer (potassium stearate), and the total processing weight is 1 kg.
Fully drying the high-temperature nylon PA5T and the modified nano potassium titanate whisker to remove water in the high-temperature nylon PA5T and the modified nano potassium titanate whisker; and (2) fully and uniformly mixing the high-temperature-resistant nylon PA12T, the modified nano potassium titanate whisker, the antioxidant and the heat stabilizer, pouring the mixture into a hopper of a double-screw extruder, starting the extruder, starting a vacuum pump, extruding the mixture by the double-screw extruder, and then granulating the mixture in a granulator at the extrusion temperature of 325 ℃ and the rotation speed of 250r/min to obtain the nano potassium titanate whisker reinforced high-temperature-resistant nylon plastic particles. The infrared spectrum of the high-temperature-resistant nylon PA5T enhanced by the nano potassium titanate whiskers shows that the modified potassium titanate whiskers are stably distributed in the nylon, and the content of functional groups of the nylon is improved. From the X-ray diffraction spectrum of the nano potassium titanate whisker reinforced high-temperature-resistant nylon PA5TIt is seen that the diffraction peak becomes more intense and sharp, which indicates that the modified potassium titanate whisker improves the crystallization property and strength of PA 5T. The elongation at break (e) of the nylon PA5T is 40 percent and the tensile strength (sigma) is obtained by the tensile stress test of the nano potassium titanate whisker reinforced high-temperature resistant nylon PA5Tb) Reaching 80.3 MPa.
Example 5
A nanometer potassium titanate whisker reinforced high temperature resistant nylon composite material and a preparation method thereof are disclosed: 60 parts of high-temperature nylon PA46, 25 parts of modified nano potassium titanate whisker (same as example 3), 2 parts of antioxidant (antioxidant 1098), 1 part of heat stabilizer (magnesium stearate), and the total processing weight is 1 kg.
Fully drying the high-temperature nylon PA46 and the modified nano potassium titanate whisker to remove water in the high-temperature nylon PA46 and the modified nano potassium titanate whisker; and (2) fully and uniformly mixing the high-temperature-resistant nylon PA46, the modified nano potassium titanate whisker, the antioxidant and the heat stabilizer, pouring the mixture into a hopper of a double-screw extruder, starting the extruder, starting a vacuum pump, extruding the mixture by the double-screw extruder, and then granulating the mixture in a granulator at the extrusion temperature of 350 ℃ and the rotation speed of 250r/min to obtain the nano potassium titanate whisker reinforced high-temperature-resistant nylon plastic particles. The infrared spectrum of the high-temperature-resistant nylon PA46 enhanced by the nano potassium titanate whiskers shows that the modified potassium titanate whiskers are stably distributed in the nylon, and the content of functional groups of the nylon is improved. As seen from the X-ray diffraction spectrum of the nano potassium titanate whisker reinforced high-temperature-resistant nylon PA46, the diffraction peak becomes stronger and sharper, which can indicate that the modified potassium titanate whisker improves the crystallization property and strength of PA 46. The elongation at break (e) of the nylon PA46 is 43.1 percent and the tensile strength (sigma) is obtained by the tensile stress test of the nano potassium titanate whisker reinforced high-temperature resistant nylon PA46b) Reaches 89.5 MPa.
Example 6
A nanometer potassium titanate whisker reinforced high temperature resistant nylon composite material and a preparation method thereof are disclosed: 55 parts of high-temperature nylon PA46, 20 parts of modified nano potassium titanate whisker (same as example 1), 5 parts of antioxidant (N', N-diphenyl-p-phenylenediamine), 0.5 part of heat stabilizer (potassium stearate), and the total processing weight is 1 kg. Fully drying the high-temperature nylon PA46 and the modified nano potassium titanate whisker to remove water in the high-temperature nylon PA46 and the modified nano potassium titanate whiskerDividing; and (2) fully and uniformly mixing the high-temperature-resistant nylon PA46, the modified nano potassium titanate whisker, the antioxidant and the heat stabilizer, pouring the mixture into a hopper of a double-screw extruder, starting the extruder, starting a vacuum pump, extruding the mixture by the double-screw extruder, and then granulating the mixture in a granulator at the extrusion temperature of 360 ℃ and the rotation speed of 300r/min to obtain the nano potassium titanate whisker reinforced high-temperature-resistant nylon plastic particles. The infrared spectrum of the high-temperature-resistant nylon PA46 enhanced by the nano potassium titanate whiskers shows that the modified potassium titanate whiskers are stably distributed in the nylon, and the content of functional groups of the nylon is improved. As seen from the X-ray diffraction spectrum of the nano potassium titanate whisker reinforced high-temperature-resistant nylon PA46, the diffraction peak becomes stronger and sharper, which can indicate that the modified potassium titanate whisker improves the crystallization property and strength of PA 46. The elongation at break (e) of the nylon PA46 is 42.5 percent and the tensile strength (sigma) is obtained by the tensile stress test of the nano potassium titanate whisker reinforced high-temperature resistant nylon PA46b) Reaches 88 MPa.
Claims (7)
1. The nano potassium titanate whisker reinforced high-temperature-resistant nylon composite material is characterized by being prepared from the following raw materials in parts by weight: 45-60 parts of high-temperature nylon, 20-35 parts of modified nano potassium titanate whiskers, 1-5 parts of an antioxidant and 0.5-2 parts of a heat stabilizer.
2. The nano potassium titanate whisker reinforced high temperature resistant nylon composite material of claim 1, characterized in that: the high-temperature nylon is PA46, PA6T, PA12T or PA 5T.
3. The nano potassium titanate whisker reinforced high temperature resistant nylon composite material of claim 1, characterized in that: the diameter of the modified nano potassium titanate whisker is 5-15 nanometers.
4. The nano potassium titanate whisker reinforced high temperature resistant nylon composite material of claim 1, characterized in that: the antioxidant is zinc dialkyl dithiophosphate, N', N-diphenyl p-phenylenediamine, antioxidant 1001 or antioxidant 1098.
5. The nano potassium titanate whisker reinforced high temperature resistant nylon composite material of claim 1, characterized in that: the heat stabilizer is bis (2,2,6, 6-tetramethyl-3-piperidyl amido) -isophthalamide, 4' -dioctyl diphenylamine, magnesium stearate or potassium stearate.
6. A method for preparing the nano potassium titanate whisker reinforced high-temperature-resistant nylon composite material as claimed in claim 1 comprises the following specific steps of drying high-temperature nylon and modified nano potassium titanate whiskers, uniformly mixing the dried high-temperature nylon and the modified nano potassium titanate whiskers with an antioxidant and a heat stabilizer, pouring the mixture into a hopper of a double-screw extruder, extruding the mixture by the double-screw extruder at a certain extrusion temperature and a certain rotation speed, and then granulating the mixture in a granulator to obtain the nano potassium titanate whisker reinforced high-temperature-resistant nylon plastic particles.
7. The method of claim 6, wherein: the extrusion temperature of the double-screw extruder is 320-360 ℃, and the rotating speed of the double-screw extruder is 200-300 r/min.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114031939A (en) * | 2021-12-03 | 2022-02-11 | 江苏博云塑业股份有限公司 | Nylon/titanic acid nanosheet composite material and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104710780A (en) * | 2013-12-16 | 2015-06-17 | 上海杰事杰新材料(集团)股份有限公司 | Ceramic whisker enhanced high-temperature-resistant nylon composite material and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104710780A (en) * | 2013-12-16 | 2015-06-17 | 上海杰事杰新材料(集团)股份有限公司 | Ceramic whisker enhanced high-temperature-resistant nylon composite material and preparation method thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114031939A (en) * | 2021-12-03 | 2022-02-11 | 江苏博云塑业股份有限公司 | Nylon/titanic acid nanosheet composite material and preparation method thereof |
| CN114031939B (en) * | 2021-12-03 | 2023-10-27 | 江苏博云塑业股份有限公司 | Nylon/titanic acid nano-sheet composite material and preparation method thereof |
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