CN108017906B - Modified nanotube/oil-containing cast nylon composite material - Google Patents
Modified nanotube/oil-containing cast nylon composite material Download PDFInfo
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- CN108017906B CN108017906B CN201810030788.9A CN201810030788A CN108017906B CN 108017906 B CN108017906 B CN 108017906B CN 201810030788 A CN201810030788 A CN 201810030788A CN 108017906 B CN108017906 B CN 108017906B
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- 239000002071 nanotube Substances 0.000 title claims abstract description 56
- 239000004677 Nylon Substances 0.000 title claims abstract description 37
- 229920001778 nylon Polymers 0.000 title claims abstract description 37
- 239000002131 composite material Substances 0.000 title claims abstract description 12
- JBKVHLHDHHXQEQ-UHFFFAOYSA-N epsilon-caprolactam Chemical compound O=C1CCCCCN1 JBKVHLHDHHXQEQ-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000004519 grease Substances 0.000 claims abstract description 20
- 230000001050 lubricating effect Effects 0.000 claims abstract description 17
- 238000010438 heat treatment Methods 0.000 claims abstract description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000000463 material Substances 0.000 claims abstract description 12
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 11
- 239000003607 modifier Substances 0.000 claims abstract description 11
- 238000000034 method Methods 0.000 claims abstract description 9
- 239000003054 catalyst Substances 0.000 claims abstract description 8
- 239000002253 acid Substances 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims abstract description 4
- 238000002844 melting Methods 0.000 claims abstract description 3
- 230000008018 melting Effects 0.000 claims abstract description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 18
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 16
- 239000003921 oil Substances 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- 238000001816 cooling Methods 0.000 claims description 8
- 239000004408 titanium dioxide Substances 0.000 claims description 8
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 claims description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 6
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 6
- WQDUMFSSJAZKTM-UHFFFAOYSA-N Sodium methoxide Chemical compound [Na+].[O-]C WQDUMFSSJAZKTM-UHFFFAOYSA-N 0.000 claims description 6
- 239000002199 base oil Substances 0.000 claims description 6
- 239000002041 carbon nanotube Substances 0.000 claims description 6
- 229910021393 carbon nanotube Inorganic materials 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 5
- HPTYUNKZVDYXLP-UHFFFAOYSA-N aluminum;trihydroxy(trihydroxysilyloxy)silane;hydrate Chemical compound O.[Al].[Al].O[Si](O)(O)O[Si](O)(O)O HPTYUNKZVDYXLP-UHFFFAOYSA-N 0.000 claims description 4
- FWDBOZPQNFPOLF-UHFFFAOYSA-N ethenyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)C=C FWDBOZPQNFPOLF-UHFFFAOYSA-N 0.000 claims description 4
- 229910052621 halloysite Inorganic materials 0.000 claims description 4
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 4
- 239000012153 distilled water Substances 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 239000010410 layer Substances 0.000 claims description 3
- MQWFLKHKWJMCEN-UHFFFAOYSA-N n'-[3-[dimethoxy(methyl)silyl]propyl]ethane-1,2-diamine Chemical compound CO[Si](C)(OC)CCCNCCN MQWFLKHKWJMCEN-UHFFFAOYSA-N 0.000 claims description 3
- 230000007935 neutral effect Effects 0.000 claims description 3
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims description 3
- 239000002620 silicon nanotube Substances 0.000 claims description 3
- 229910021430 silicon nanotube Inorganic materials 0.000 claims description 3
- 239000002356 single layer Substances 0.000 claims description 3
- 238000000967 suction filtration Methods 0.000 claims description 3
- UUEWCQRISZBELL-UHFFFAOYSA-N 3-trimethoxysilylpropane-1-thiol Chemical compound CO[Si](OC)(OC)CCCS UUEWCQRISZBELL-UHFFFAOYSA-N 0.000 claims description 2
- UPMLOUAZCHDJJD-UHFFFAOYSA-N 4,4'-Diphenylmethane Diisocyanate Chemical compound C1=CC(N=C=O)=CC=C1CC1=CC=C(N=C=O)C=C1 UPMLOUAZCHDJJD-UHFFFAOYSA-N 0.000 claims description 2
- 239000005057 Hexamethylene diisocyanate Substances 0.000 claims description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 2
- RRAMGCGOFNQTLD-UHFFFAOYSA-N hexamethylene diisocyanate Chemical compound O=C=NCCCCCCN=C=O RRAMGCGOFNQTLD-UHFFFAOYSA-N 0.000 claims description 2
- 229910052744 lithium Inorganic materials 0.000 claims description 2
- AYLRODJJLADBOB-QMMMGPOBSA-N methyl (2s)-2,6-diisocyanatohexanoate Chemical compound COC(=O)[C@@H](N=C=O)CCCCN=C=O AYLRODJJLADBOB-QMMMGPOBSA-N 0.000 claims description 2
- 229910052961 molybdenite Inorganic materials 0.000 claims description 2
- 229910052982 molybdenum disulfide Inorganic materials 0.000 claims description 2
- 239000000376 reactant Substances 0.000 claims description 2
- QDRKDTQENPPHOJ-UHFFFAOYSA-N sodium ethoxide Chemical compound [Na+].CC[O-] QDRKDTQENPPHOJ-UHFFFAOYSA-N 0.000 claims description 2
- 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 2
- BPSIOYPQMFLKFR-UHFFFAOYSA-N trimethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CO[Si](OC)(OC)CCCOCC1CO1 BPSIOYPQMFLKFR-UHFFFAOYSA-N 0.000 claims 1
- 238000002360 preparation method Methods 0.000 abstract description 3
- 230000000052 comparative effect Effects 0.000 description 7
- 238000006243 chemical reaction Methods 0.000 description 6
- 238000011056 performance test Methods 0.000 description 5
- 238000005299 abrasion Methods 0.000 description 4
- 238000005452 bending Methods 0.000 description 4
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical class [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 238000005266 casting Methods 0.000 description 3
- 230000006835 compression Effects 0.000 description 2
- 238000007906 compression Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 239000012943 hotmelt Substances 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 230000004913 activation Effects 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 239000010687 lubricating oil Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- HQYALQRYBUJWDH-UHFFFAOYSA-N trimethoxy(propyl)silane Chemical compound CCC[Si](OC)(OC)OC HQYALQRYBUJWDH-UHFFFAOYSA-N 0.000 description 1
- 238000009827 uniform distribution Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L77/00—Compositions of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Compositions of derivatives of such polymers
- C08L77/02—Polyamides derived from omega-amino carboxylic acids or from lactams thereof
-
- 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
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2237—Oxides; Hydroxides of metals of titanium
- C08K2003/2241—Titanium dioxide
-
- 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
Abstract
The invention relates to a modified nanotube/oil-containing cast nylon composite material. The material is prepared by the following method, and the preparation method comprises the following steps: (1) adding the nanotube into acid liquor, and performing ultrasonic stirring to obtain an activated nanotube; (2) adding the activated nanotube obtained in the previous step into ethanol, adding a silane coupling agent, and reacting for 1.0-8.0 hours to obtain a modified nanotube; (3) adding the modified nanotube into lubricating grease to obtain a modifier; wherein 0.1-8.0 g of lubricating grease is added to every 1g of modified nanotube; (4) and heating and melting caprolactam, adding a modifier and then adding a catalyst to obtain the cast nylon composite material. The cast nylon obtained by the invention has obviously improved tensile strength and elongation at break.
Description
Technical Field
The invention belongs to the technical field of polymer composite materials, and discloses a cast nylon composite material modified by a modified nanotube and lubricating grease.
Technical Field
The casting nylon is also called monomer casting nylon (MC nylon), hot-melt caprolactam monomer is cast into a preheated mould by using an alkaline catalyst and a cocatalyst, the hot-melt caprolactam monomer rapidly generates anion in-situ polymerization reaction in the mould, and the casting nylon product is obtained after cooling and demoulding. The cast nylon product has the advantages of simple process, large molecular weight, uniform distribution, wide use temperature, good mechanical property and the like. However, the existing common cast nylon also has the defects of poor low-temperature toughness, poor friction resistance and abrasion resistance, poor self-lubricating property and the like. In actual use, the friction performance is particularly important, a method for preparing the oil-containing cast nylon by adding lubricating grease is generally adopted in order to improve the friction resistance of the cast nylon material, but the mechanical property of the material is reduced due to the addition of the grease, so that the wider application of the cast nylon material is limited, and high-end products mainly depend on import. In order to improve the mechanical property of the cast nylon, a method of adding nano particles/tubes into the cast nylon for modification is also available, but although the mechanical strength is improved to a certain extent by adding the nano particles/tubes, the friction property cannot be improved to a high degree.
Disclosure of Invention
The invention provides a modified nanotube/oil-containing cast nylon composite material and a preparation method thereof, aiming at the defects of the prior art. The method adds the nanotube into the cast nylon, utilizes the lubricating grease and the modified nanotube to form a well-combined pipe network structure, and the two materials are uniformly dispersed in the cast nylon under the synergistic effect, so that the comprehensive performance of the mechanical property and the friction property of the prepared material is improved.
The technical scheme of the invention is as follows:
a modified nanotube/oil-containing cast nylon composite material is characterized in that the material is prepared by the following method, and the preparation method comprises the following steps:
(1) adding the nanotube into acid liquor, ultrasonically stirring for 0.5-1.0 h, washing with distilled water to be neutral, and performing suction filtration to obtain an activated nanotube; wherein, every 1g of the nanotube needs 100-150 ml of acid liquor, and the acid liquor is 1-2 mol/L hydrochloric acid solution;
(2) adding the activated nanotube obtained in the previous step into ethanol, adding a silane coupling agent, reacting for 1.0-8.0 hours at the temperature of 40-110 ℃, washing, centrifuging and drying to obtain a modified nanotube; wherein, every 1g of the nanotube is added with 100-200 ml of ethanol and 0.1-1.0 g of silane coupling agent;
(3) adding the modified nanotube into lubricating grease, and performing ultrasonic dispersion for 3-7 hours at the temperature of 80-130 ℃ to obtain a modifier; wherein 0.1-8.0 g of lubricating grease is added to every 1g of modified nanotube;
(4) heating caprolactam to 90-110 ℃ for melting, then heating to 120-140 ℃, adding the modifier obtained in the previous step, and reacting for 5-15 minutes under a reduced pressure condition; then cooling to 125-135 ℃, adding a catalyst, and reacting for 5-15 minutes under a reduced pressure condition; wherein 1.0-5.0 g of modifier is added to every 100g of caprolactam, and 0.1-0.9 g of catalyst is added to every 100g of caprolactam;
(5) heating the reactant obtained in the previous step to 135-145 ℃, adding a cocatalyst, mixing, pouring into a mold, keeping the temperature at 150-180 ℃ for 20-50 minutes, cooling, and demolding to obtain the cast nylon composite material; wherein, 0.1-1.0 g of cocatalyst is added into every 100g of caprolactam;
the nanotube is one or more of a single-layer carbon nanotube, a multi-layer carbon nanotube, a titanium dioxide nanotube, a halloysite nanotube and a silicon nanotube.
The lubricating oil or lubricating grease is methyl silicone oil, base oil, white special lubricating grease, bearing lubricating grease and MoS2One or more of lithium grease.
The silane coupling agent is specifically one or more of gamma-aminopropyltriethoxysilane (KH-550), gamma- (2, 3-glycidoxy) propyltrimethoxysilane (KH-560), gamma- (methacryloyloxy) propyltrimethoxysilane (KH-570), vinyltriethoxysilane (KH-151), gamma-mercaptopropyltrimethoxysilane (KH-580), and N- (β -aminoethyl) -gamma-aminopropylmethyldimethoxysilane (KH-602).
The catalyst is one or more of sodium hydroxide, potassium hydroxide, sodium methoxide and sodium ethoxide
The cocatalyst is one or more of toluene-2, 4-diisocyanate, hexamethylene diisocyanate, diphenylmethane diisocyanate and lysine diisocyanate.
The pressure in the step (4) under reduced pressure is preferably 0.8-0.9 MPa.
The invention has the beneficial effects that:
according to the invention, the modified nanotube and the lubricating grease are utilized to form a special pipe network structure, and the modified nanotube and the lubricating grease are uniformly distributed in the cast nylon, so that the tensile strength and the elongation at break of the modified nanotube are obviously improved, and the friction resistance and the wear resistance of the material are obviously improved compared with those of common oil-containing cast nylon. Compared with the common oil-containing cast nylon, the friction coefficient is reduced by 45%, the abrasion loss is reduced by 52%, the elongation at break is improved by 28%, the bending strength is improved by 35%, the bending modulus is improved by 24%, the compression strength is improved by 22%, and other properties are improved or leveled. Compared with the common cast nylon (comparative example 1), the performance of the cast nylon is improved for most parts.
Detailed Description
The present invention will be more fully described with reference to the following examples in order to facilitate the understanding of the invention, but the scope of the invention is not limited to the following specific examples.
The nanotube is specifically a single-layer carbon nanotube, a multi-layer carbon nanotube, a titanium dioxide nanotube, a halloysite nanotube or a silicon nanotube, which are commercially known materials and have the diameter of 2-20 nm.
Unless otherwise specified, the reagents and materials used in the present invention are commercially available or can be prepared by known methods.
Example 1
(1) Weighing 1g of titanium dioxide nanotube, adding the titanium dioxide nanotube into 150ml of 1mol/L hydrochloric acid solution, ultrasonically stirring for 1.0 hour, washing the titanium dioxide nanotube to be neutral by using distilled water, and performing suction filtration to obtain the nanotube after impurity removal and activation.
(2) Adding 1g of the titanium dioxide nanotube obtained in the previous step into 100ml of ethanol, adding 0.1g of gamma-aminopropyltriethoxysilane (KH-550) silane coupling agent, reacting for 6 hours at 75 ℃, washing, centrifuging and drying to obtain the modified titanium dioxide nanotube.
(3) Adding 1g of modified titanium dioxide nanotube into 7g of base oil, carrying out ultrasonic dispersion for 5 hours in an environment of 130 ℃, and finishing the ultrasonic dispersion to obtain the modifier formed by the modified titanium dioxide nanotube and the base oil.
(4) 100g of caprolactam is heated to 110 ℃ to melt, then the temperature is raised to 140 ℃, 1g of modifier is added, and the reaction is carried out for 15 minutes under the reduced pressure condition (the vacuum degree is 0.8MPa) to remove water. After the temperature was decreased to 125 deg.C, 0.3g of sodium hydroxide was added thereto, and the reaction was carried out under reduced pressure for 15 minutes (degree of vacuum 0.8MPa) to remove water.
(5) And (3) heating to 145 ℃, adding 0.2g of cocatalyst toluene-2.4-diisocyanate, uniformly mixing, pouring into a mold, keeping at 160 ℃ for 40 minutes, cooling, and demolding to obtain the cast nylon composite material.
Comparative example 1
(1) 100g of caprolactam are melted by heating to 110 ℃.
(2) And (3) carrying out reduced pressure reaction at 110 ℃ for 5-15 minutes (the vacuum degree is 0.8MPa) to remove water, heating to 125 ℃, adding 0.3g of sodium hydroxide, and carrying out reaction under the reduced pressure condition for 10 minutes to remove water (the vacuum degree is 0.8 MPa).
(3) Heating to 145 ℃, adding 0.2g of cocatalyst toluene-2.4-diisocyanate, uniformly mixing, pouring into a preheated mold, keeping at 160 ℃ for 40 minutes, and cooling and demolding to obtain the cast nylon product.
Comparative example 2
(1) 100g of caprolactam are melted by heating to 110 ℃.
(2) And (3) carrying out reduced pressure reaction at 110 ℃ for 5-15 minutes (the vacuum degree is 0.8MPa) to remove water, heating to 125 ℃, adding 0.3g of sodium hydroxide, and carrying out reduced pressure reaction (the vacuum degree is 0.8MPa) for 10 minutes to remove water. The temperature was raised to 140 ℃ and 1g of base oil was added.
(3) Heating to 145 ℃, adding 0.2g of cocatalyst toluene-2.4-diisocyanate, uniformly mixing, pouring into a preheated mold, keeping at 160 ℃ for 40 minutes, and cooling and demolding to obtain the cast nylon product.
The results of the performance test are shown in the attached Table 1
Attached table 1
As can be seen from the data in attached Table 1, the conventional oil-containing cast nylon (comparative example 2) has a certain friction coefficient lower than that of the conventional cast nylon (comparative example 1), but the abrasion loss is not reduced and the mechanical properties are all reduced to different degrees. Compared with the comparative example 2, the modified titanium dioxide nanotube/oil-containing cast nylon material (example 1) prepared by the invention has the advantages that the friction coefficient is reduced by 45%, the abrasion loss is reduced by 52%, the elongation at break is improved by 28%, the bending strength is improved by 35%, the bending modulus is improved by 24%, the compression strength is improved by 22%, and other properties are improved or leveled. Compared with the common cast nylon (comparative example 1), the performance of the cast nylon is improved for most parts.
Example 2
The other procedure was conducted in the same manner as in example 1 except that 0.1g of the gamma-aminopropyltriethoxysilane (KH-550) silane coupling agent in the step (2) was replaced with 0.2g of vinyltriethoxysilane (KH-151) silane coupling agent. The performance test results are similar to those of example 1.
Example 3
The other steps were carried out in the same manner as in example 1 except that 7g of the base oil in the step (3) was changed to 4g of methyl silicone oil and the temperature at which the modifier was added was changed from 140 ℃ to 135 ℃. The performance test results are similar to those of example 1.
Example 4
The other steps were conducted in the same manner as in example 1 except that 0.3g of sodium hydroxide in step (4) was changed to 0.25g of sodium methoxide. The performance test results are similar to those of example 1.
Example 5
The other steps are the same as example 1 except that 1g of the titanium dioxide nanotubes in step (1) are replaced by 1g of the halloysite nanotubes, and the amount of the silane coupling agent used in step (2) is changed from 0.1g to 0.15 g. The performance test is similar to that of example 1.
The invention is not the best known technology.
Claims (1)
1. A modified nanotube/oil-containing cast nylon composite material, characterized in that the material is prepared by a method comprising the steps of:
(1) adding the nanotube into acid liquor, ultrasonically stirring for 0.5-1.0 h, washing with distilled water to be neutral, and performing suction filtration to obtain an activated nanotube; wherein, every 1g of the nanotube needs 100-150 ml of acid liquor, and the acid liquor is 1-2 mol/L hydrochloric acid solution;
(2) adding the activated nanotube obtained in the previous step into ethanol, adding a silane coupling agent, reacting for 1.0-8.0 hours at the temperature of 40-110 ℃, washing, centrifuging and drying to obtain a modified nanotube; wherein, every 1g of the nanotube is added with 100-200 ml of ethanol and 0.1-1.0 g of silane coupling agent;
(3) adding the modified nanotube into lubricating grease, and performing ultrasonic dispersion for 3-7 hours at the temperature of 80-130 ℃ to obtain a modifier; wherein 0.1-8.0 g of lubricating grease is added to every 1g of modified nanotube;
(4) heating caprolactam to 90-110 ℃ for melting, then heating to 120-140 ℃, adding the modifier obtained in the previous step, and reacting for 5-15 minutes under a reduced pressure condition; then cooling to 125-135 ℃, adding a catalyst, and reacting for 5-15 minutes under a reduced pressure condition; wherein 1.0-5.0 g of modifier is added to every 100g of caprolactam, and 0.1-0.9 g of catalyst is added to every 100g of caprolactam;
(5) heating the reactant obtained in the previous step to 135-145 ℃, adding a cocatalyst, mixing, pouring into a mold, keeping the temperature at 150-180 ℃ for 20-50 minutes, cooling, and demolding to obtain the cast nylon composite material; wherein, 0.1-1.0 g of cocatalyst is added into every 100g of caprolactam;
the nano tube is one or more of a single-layer carbon nano tube, a multi-layer carbon nano tube, a titanium dioxide nano tube, a halloysite nano tube and a silicon nano tube;
the lubricating grease is methyl silicone oil, base oil, white special lubricating grease, bearing lubricating grease and MoS2One or more of lithium grease;
the silane coupling agent is one or more of gamma-aminopropyltriethoxysilane, gamma- (2, 3-epoxypropoxy) propyltrimethoxysilane, gamma- (methacryloyloxy) propyltrimethoxysilane, vinyl triethoxysilane, gamma-mercaptopropyltrimethoxysilane and N- (β -aminoethyl) -gamma-aminopropylmethyldimethoxysilane;
the catalyst is one or more of sodium hydroxide, potassium hydroxide, sodium methoxide and sodium ethoxide;
the cocatalyst is one or more of toluene-2, 4-diisocyanate, hexamethylene diisocyanate, diphenylmethane diisocyanate and lysine diisocyanate.
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| CN201810030788.9A CN108017906B (en) | 2018-01-12 | 2018-01-12 | Modified nanotube/oil-containing cast nylon composite material |
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| CN201810030788.9A CN108017906B (en) | 2018-01-12 | 2018-01-12 | Modified nanotube/oil-containing cast nylon composite material |
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| CN102153744B (en) * | 2011-02-23 | 2013-01-23 | 株洲时代新材料科技股份有限公司 | Preparation method of halloysite nanotube reinforced flame-retardant anionic polymerization nylon |
| CN102942694B (en) * | 2012-10-17 | 2014-09-17 | 河南科技大学 | Oil-filled monomer casting nylon composite material |
| CN103881144B (en) * | 2014-04-04 | 2016-05-11 | 中国热带农业科学院农产品加工研究所 | A kind of preparation method of rubber combined supporting material |
| CN105623243B (en) * | 2014-10-31 | 2019-01-08 | 徐工集团工程机械股份有限公司 | A kind of nylon composite materials and preparation method thereof |
| CN105418969B (en) * | 2015-12-04 | 2017-12-29 | 南昌航空大学 | A kind of preparation method of the carbon nanotube grafting carbon fiber reinforcement based on click chemistry |
| CN105860086B (en) * | 2016-03-30 | 2019-05-24 | 南昌航空大学 | A kind of preparation method of the grafted by super branched polymer carbon nanotube based on click chemistry |
| CN106497034B (en) * | 2016-11-14 | 2018-12-07 | 河北工业大学 | A kind of oil filled mc nylon/rare earth/graphene oxide composite material |
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2018
- 2018-01-12 CN CN201810030788.9A patent/CN108017906B/en not_active Expired - Fee Related
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