CN113683773A - Method for synergistically enhancing MC nylon composite material by using nano particles - Google Patents
Method for synergistically enhancing MC nylon composite material by using nano particles Download PDFInfo
- Publication number
- CN113683773A CN113683773A CN202110862249.3A CN202110862249A CN113683773A CN 113683773 A CN113683773 A CN 113683773A CN 202110862249 A CN202110862249 A CN 202110862249A CN 113683773 A CN113683773 A CN 113683773A
- Authority
- CN
- China
- Prior art keywords
- particles
- glass fiber
- gamma
- composite material
- product
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 239000004677 Nylon Substances 0.000 title claims abstract description 42
- 229920001778 nylon Polymers 0.000 title claims abstract description 42
- 238000000034 method Methods 0.000 title claims abstract description 30
- 239000002131 composite material Substances 0.000 title claims abstract description 26
- 239000002105 nanoparticle Substances 0.000 title claims abstract description 21
- 230000002708 enhancing effect Effects 0.000 title claims abstract description 10
- 239000002245 particle Substances 0.000 claims abstract description 71
- 239000003365 glass fiber Substances 0.000 claims abstract description 39
- 239000010445 mica Substances 0.000 claims abstract description 38
- 229910052618 mica group Inorganic materials 0.000 claims abstract description 38
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 claims abstract description 16
- 125000003700 epoxy group Chemical group 0.000 claims abstract description 11
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 claims abstract description 9
- NBXZNTLFQLUFES-UHFFFAOYSA-N triethoxy(propyl)silane Chemical compound CCC[Si](OCC)(OCC)OCC NBXZNTLFQLUFES-UHFFFAOYSA-N 0.000 claims abstract description 8
- JBKVHLHDHHXQEQ-UHFFFAOYSA-N epsilon-caprolactam Chemical group O=C1CCCCCN1 JBKVHLHDHHXQEQ-UHFFFAOYSA-N 0.000 claims description 28
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 24
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 20
- 238000001035 drying Methods 0.000 claims description 19
- 238000006243 chemical reaction Methods 0.000 claims description 17
- 238000001816 cooling Methods 0.000 claims description 15
- 238000002156 mixing Methods 0.000 claims description 13
- 238000006482 condensation reaction Methods 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 10
- 238000010992 reflux Methods 0.000 claims description 10
- 230000002195 synergetic effect Effects 0.000 claims description 10
- 238000009210 therapy by ultrasound Methods 0.000 claims description 10
- 238000001291 vacuum drying Methods 0.000 claims description 10
- 238000005406 washing Methods 0.000 claims description 10
- SJECZPVISLOESU-UHFFFAOYSA-N 3-trimethoxysilylpropan-1-amine Chemical compound CO[Si](OC)(OC)CCCN SJECZPVISLOESU-UHFFFAOYSA-N 0.000 claims description 8
- DVKJHBMWWAPEIU-UHFFFAOYSA-N toluene 2,4-diisocyanate Chemical compound CC1=CC=C(N=C=O)C=C1N=C=O DVKJHBMWWAPEIU-UHFFFAOYSA-N 0.000 claims description 8
- 238000011065 in-situ storage Methods 0.000 claims description 5
- 238000006116 polymerization reaction Methods 0.000 claims description 5
- 238000000926 separation method Methods 0.000 claims description 5
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 3
- 238000013329 compounding Methods 0.000 claims description 3
- 230000003014 reinforcing effect Effects 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 229910052681 coesite Inorganic materials 0.000 abstract description 4
- 229910052906 cristobalite Inorganic materials 0.000 abstract description 4
- 238000005516 engineering process Methods 0.000 abstract description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 abstract description 4
- 229910052682 stishovite Inorganic materials 0.000 abstract description 4
- 229910052905 tridymite Inorganic materials 0.000 abstract description 4
- 229920006351 engineering plastic Polymers 0.000 abstract description 3
- 230000004048 modification Effects 0.000 abstract description 2
- 238000012986 modification Methods 0.000 abstract description 2
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 6
- 238000002360 preparation method Methods 0.000 description 4
- 238000005303 weighing Methods 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 2
- 230000018044 dehydration Effects 0.000 description 2
- 238000006297 dehydration reaction Methods 0.000 description 2
- 239000000945 filler Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000000178 monomer Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 230000003213 activating effect Effects 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 150000001450 anions Chemical group 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000000977 initiatory effect Effects 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 230000009878 intermolecular interaction Effects 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 238000002715 modification method Methods 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 238000007151 ring opening polymerisation reaction Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G69/00—Macromolecular compounds obtained by reactions forming a carboxylic amide link in the main chain of the macromolecule
- C08G69/02—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids
- C08G69/08—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids derived from amino-carboxylic acids
- C08G69/14—Lactams
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G69/00—Macromolecular compounds obtained by reactions forming a carboxylic amide link in the main chain of the macromolecule
- C08G69/02—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids
- C08G69/08—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids derived from amino-carboxylic acids
- C08G69/14—Lactams
- C08G69/16—Preparatory processes
-
- 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
- C08J5/005—Reinforced macromolecular compounds with nanosized materials, e.g. nanoparticles, nanofibres, nanotubes, nanowires, nanorods or nanolayered 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
- 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
- C08J5/08—Reinforcing macromolecular compounds with loose or coherent fibrous material using pretreated fibrous materials glass fibres
-
- 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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-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
- C08K7/00—Use of ingredients characterised by shape
- C08K7/02—Fibres or whiskers
- C08K7/04—Fibres or whiskers inorganic
- C08K7/14—Glass
-
- 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
- C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
-
- 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
- C08J2377/02—Polyamides derived from omega-amino carboxylic acids or from lactams thereof
Abstract
The invention discloses a method for synergistically enhancing an MC nylon composite material by utilizing nano particles, which belongs to the field of engineering plastic modification and comprises the following steps: s1, modifying mica with gamma-Aminopropyltriethoxysilane (APTES) to prepare amino modified mica particles; s2, modifying the glass fiber particles by adopting gamma-glycidyl ether propyl triethoxysilane (gamma-GPS) to prepare the epoxy group modified glass fiber particles. Compared with pure MC nylon, the MC nylon/SiC @ SiO2 composite material prepared by the method has the advantages of high mechanical strength, good heat resistance, good wear resistance and the like, can meet the requirements of heat resistance and frictional wear resistance under higher load, and has wide application prospect in the high and new technology field.
Description
Technical Field
The invention relates to the field of engineering plastic modification, in particular to a method for synergistically enhancing an MC nylon composite material by using nanoparticles.
Background
Monomer casting nylon (MC nylon, MC PA6 for short) is a nylon product obtained by anion ring-opening polymerization reaction of caprolactam monomer under the conditions of activating agent, initiating agent and specific temperature, because MC nylon has the advantages of simple forming process, high mechanical strength, good chemical stability and light weight, etc., it can replace steel, copper, aluminum, etc. to be used for manufacturing parts such as bush, shaft sleeve, gear, rack, worm gear, pulley, loom shuttle, propeller and various sealing rings, etc., and has the functions of reducing weight and cost, therefore, MC nylon is widely used in the fields of textile machinery, national defense, chemical industry, etc., with the development of science and technology, MC nylon has certain defects, which leads to the application of nylon products to be limited, for example, because of poor heat resistance, the MC nylon has limited application in the high-temperature field, and relatively low mechanical strength and toughness compared with metal materials, making their use in mechanical load-bearing articles limited.
The inorganic nano particles are adopted to modify the polymer material, so that the material performance can be effectively improved, the cost is low, and the inorganic nano particles become one of novel materials with the most development potential.
The invention provides a method for synergistically enhancing MC nylon engineering plastics by using nano particles, which takes massive mica powder and glass fiber powder with high length-diameter ratio as raw materials, adopts gamma-Aminopropyltriethoxysilane (APTES) to modify mica particles, adopts gamma-glycidyl ether propyl triethoxysilane (gamma-GPS) to modify glass fiber particles, improves the compatibility of the glass fiber particles in MC nylon and monomers, and improves the intermolecular interaction force of a filler and a nylon molecular main chain and the interaction force between the fillers; the MC nylon modification method provided by the invention has the advantages of rich raw materials, short production period, simple and easy technological process and the like, and the synergistically enhanced MC nylon composite material prepared by the method has the characteristics of high hardness, good thermal stability, excellent mechanical properties and the like.
Disclosure of Invention
1. Technical problem to be solved
Aiming at the problems in the prior art, the invention aims to provide a method for synergistically enhancing an MC nylon composite material by utilizing nano particles.
2. Technical scheme
In order to solve the problems, the invention adopts the following technical scheme:
a method for synergistically enhancing an MC nylon composite material by utilizing nanoparticles comprises the following steps:
s1, modifying mica with gamma-Aminopropyltriethoxysilane (APTES) to prepare amino modified mica particles;
s2, modifying the glass fiber particles by adopting gamma-glycidyl ether propyl triethoxysilane (gamma-GPS) to prepare epoxy group modified glass fiber particles;
s3, compounding the MC nylon with the amino-modified mica particles and the epoxy-modified glass fiber particles through an in-situ polymerization method to construct a reinforcing network, and preparing the nano particle synergetic reinforced MC nylon composite material. Compared with pure MC nylon, the MC nylon/SiC @ SiO2 composite material prepared by the method has the advantages of high mechanical strength, good heat resistance, good wear resistance and the like, can meet the requirements of heat resistance and frictional wear resistance under higher load, and has wide application prospect in the high and new technology field.
As a preferable embodiment of the present invention, in step S1, the method specifically includes the following steps:
s11, placing the mica particles in a drying oven at 150 ℃ for constant temperature for 4h, cooling to room temperature, dispersing the mica particles in absolute ethyl alcohol, and carrying out ultrasonic treatment for 20-90 min;
s12, mixing the mica particles with the gamma-aminopropyl triethoxysilane (APTES) according to the mass ratio of 100: (2-7), adding 3-aminopropyl trimethoxy silane (APTMS) for reaction, raising the reaction temperature to 60 ℃, and carrying out reflux condensation reaction for 4-8h to obtain a product;
s13, performing centrifugal separation on the product, washing the product for 3 to 5 times by using absolute ethyl alcohol, and drying the product in a vacuum drying oven at 70 ℃ for 8 to 16 hours to prepare the amino modified mica particles.
As a preferable embodiment of the present invention, in step S2, the method specifically includes the following steps:
s21, placing the glass fiber particles in a drying oven at 150 ℃ and keeping the temperature for 4 hours, cooling to room temperature, dispersing the glass fiber particles in absolute ethyl alcohol, and carrying out ultrasonic treatment for 20-90 min;
s22, mixing the glass fiber particles and the gamma-glycidyl ether propyl triethoxysilane (gamma-GPS) according to the mass ratio of 100: (2-7), adding a silane coupling agent (gamma-GPS) for reaction, adjusting the pH to 5-6, raising the reaction temperature to 60 ℃, and carrying out reflux condensation reaction for 4-8 hours;
and S23, centrifugally separating the product, washing the product for 3 to 5 times by using absolute ethyl alcohol, and drying the product for 8 to 16 hours in a vacuum drying oven at the temperature of 70 ℃ to obtain the epoxy group modified glass fiber particles.
As a preferable embodiment of the present invention, in step S3, the method specifically includes the following steps:
s31, adding caprolactam monomer into a reactor, heating to 75-95 ℃ to melt all caprolactam, the amino-modified mica particles and the epoxy-modified glass fiber particles according to the mass ratio of 100: (0.1-6): (0.1-6), stirring strongly to disperse uniformly, heating to 115 ℃ and 135 ℃, and dehydrating in vacuum for 20-60 min;
s32, first-stage vacuum relief, and mixing caprolactam and sodium hydroxide according to a molar ratio of 100: (0.1-1.0), then adding sodium hydroxide, and dehydrating in vacuum at 135-145 ℃ for 20-60 min;
s33, secondary vacuum relief, and mixing caprolactam and toluene diisocyanate according to a molar ratio of 100: (0.1-0.8), then adding toluene diisocyanate, quickly shaking up, quickly pouring into a mold preheated to 160-180 ℃, preserving heat for 20-30 min, cooling to room temperature, and demolding to obtain the nano particle synergistic reinforced MC nylon composite material.
3. Advantageous effects
Compared with the prior art, the invention has the advantages that:
compared with pure MC nylon, the MC nylon/SiC @ SiO2 composite material prepared by the method has the advantages of high mechanical strength, good heat resistance, good wear resistance and the like, can meet the requirements of heat resistance and frictional wear resistance under higher load, and has wide application prospect in the high and new technology field.
Drawings
FIG. 1 is a flow chart of a method for synergistically enhancing MC nylon composite material by using nanoparticles according to the present invention.
Detailed Description
The technical solution in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention. It is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments, and all other embodiments obtained by those skilled in the art without any inventive work are within the scope of the present invention.
Example 1:
referring to fig. 1, a method for synergistically enhancing an MC nylon composite material by using nanoparticles includes the following steps:
s1, modifying mica with gamma-Aminopropyltriethoxysilane (APTES) to prepare amino modified mica particles:
s11, placing the mica particles in a drying oven at 150 ℃ for constant temperature for 4h, cooling to room temperature, dispersing the mica particles in absolute ethyl alcohol, and carrying out ultrasonic treatment for 20-90 min;
s12, mixing the mica particles with gamma-aminopropyl triethoxysilane (APTES) according to the mass ratio of 100: (2-7), adding 3-aminopropyl trimethoxy silane (APTMS) for reaction, raising the reaction temperature to 60 ℃, and carrying out reflux condensation reaction for 4-8h to obtain a product;
s13, performing centrifugal separation on the product, washing the product for 3-5 times by using absolute ethyl alcohol, and drying the product in a vacuum drying oven at 70 ℃ for 8-16 h to obtain amino modified mica particles;
s2, modifying the glass fiber particles by adopting gamma-glycidyl ether propyl triethoxysilane (gamma-GPS) to prepare the epoxy group modified glass fiber particles:
s21, placing the glass fiber particles in an oven at 150 ℃ and keeping the temperature for 4 hours, dispersing the glass fiber particles in absolute ethyl alcohol after cooling to room temperature, and carrying out ultrasonic treatment for 20-90 min;
s22, mixing the glass fiber particles with gamma-glycidyl ether propyl triethoxysilane (gamma-GPS) according to the mass ratio of 100: (2-7), adding a silane coupling agent (gamma-GPS) for reaction, adjusting the pH to 5-6, raising the reaction temperature to 60 ℃, and carrying out reflux condensation reaction for 4-8 hours;
s23, centrifugally separating the product, washing the product for 3-5 times by using absolute ethyl alcohol, and drying the product in a vacuum drying oven at 70 ℃ for 8-16 h to obtain epoxy group modified glass fiber particles;
s3, compounding MC nylon, amino-modified mica particles and epoxy-modified glass fiber particles through an in-situ polymerization method, constructing a reinforcing network, and preparing the nano particle synergetic reinforced MC nylon composite material:
s31, adding caprolactam monomer into a reactor, heating to 75-95 ℃ to melt the caprolactam monomer completely, and mixing the caprolactam monomer, the amino-modified mica particles and the epoxy-modified glass fiber particles according to a mass ratio of 100: (0.1-6): (0.1-6), stirring strongly to disperse uniformly, heating to 115 ℃ and 135 ℃, and dehydrating in vacuum for 20-60 min;
s32, first-stage vacuum relief, and mixing caprolactam and sodium hydroxide according to a molar ratio of 100: (0.1-1.0), then adding sodium hydroxide, and dehydrating in vacuum at 135-145 ℃ for 20-60 min;
s33, secondary vacuum relief, and mixing caprolactam and toluene diisocyanate according to a molar ratio of 100: (0.1-0.8), then adding toluene diisocyanate, quickly shaking up, quickly pouring into a mold preheated to 160-180 ℃, preserving heat for 20-30 min, cooling to room temperature, and demolding to obtain the nano particle synergistic reinforced MC nylon composite material.
Example 2:
1. preparation of amino-modified mica particles: placing 4 g of mica particles in a drying oven at 150 ℃ for constant temperature for 4h, cooling to room temperature, dispersing in 250 mL of absolute ethyl alcohol, and performing ultrasonic treatment for 40 min; adding 0.15 g of APTMS, raising the reaction temperature to 60 ℃, carrying out reflux condensation reaction for 6 h, carrying out centrifugal separation on the product, washing the product for 5 times by using absolute ethyl alcohol, and drying the product in a vacuum drying oven at 70 ℃ for 8h to obtain amino modified mica particles;
2. preparation of epoxy group modified glass fiber particles: placing 4 g of glass fiber particles in a drying oven with the temperature of 150 ℃ for constant temperature for 4h, cooling to room temperature, dispersing in 250 mL of absolute ethyl alcohol, and performing ultrasonic treatment for 40 min; adding 0.15 g of gamma-GPS, adjusting the Ph to 5.5 by using acetic acid, raising the reaction temperature to 60 ℃, and carrying out reflux condensation reaction for 6 hours; centrifugally separating the product, washing the product for 5 times by using absolute ethyl alcohol, and drying the product for 8 hours in a vacuum drying oven at 70 ℃ to obtain epoxy group modified glass fiber particles;
3. preparing a composite material by an in-situ polymerization method: weighing 100g of caprolactam monomer, adding the caprolactam monomer into a reactor, heating to 85 ℃ to melt the caprolactam monomer, weighing 1g of amino-modified mica particles and 1g of epoxy-modified glass fiber particles, adding the amino-modified mica particles and the epoxy-modified glass fiber particles into the reactor, uniformly dispersing, heating to 130 ℃, and performing vacuum dehydration for 20 min; removing vacuum, adding 0.5 g of sodium hydroxide, and vacuum dehydrating at 140 deg.C for 20 min; and (3) removing vacuum, adding 0.5 g of toluene diisocyanate, quickly shaking up, quickly pouring into a mold preheated to 165 ℃ in advance, preserving heat for 20min, cooling to room temperature, and demolding to obtain the MC nylon/SiC @ SiO2 composite material product.
Example 3:
1. preparation of amino-modified mica particles: placing 20 g of mica particles in a drying oven at 150 ℃ for constant temperature for 4h, cooling to room temperature, dispersing in 4000 mL of absolute ethanol, and performing ultrasonic treatment for 60 min; adding 0.8 g of APTMS, raising the reaction temperature to 60 ℃, carrying out reflux condensation reaction for 6 h, carrying out centrifugal separation on the product, washing the product for 5 times by using absolute ethyl alcohol, and drying the product in a vacuum drying oven at 70 ℃ for 8h to obtain amino modified mica particles;
2. preparation of epoxy group modified glass fiber particles: placing 20 g of glass fiber particles in a drying oven with the temperature of 150 ℃ for 4h, cooling to room temperature, dispersing in 4000 mL of absolute ethyl alcohol, and performing ultrasonic treatment for 60 min; adding 0.8 g of gamma-GPS, adjusting the pH value to 5.5 by using acetic acid, raising the reaction temperature to 60 ℃, and carrying out reflux condensation reaction for 6 hours; and (3) centrifugally separating the product, washing the product for 5 times by using absolute ethyl alcohol, and drying the product for 8 hours in a vacuum drying oven at 70 ℃ to obtain the epoxy group modified glass fiber particles.
3. Preparing a composite material by an in-situ polymerization method: weighing 200g of caprolactam monomer, adding the caprolactam monomer into a reactor, heating to 85 ℃ to melt the caprolactam monomer, weighing 1.8g of amino-modified mica particles and 1.8g of epoxy-modified glass fiber particles, adding the amino-modified mica particles and the epoxy-modified glass fiber particles into the reactor, uniformly dispersing, heating to 130 ℃, and performing vacuum dehydration for 20 min; removing vacuum, adding 0.95 g of sodium hydroxide, and vacuum dehydrating at 140 deg.C for 20 min; and (3) removing vacuum, adding 1g of toluene diisocyanate, quickly shaking up, quickly pouring into a mold preheated to 170 ℃, preserving heat for 20min, cooling to room temperature, and demolding to obtain the synergistic reinforced MC nylon composite material product.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the equivalent replacement or change according to the technical solution and the modified concept of the present invention should be covered by the scope of the present invention.
Claims (4)
1. A method for cooperatively enhancing an MC nylon composite material by utilizing nano particles is characterized by comprising the following steps:
s1, modifying mica with gamma-Aminopropyltriethoxysilane (APTES) to prepare amino modified mica particles;
s2, modifying the glass fiber particles by adopting gamma-glycidyl ether propyl triethoxysilane (gamma-GPS) to prepare epoxy group modified glass fiber particles;
s3, compounding the MC nylon with the amino-modified mica particles and the epoxy-modified glass fiber particles through an in-situ polymerization method to construct a reinforcing network, and preparing the nano particle synergetic reinforced MC nylon composite material.
2. The method for the synergistic enhancement of the MC nylon composite material by the nano particles as claimed in claim 1, wherein in step S1, the method comprises the following steps:
s11, placing the mica particles in a drying oven at 150 ℃ for constant temperature for 4h, cooling to room temperature, dispersing the mica particles in absolute ethyl alcohol, and carrying out ultrasonic treatment for 20-90 min;
s12, mixing the mica particles with the gamma-aminopropyl triethoxysilane (APTES) according to the mass ratio of 100: (2-7), adding 3-aminopropyl trimethoxy silane (APTMS) for reaction, raising the reaction temperature to 60 ℃, and carrying out reflux condensation reaction for 4-8h to obtain a product;
s13, performing centrifugal separation on the product, washing the product for 3 to 5 times by using absolute ethyl alcohol, and drying the product in a vacuum drying oven at 70 ℃ for 8 to 16 hours to prepare the amino modified mica particles.
3. The method for the synergistic enhancement of the MC nylon composite material by the nano particles as claimed in claim 1, wherein in step S2, the method comprises the following steps:
s21, placing the glass fiber particles in a drying oven at 150 ℃ and keeping the temperature for 4 hours, cooling to room temperature, dispersing the glass fiber particles in absolute ethyl alcohol, and carrying out ultrasonic treatment for 20-90 min;
s22, mixing the glass fiber particles and the gamma-glycidyl ether propyl triethoxysilane (gamma-GPS) according to the mass ratio of 100: (2-7), adding a silane coupling agent (gamma-GPS) for reaction, adjusting the pH to 5-6, raising the reaction temperature to 60 ℃, and carrying out reflux condensation reaction for 4-8 hours;
and S23, centrifugally separating the product, washing the product for 3 to 5 times by using absolute ethyl alcohol, and drying the product for 8 to 16 hours in a vacuum drying oven at the temperature of 70 ℃ to obtain the epoxy group modified glass fiber particles.
4. The method for the synergistic enhancement of the MC nylon composite material by the nano particles as claimed in claim 1, wherein in step S3, the method comprises the following steps:
s31, adding caprolactam monomer into a reactor, heating to 75-95 ℃ to melt all caprolactam, the amino-modified mica particles and the epoxy-modified glass fiber particles according to the mass ratio of 100: (0.1-6): (0.1-6), stirring strongly to disperse uniformly, heating to 115 ℃ and 135 ℃, and dehydrating in vacuum for 20-60 min;
s32, first-stage vacuum relief, and mixing caprolactam and sodium hydroxide according to a molar ratio of 100: (0.1-1.0), then adding sodium hydroxide, and dehydrating in vacuum at 135-145 ℃ for 20-60 min;
s33, secondary vacuum relief, and mixing caprolactam and toluene diisocyanate according to a molar ratio of 100: (0.1-0.8), then adding toluene diisocyanate, quickly shaking up, quickly pouring into a mold preheated to 160-180 ℃, preserving heat for 20-30 min, cooling to room temperature, and demolding to obtain the nano particle synergistic reinforced MC nylon composite material.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202110862249.3A CN113683773A (en) | 2021-07-29 | 2021-07-29 | Method for synergistically enhancing MC nylon composite material by using nano particles |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202110862249.3A CN113683773A (en) | 2021-07-29 | 2021-07-29 | Method for synergistically enhancing MC nylon composite material by using nano particles |
Publications (1)
Publication Number | Publication Date |
---|---|
CN113683773A true CN113683773A (en) | 2021-11-23 |
Family
ID=78578232
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN202110862249.3A Pending CN113683773A (en) | 2021-07-29 | 2021-07-29 | Method for synergistically enhancing MC nylon composite material by using nano particles |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN113683773A (en) |
Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1718421A (en) * | 2004-07-29 | 2006-01-11 | 南京理工大学 | Preparation method of composite material of fiber and granular synergistic reinforced pouring nylon |
CN103509336A (en) * | 2012-10-18 | 2014-01-15 | 中国科学院化学研究所 | Monomer casting (MC) nylon composite material and preparation method thereof |
CN103923312A (en) * | 2014-04-02 | 2014-07-16 | 合肥杰事杰新材料股份有限公司 | High-strength and low-retraction casting nylon composite material and preparation method thereof |
CN104098764A (en) * | 2013-04-09 | 2014-10-15 | 合肥杰事杰新材料股份有限公司 | Cast nylon 6 heatproof composite material and preparation method thereof |
CN106189214A (en) * | 2016-08-02 | 2016-12-07 | 苏州锐特捷化工制品有限公司 | A kind of preparation method of high intensity MC nylon modified fibre composite base material |
CN111961337A (en) * | 2020-08-13 | 2020-11-20 | 扬州尼尔工程塑料有限公司 | MC nylon/SiC @ SiO2Method for preparing composite material |
-
2021
- 2021-07-29 CN CN202110862249.3A patent/CN113683773A/en active Pending
Patent Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1718421A (en) * | 2004-07-29 | 2006-01-11 | 南京理工大学 | Preparation method of composite material of fiber and granular synergistic reinforced pouring nylon |
CN103509336A (en) * | 2012-10-18 | 2014-01-15 | 中国科学院化学研究所 | Monomer casting (MC) nylon composite material and preparation method thereof |
CN104098764A (en) * | 2013-04-09 | 2014-10-15 | 合肥杰事杰新材料股份有限公司 | Cast nylon 6 heatproof composite material and preparation method thereof |
CN103923312A (en) * | 2014-04-02 | 2014-07-16 | 合肥杰事杰新材料股份有限公司 | High-strength and low-retraction casting nylon composite material and preparation method thereof |
CN106189214A (en) * | 2016-08-02 | 2016-12-07 | 苏州锐特捷化工制品有限公司 | A kind of preparation method of high intensity MC nylon modified fibre composite base material |
CN111961337A (en) * | 2020-08-13 | 2020-11-20 | 扬州尼尔工程塑料有限公司 | MC nylon/SiC @ SiO2Method for preparing composite material |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN101220196B (en) | Poly(ether-ether-ketone) composite material, production method and application of sealing member | |
CN102010593B (en) | Mineral and long glass fiber reinforced nylon 6 composite material and preparation method thereof | |
CN109694570B (en) | High-strength super-wear-resistant MC nylon composite material and preparation method thereof | |
CN102010547A (en) | Mineral/long glass fiber reinforced polypropylene composite material and preparation method thereof | |
CN106380678A (en) | High dielectric property polypropylene/nylon/whisker composite material and preparation method thereof | |
CN104974346A (en) | Preparation method of liquid-crystal allyl-compound-modified bismaleimide resin | |
CN111534095A (en) | ZnS quantum dot/MXene/polymer-based super-wear-resistant self-lubricating composite material and preparation method and application thereof | |
CN1123602C (en) | Refractory antiwear polyimide as sealing material and its preparing process and application | |
CN106633857A (en) | High heat resistance and wear resistance glass fiber enhanced nylon material for engine and preparation method | |
CN109306179A (en) | Purposes of the polyamide 5X as enhancing thermoplastic compounds apparent mass improver | |
CN100480323C (en) | Bi-maleimide self-lubricating nano-composite material and preparing method thereof | |
CN113683773A (en) | Method for synergistically enhancing MC nylon composite material by using nano particles | |
CN101457021A (en) | Nano silicon nitride/bimaleimide resin/cyanate ester resin composite material and preparation method thereof | |
CN106834777A (en) | A kind of preparation method of low-expansion coefficient composition metal base ceramic die material | |
CN101579903B (en) | Application of polyamide alloy in preparation of pipelines and pipe fittings with flanges or wellhead seat products | |
CN103570937B (en) | Phenolic resin/MC nylon composite material, and preparation method thereof | |
CN112029265A (en) | Blank of automobile plate spring baffle or bracket and preparation method of finished product of blank | |
CN111925648A (en) | Method for synergistically modifying MC nylon engineering plastic by using graphene oxide/polytetrafluoroethylene compound | |
CN107189159B (en) | Single-screw ultrahigh molecular weight polyethylene high-temperature-resistant pipe and preparation method thereof | |
CN103289079B (en) | Composite material of nylon 6/aramid fibres and preparation method for same | |
WO2006053492A1 (en) | The use of polyamide composite for preparing pump or valve | |
CN106243701A (en) | A kind of preparation method of high temperature resistant expansion composite environmental-friendly construction substrate | |
CN111961337A (en) | MC nylon/SiC @ SiO2Method for preparing composite material | |
CN104672770A (en) | Heat-resistant carbon fiber-reinforced polyformaldehyde composite material and preparation method thereof | |
CN105647103B (en) | A kind of improved polyoxymethylene composite and preparation method thereof |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
PB01 | Publication | ||
PB01 | Publication | ||
SE01 | Entry into force of request for substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
RJ01 | Rejection of invention patent application after publication |
Application publication date: 20211123 |
|
RJ01 | Rejection of invention patent application after publication |