CN114031938A - High-temperature nylon and preparation method thereof - Google Patents
High-temperature nylon and preparation method thereof Download PDFInfo
- Publication number
- CN114031938A CN114031938A CN202111367583.8A CN202111367583A CN114031938A CN 114031938 A CN114031938 A CN 114031938A CN 202111367583 A CN202111367583 A CN 202111367583A CN 114031938 A CN114031938 A CN 114031938A
- Authority
- CN
- China
- Prior art keywords
- parts
- weight
- nylon
- stirring
- nanorods
- 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.)
- Granted
Links
- 239000004677 Nylon Substances 0.000 title claims abstract description 83
- 229920001778 nylon Polymers 0.000 title claims abstract description 83
- 238000002360 preparation method Methods 0.000 title claims abstract description 30
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 213
- 239000002073 nanorod Substances 0.000 claims abstract description 111
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 100
- 150000001875 compounds Chemical class 0.000 claims abstract description 40
- 229920001971 elastomer Polymers 0.000 claims abstract description 31
- 239000000806 elastomer Substances 0.000 claims abstract description 31
- 229920006111 poly(hexamethylene terephthalamide) Polymers 0.000 claims abstract description 27
- 239000003963 antioxidant agent Substances 0.000 claims abstract description 12
- 230000003078 antioxidant effect Effects 0.000 claims abstract description 12
- 239000002994 raw material Substances 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 9
- 230000008569 process Effects 0.000 claims abstract description 9
- 238000003756 stirring Methods 0.000 claims description 89
- 238000001035 drying Methods 0.000 claims description 44
- 235000012239 silicon dioxide Nutrition 0.000 claims description 31
- 238000005406 washing Methods 0.000 claims description 31
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 28
- 238000006243 chemical reaction Methods 0.000 claims description 21
- 238000002156 mixing Methods 0.000 claims description 14
- 238000001125 extrusion Methods 0.000 claims description 13
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 claims description 13
- 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 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 9
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 9
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 9
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 9
- DZGCGKFAPXFTNM-UHFFFAOYSA-N ethanol;hydron;chloride Chemical compound Cl.CCO DZGCGKFAPXFTNM-UHFFFAOYSA-N 0.000 claims description 9
- WTJKGGKOPKCXLL-RRHRGVEJSA-N phosphatidylcholine Chemical compound CCCCCCCCCCCCCCCC(=O)OC[C@H](COP([O-])(=O)OCC[N+](C)(C)C)OC(=O)CCCCCCCC=CCCCCCCCC WTJKGGKOPKCXLL-RRHRGVEJSA-N 0.000 claims description 9
- 229920001577 copolymer Polymers 0.000 claims description 8
- 239000000463 material Substances 0.000 claims description 8
- ROFVEXUMMXZLPA-UHFFFAOYSA-N Bipyridyl Chemical compound N1=CC=CC=C1C1=CC=CC=N1 ROFVEXUMMXZLPA-UHFFFAOYSA-N 0.000 claims description 7
- 238000007599 discharging Methods 0.000 claims description 7
- 238000005469 granulation Methods 0.000 claims description 7
- 230000003179 granulation Effects 0.000 claims description 7
- OETHQSJEHLVLGH-UHFFFAOYSA-N metformin hydrochloride Chemical compound Cl.CN(C)C(=N)N=C(N)N OETHQSJEHLVLGH-UHFFFAOYSA-N 0.000 claims description 7
- 229960004329 metformin hydrochloride Drugs 0.000 claims description 7
- XZWYZXLIPXDOLR-UHFFFAOYSA-N metformin hydrochloride Natural products CN(C)C(=N)NC(N)=N XZWYZXLIPXDOLR-UHFFFAOYSA-N 0.000 claims description 7
- UUEWCQRISZBELL-UHFFFAOYSA-N 3-trimethoxysilylpropane-1-thiol Chemical compound CO[Si](OC)(OC)CCCS UUEWCQRISZBELL-UHFFFAOYSA-N 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- GAODDBNJCKQQDY-UHFFFAOYSA-N 2-methyl-4,6-bis(octylsulfanylmethyl)phenol Chemical compound CCCCCCCCSCC1=CC(C)=C(O)C(CSCCCCCCCC)=C1 GAODDBNJCKQQDY-UHFFFAOYSA-N 0.000 claims description 2
- 229920002943 EPDM rubber Polymers 0.000 claims description 2
- FACXGONDLDSNOE-UHFFFAOYSA-N buta-1,3-diene;styrene Chemical class C=CC=C.C=CC1=CC=CC=C1.C=CC1=CC=CC=C1 FACXGONDLDSNOE-UHFFFAOYSA-N 0.000 claims description 2
- 229920000468 styrene butadiene styrene block copolymer Polymers 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 1
- 239000000126 substance Substances 0.000 abstract description 28
- 230000000694 effects Effects 0.000 abstract description 6
- 238000012360 testing method Methods 0.000 description 17
- 230000032683 aging Effects 0.000 description 16
- 239000011159 matrix material Substances 0.000 description 12
- 230000014759 maintenance of location Effects 0.000 description 10
- 238000004132 cross linking Methods 0.000 description 9
- 150000003839 salts Chemical class 0.000 description 9
- MPTQRFCYZCXJFQ-UHFFFAOYSA-L copper(II) chloride dihydrate Chemical compound O.O.[Cl-].[Cl-].[Cu+2] MPTQRFCYZCXJFQ-UHFFFAOYSA-L 0.000 description 8
- VZJJZMXEQNFTLL-UHFFFAOYSA-N chloro hypochlorite;zirconium;octahydrate Chemical compound O.O.O.O.O.O.O.O.[Zr].ClOCl VZJJZMXEQNFTLL-UHFFFAOYSA-N 0.000 description 7
- 229910052751 metal Inorganic materials 0.000 description 7
- 239000002184 metal Substances 0.000 description 7
- 239000000243 solution Substances 0.000 description 7
- 230000007797 corrosion Effects 0.000 description 6
- 238000005260 corrosion Methods 0.000 description 6
- 239000002539 nanocarrier Substances 0.000 description 6
- 230000035484 reaction time Effects 0.000 description 6
- 229910052710 silicon Inorganic materials 0.000 description 6
- 239000010703 silicon Substances 0.000 description 6
- 239000004952 Polyamide Substances 0.000 description 5
- 238000007605 air drying Methods 0.000 description 5
- 239000001257 hydrogen Substances 0.000 description 5
- 229910052739 hydrogen Inorganic materials 0.000 description 5
- 230000004048 modification Effects 0.000 description 5
- 238000012986 modification Methods 0.000 description 5
- 229920002647 polyamide Polymers 0.000 description 5
- 229920000642 polymer Polymers 0.000 description 5
- 238000003379 elimination reaction Methods 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 239000011259 mixed solution Substances 0.000 description 4
- 230000001590 oxidative effect Effects 0.000 description 4
- 239000004033 plastic Substances 0.000 description 4
- 229920003023 plastic Polymers 0.000 description 4
- 239000002244 precipitate Substances 0.000 description 4
- 238000010992 reflux Methods 0.000 description 4
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- 229920003231 aliphatic polyamide Polymers 0.000 description 3
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 3
- 125000000956 methoxy group Chemical group [H]C([H])([H])O* 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000011148 porous material Substances 0.000 description 3
- 125000003396 thiol group Chemical group [H]S* 0.000 description 3
- 239000004953 Aliphatic polyamide Substances 0.000 description 2
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 description 2
- 239000004760 aramid Substances 0.000 description 2
- 229920003235 aromatic polyamide Polymers 0.000 description 2
- 125000003118 aryl group Chemical group 0.000 description 2
- 239000012752 auxiliary agent Substances 0.000 description 2
- 230000004888 barrier function Effects 0.000 description 2
- 229910001431 copper ion Inorganic materials 0.000 description 2
- 239000007822 coupling agent Substances 0.000 description 2
- 239000003000 extruded plastic Substances 0.000 description 2
- 238000002347 injection Methods 0.000 description 2
- 239000007924 injection Substances 0.000 description 2
- 230000003993 interaction Effects 0.000 description 2
- 239000003446 ligand Substances 0.000 description 2
- 229910021645 metal ion Inorganic materials 0.000 description 2
- 230000005012 migration Effects 0.000 description 2
- 238000013508 migration Methods 0.000 description 2
- 239000002991 molded plastic Substances 0.000 description 2
- 239000000178 monomer Substances 0.000 description 2
- 229920006115 poly(dodecamethylene terephthalamide) Polymers 0.000 description 2
- 230000001681 protective effect Effects 0.000 description 2
- 230000009257 reactivity Effects 0.000 description 2
- 229920006012 semi-aromatic polyamide Polymers 0.000 description 2
- 238000002444 silanisation Methods 0.000 description 2
- 230000002195 synergetic effect Effects 0.000 description 2
- 238000009864 tensile test Methods 0.000 description 2
- 229910052726 zirconium Inorganic materials 0.000 description 2
- -1 zirconium ions Chemical class 0.000 description 2
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical group C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 1
- 239000006087 Silane Coupling Agent Substances 0.000 description 1
- 229920000147 Styrene maleic anhydride Polymers 0.000 description 1
- 230000006750 UV protection Effects 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 125000003368 amide group Chemical group 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000007385 chemical modification Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000000536 complexating effect Effects 0.000 description 1
- 238000007334 copolymerization reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 150000004985 diamines Chemical class 0.000 description 1
- 238000010292 electrical insulation Methods 0.000 description 1
- 230000008030 elimination Effects 0.000 description 1
- 229920006351 engineering plastic Polymers 0.000 description 1
- 239000012760 heat stabilizer Substances 0.000 description 1
- 125000000879 imine group Chemical group 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 239000005543 nano-size silicon particle Substances 0.000 description 1
- 125000004433 nitrogen atom Chemical group N* 0.000 description 1
- 229920006119 nylon 10T Polymers 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 229920006128 poly(nonamethylene terephthalamide) Polymers 0.000 description 1
- 229920000768 polyamine Polymers 0.000 description 1
- 238000006068 polycondensation reaction Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000000758 substrate Substances 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
- C08L77/06—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
- C08K2201/011—Nanostructured additives
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention relates to the technical field of nylon preparation, and particularly discloses high-temperature nylon and a preparation method thereof. The high-temperature nylon is prepared from the following raw materials in parts by weight: 35-50 parts of nylon 6T, 35-50 parts of nylon 12T, 10-20 parts of elastomer, 0.5-1.5 parts of antioxidant and 3-8 parts of functionalized mesoporous silica nano-rod. The functional compound is loaded on the mesoporous silica nanorods and then is blended and modified with nylon, so that the preparation method is simple in process and remarkable in effect, and the prepared high-temperature nylon has thermal-oxidative-aging resistance and chemical resistance and has a good market prospect.
Description
Technical Field
The invention relates to the technical field of nylon preparation, in particular to high-temperature nylon and a preparation method thereof.
Background
The polyamide is commonly called nylon and is a general name of a high polymer which contains amide groups in a macromolecular main chain repeating structure and can form a certain hydrogen bond density. In plastic applications, the plastic has become the most widely used engineering plastic with the largest amount due to its excellent physical and mechanical properties, electrical insulation properties, oil resistance, wear resistance, solvent resistance, corrosion resistance, self-lubricity, and other characteristics. Polyamides can be classified into aliphatic polyamides, wholly aromatic polyamides and semi-aromatic polyamides according to the monomer composition. The semi-aromatic polyamide is polyamide which is formed by polycondensation of raw material dibasic acid or diamine monomer containing aromatic rings under certain reaction conditions, the molecular main chain has aromatic rings with good heat resistance and can form hydrogen bonds, so that the advantages of wholly aromatic polyamide and aliphatic polyamide are combined, the polyamide has excellent thermal property, rigidity, chemical resistance, dimensional stability and good processability, main products comprise PA6T, PA9T, PA10T, PA12T and the like, and the polyamide is widely applied to the fields of automobiles, packaging industry, sports equipment, electronics industry, aviation and the like at present.
Chinese patent 201410789880.5 discloses a high-fluidity high-temperature nylon and a preparation method thereof, wherein the high-fluidity high-temperature nylon is prepared by copolymerizing 30-85 wt% of high-temperature nylon salt, 10-50 wt% of aliphatic nylon salt, 1-15 wt% of polyamine, 0.4-20 wt% of auxiliary agent and 1-25 wt% of water, and the auxiliary agent comprises 0.1-5 wt% of heat stabilizer, 0.1-5 wt% of antioxidant, 0.1-5 wt% of end capping agent and 0.1-5 wt% of catalyst. The application adopts copolymerization to modify high-temperature nylon, belongs to chemical modification, and the performance of the prepared modified nylon is more stable than that of modified nylon obtained by physical modification. But the high-temperature nylon has single performance and is difficult to meet diversified market demands, so that the research on the high-temperature nylon with excellent comprehensive performance has important significance.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides high-temperature nylon and a preparation method thereof.
In order to solve the technical problems, the invention adopts the technical scheme that:
the high-temperature nylon is prepared from the following raw materials: nylon 6T, nylon 12T, an elastomer, an antioxidant and a functionalized mesoporous silica nanorod.
The high-temperature nylon is prepared from the following raw materials in parts by weight: 35-50 parts of nylon 6T, 35-50 parts of nylon 12T, 10-20 parts of elastomer, 0.5-1.5 parts of antioxidant and 3-8 parts of functionalized mesoporous silica nano-rod.
The elastomer is any one of maleic anhydride grafted ethylene-octene copolymer, maleic anhydride grafted hydrogenated styrene-butadiene-styrene triblock copolymer and maleic anhydride grafted ethylene propylene diene monomer.
The antioxidant is any one of antioxidant 1098, antioxidant KY2468 and antioxidant 1520.
The nano silicon dioxide can penetrate into the vicinity of a double bond of a high molecular compound due to the volume effect and the quantum tunnel effect and is overlapped with an electron cloud to form a space network structure, so that the mechanical strength, toughness, wear resistance, ageing resistance, ultraviolet resistance and other properties of the high molecular material are greatly improved. The mesoporous silica nanorods with the pore structures are often used as excellent nano-carriers for adsorption and continuous release of active molecules due to the advantages of adjustable pore diameters, controllable morphology, ordered pore channels, large specific surface area, easy modification of the surface and the like.
The preparation method of the functionalized mesoporous silica nanorod comprises the following steps:
s1, adding 3-5 parts by weight of hexadecyl trimethyl ammonium bromide into 20-30 parts by weight of water, uniformly dispersing by ultrasonic, adding 0.3-0.5 part by weight of phosphatidylcholine, stirring at the room temperature at the rotation speed of 1000-1500rpm for 20-40min, then adding 20-30 parts by weight of 20-30 wt% ammonia water, continuously stirring for 1-3h, then adding 10-20 parts by weight of tetraethyl orthosilicate, continuously stirring for 3-5h, and after the stirring is finished, centrifuging, washing and drying to obtain silicon dioxide nanorods;
s2, adding all the silicon dioxide nanorods obtained in the step S1 into 40-60 parts by weight of 10-15% hydrochloric acid ethanol solution, stirring and reacting at 70-80 ℃ at the rotating speed of 400-800rpm for 8-16h, and centrifuging, washing and drying after the reaction is finished to obtain mesoporous silicon dioxide nanorods;
s3, adding 4-6 parts by weight of functional compound into 15-30 parts by weight of acetone, stirring at the rotation speed of 1200-1800rpm for 20-40min at room temperature, then adding all the mesoporous silica nanorods obtained in the step S2, continuously stirring for 12-24h, centrifuging after finishing stirring, washing, and drying to obtain the functionalized mesoporous silica nanorods.
Further, the preparation method of the functionalized mesoporous silica nanorod comprises the following steps:
s1, adding 3-5 parts by weight of hexadecyl trimethyl ammonium bromide into 20-30 parts by weight of water, uniformly dispersing by ultrasonic, adding 0.3-0.5 part by weight of phosphatidylcholine, stirring at the room temperature at the rotation speed of 1000-1500rpm for 20-40min, then adding 20-30 parts by weight of 20-30 wt% ammonia water, continuously stirring for 1-3h, then adding 10-20 parts by weight of tetraethyl orthosilicate, continuously stirring for 3-5h, and after the stirring is finished, centrifuging, washing and drying to obtain silicon dioxide nanorods;
s2, adding 6-10 parts by weight of (3-mercaptopropyl) trimethoxysilane into 310 parts by weight of 250-310 parts by weight of anhydrous ethanol, stirring at the rotation speed of 1000-1500rpm at room temperature for 10-20min, then adding all the silica nanorods obtained in the step S1, stirring at the rotation speed of 300-600rpm at the temperature of 65-75 ℃ for reaction for 8-15h, centrifuging after the reaction is finished, washing, and drying to obtain modified silica nanorods;
s3, adding all the modified silicon dioxide nanorods obtained in the step S2 into 40-60 parts by weight of 10-15% hydrochloric acid ethanol solution, stirring and reacting at 70-80 ℃ at the rotating speed of 400-800rpm for 8-16h, and centrifuging, washing and drying after the reaction is finished to obtain the modified mesoporous silicon dioxide nanorods;
s4, adding 4-6 parts by weight of functional compound into 15-30 parts by weight of acetone, stirring at the rotation speed of 1200-1800rpm for 20-40min at room temperature, then adding all the modified mesoporous silica nanorods obtained in the step S3, continuously stirring for 12-24h, and centrifuging, washing and drying after the stirring is finished to obtain the functionalized mesoporous silica nanorods.
According to the invention, (3-mercaptopropyl) trimethoxysilane is adopted to modify the silicon dioxide nanorods, and methoxy groups in a silane coupling agent and silicon hydroxyl hydrogen on the surfaces of the silicon dioxide nanorods are subjected to elimination reaction to form firm chemical bonds, so that mercapto functional groups are connected to the surfaces of the silicon dioxide nanorods in a chemical bonding manner, and an active center is provided for the combination of functional compounds; meanwhile, along with the elimination of silicon hydroxyl on the surface of the silicon dioxide nanorod, the interface compatibility between the nano-carrier and the polymer matrix is also improved, so that the dispersibility of the silicon dioxide nanorod in the matrix is improved.
The preparation method of the functional compound comprises the following steps: adding 1-3 parts by weight of metformin hydrochloride and 1-3 parts by weight of 2, 2-bipyridine into 50-80 parts by weight of acetone, stirring at the rotation speed of 1000rpm of 600-.
The metal salt is a mixture of copper chloride dihydrate and zirconium oxychloride octahydrate, wherein the mass ratio of the copper chloride dihydrate to the zirconium oxychloride octahydrate is 1 (1-3).
According to the invention, metformin hydrochloride and 2, 2-bipyridine are used as bidentate ligands, two nitrogen atoms of an imine group and a pyridine ring group are respectively used as coordination sites to coordinate with metal ions to form a functional compound, the functional compound can increase the density of chemical bonds and form an excellent protective barrier through chemical interaction and binding affinity between a molecular active part and a nano carrier-modified mesoporous silica nanorod, and a compact cross-linked network is formed between polymer matrixes, so that the nylon performance is improved.
The copper chloride dihydrate and the zirconium oxychloride octahydrate are compounded to serve as the metal salt, and the reason is that the compound formed by the zirconium ions with the octahedral structure with high atomic weight has higher chemical reactivity, so that the binding effect between the functional compound and the modified mesoporous silica nanorods is enhanced, and the crosslinking strength is improved; the compound formed by copper ions with a distorted octahedral structure with high-efficiency dipole moment has high electron affinity, occupies partial mesoporous channels of the silicon dioxide nanorods, increases the chemical bond density, reduces free volume crosslinking, and induces the crosslinking strength in the matrix; the two have synergistic effect, and the crosslinking strength of the matrix is improved together, so that the chemical resistance of the nylon is improved. In addition, according to the Mark triangle principle of the classic aging of macromolecules, the introduction of a crosslinking structure can improve the aging resistance of a system.
The preparation method of the high-temperature nylon comprises the following steps:
drying nylon 6T, nylon 12T and the elastomer in a blast drying oven at 75-85 ℃ for 8-15h according to the formula, then adding the nylon 6T, the nylon 12T, the elastomer, the antioxidant and the functionalized mesoporous silica nanorods into an internal mixer for internal mixing, discharging the internal mixed materials into a screw extruder, and carrying out melt blending extrusion granulation to obtain the high-temperature nylon.
The banburying temperature of the banbury mixer is 295-315 ℃, and the banburying reaction time is 8-12 min.
The extrusion process conditions of the screw extruder are that the first zone is 275-285 ℃, the second zone is 295-305 ℃, the third zone is 315-325 ℃, the fourth zone is 315-325 ℃, the fifth zone is 315-325 ℃, and the rotation speed of the screw is 40-50 r/min.
The invention has the following advantages:
1. according to the invention, the mesoporous silica nanorods are used as a nano-carrier, and then the functional compound is loaded on the mesoporous silica nanorods, so that the migration of functional compound molecules in a matrix is effectively limited, and the continuous release of effective active molecules in the functional compound is realized.
2. When the mesoporous silica nanorod is prepared, the silica nanorod is subjected to silanization modification, on one hand, the methoxy group in the coupling agent and the silicon hydroxyl hydrogen on the surface of the silica nanorod are subjected to elimination reaction to form a firm chemical bond, so that a mercapto functional group is connected to the surface of the silica nanorod in a chemical bonding manner, and an effective reaction active center is provided for the combination of functional compounds; on the other hand, the silicon hydroxyl content on the surface of the silicon dioxide nano rod is improved, and the interface compatibility between the nano carrier and the polymer matrix is also improved, so that the dispersibility of the carrier in the matrix is improved, and the performance is promoted to be improved.
3. The functional compound prepared by complexing the coordination site of the bidentate ligand and metal ions is adopted during the functional modification of the mesoporous silica nanorod, the density of chemical bonds is increased and an excellent protective barrier is formed through the chemical interaction and the binding affinity between the molecular active part and the nano carrier-modified mesoporous silica nanorod, and a compact cross-linked network is formed between high molecular substrates, so that the chemical resistance and the aging resistance of nylon are improved.
4. The functional compound is loaded on the mesoporous silica nanorods to prepare the functionalized mesoporous silica nanorods, and then the functionalized mesoporous silica nanorods are blended and modified with nylon, so that the preparation method is simple in process and remarkable in effect, and the prepared high-temperature nylon has thermal-oxidative-aging resistance and chemical resistance and has good market prospect.
Detailed Description
The above summary of the present invention is described in further detail below with reference to specific embodiments, but it should not be understood that the scope of the above subject matter of the present invention is limited to the following examples.
Introduction of some raw materials in this application:
nylon 6T, abbreviated PA6T, model: C430N, supplied by mitsui chemical company, japan.
Nylon 12T, abbreviated PA12T, model: NC010, supplied by dupont, usa.
Maleic anhydride grafted ethylene-octene copolymer, grade: GR216, graft maleic anhydride content: 0.5-1%, tensile strength at break: 9MPa, elongation at break: 1000%, supplied by dow corporation, usa.
Example 1
The high-temperature nylon is prepared from the following raw materials in parts by weight: 40 parts of nylon 6T, 40 parts of nylon 12T, 14 parts of elastomer, 1 part of antioxidant 1098 and 5 parts of mesoporous silica nanorods.
The elastomer is a maleic anhydride grafted ethylene-octene copolymer.
The preparation method of the mesoporous silica nanorod comprises the following steps:
s1, adding 3.5 parts by weight of hexadecyl trimethyl ammonium bromide into 25 parts by weight of water, uniformly dispersing by ultrasonic, adding 0.4 part by weight of phosphatidylcholine, stirring at room temperature at the rotating speed of 1200rpm for 30min, then adding 25 parts by weight of 25 wt% ammonia water, continuing stirring for 2h, then adding 15 parts by weight of tetraethyl orthosilicate, continuing stirring for 4h, and after the stirring is finished, centrifuging, washing and drying to obtain a silicon dioxide nanorod;
s2, adding all the silicon dioxide nanorods obtained in the step S1 into 50 parts by weight of hydrochloric acid ethanol solution with volume fraction of 13%, stirring and reacting at 75 ℃ for 12 hours at the rotating speed of 500rpm, centrifuging after the reaction is finished, washing, and drying to obtain the mesoporous silicon dioxide nanorods.
The preparation method of the high-temperature nylon comprises the following steps:
drying nylon 6T, nylon 12T and the elastomer in an air drying oven at 80 ℃ for 12 hours according to the formula, then adding the nylon 6T, the nylon 12T, the elastomer, the antioxidant 1098 and the mesoporous silica nanorods into an internal mixer for internal mixing, discharging the internally mixed materials into a screw extruder, and carrying out melt blending extrusion granulation to obtain the high-temperature nylon.
The banburying temperature of the banbury mixer is 305 ℃, and the banburying reaction time is 10 min.
The extrusion process conditions of the screw extruder are that the first zone is 280 ℃, the second zone is 300 ℃, the third zone is 320 ℃, the fourth zone is 320 ℃, the fifth zone is 320 ℃, and the rotating speed of the screw is 46 r/min.
Example 2
The high-temperature nylon is prepared from the following raw materials in parts by weight: 40 parts of nylon 6T, 40 parts of nylon 12T, 14 parts of elastomer, 1 part of antioxidant 1098 and 5 parts of functionalized mesoporous silica nanorods.
The elastomer is a maleic anhydride grafted ethylene-octene copolymer.
The preparation method of the functionalized mesoporous silica nanorod comprises the following steps:
s1, adding 3.5 parts by weight of hexadecyl trimethyl ammonium bromide into 25 parts by weight of water, uniformly dispersing by ultrasonic, adding 0.4 part by weight of phosphatidylcholine, stirring at room temperature at the rotating speed of 1200rpm for 30min, then adding 25 parts by weight of 25 wt% ammonia water, continuing stirring for 2h, then adding 15 parts by weight of tetraethyl orthosilicate, continuing stirring for 4h, and after the stirring is finished, centrifuging, washing and drying to obtain a silicon dioxide nanorod;
s2, adding all the modified silica nanorods obtained in the step S1 into 50 parts by weight of 13% hydrochloric acid ethanol solution, stirring and reacting at 75 ℃ for 12 hours at a rotating speed of 500rpm, and centrifuging, washing and drying after the reaction is finished to obtain mesoporous silica nanorods;
s3, adding 5 parts by weight of functional compound into 20 parts by weight of acetone, stirring at the room temperature at the rotating speed of 1500rpm for 30min, then adding all the mesoporous silica nanorods obtained in the step S2, continuing stirring for 18h, and after the stirring is finished, centrifuging, washing and drying to obtain the functionalized mesoporous silica nanorods.
The preparation method of the functional compound comprises the following steps: adding 2 parts by weight of metformin hydrochloride and 1.6 parts by weight of 2, 2-bipyridine into 70 parts by weight of acetone, stirring at the rotating speed of 800rpm for 20min, adding 5 parts by weight of copper chloride dihydrate, continuing stirring for 10min, heating and refluxing at 50 ℃ for 2h, finally centrifuging the obtained mixed solution, taking the bottom precipitate, and drying to obtain the functional compound.
The preparation method of the high-temperature nylon comprises the following steps:
drying nylon 6T, nylon 12T and the elastomer in an air drying oven at 80 ℃ for 12 hours according to the formula, then adding the nylon 6T, the nylon 12T, the elastomer, the antioxidant 1098 and the functionalized mesoporous silica nanorods into an internal mixer for internal mixing, discharging the internally mixed materials into a screw extruder, and carrying out melt blending extrusion granulation to obtain the high-temperature nylon.
The banburying temperature of the banbury mixer is 305 ℃, and the banburying reaction time is 10 min.
The extrusion process conditions of the screw extruder are that the first zone is 280 ℃, the second zone is 300 ℃, the third zone is 320 ℃, the fourth zone is 320 ℃, the fifth zone is 320 ℃, and the rotating speed of the screw is 46 r/min.
Example 3
The high-temperature nylon is prepared from the following raw materials in parts by weight: 40 parts of nylon 6T, 40 parts of nylon 12T, 14 parts of elastomer, 1 part of antioxidant 1098 and 5 parts of functionalized mesoporous silica nanorods.
The elastomer is a maleic anhydride grafted ethylene-octene copolymer.
The preparation method of the functionalized mesoporous silica nanorod comprises the following steps:
s1, adding 3.5 parts by weight of hexadecyl trimethyl ammonium bromide into 25 parts by weight of water, uniformly dispersing by ultrasonic, adding 0.4 part by weight of phosphatidylcholine, stirring at room temperature at the rotating speed of 1200rpm for 30min, then adding 25 parts by weight of 25 wt% ammonia water, continuing stirring for 2h, then adding 15 parts by weight of tetraethyl orthosilicate, continuing stirring for 4h, and after the stirring is finished, centrifuging, washing and drying to obtain a silicon dioxide nanorod;
s2, adding 7.5 parts by weight of (3-mercaptopropyl) trimethoxysilane into 300 parts by weight of absolute ethyl alcohol, stirring at the rotating speed of 1200rpm for 15min at room temperature, then adding all the silica nanorods obtained in the step S1, stirring at the rotating speed of 500rpm at the temperature of 70 ℃ for reaction for 12h, and after the reaction is finished, centrifuging, washing and drying to obtain modified silica nanorods;
s3, adding all the modified silicon dioxide nanorods obtained in the step S2 into 50 parts by weight of hydrochloric acid ethanol solution with volume fraction of 13%, stirring and reacting at 75 ℃ for 12 hours at a rotating speed of 500rpm, centrifuging, washing and drying after the reaction is finished, so as to obtain modified mesoporous silicon dioxide nanorods;
s4, adding 5 parts by weight of functional compound into 20 parts by weight of acetone, stirring at the room temperature at the rotating speed of 1500rpm for 30min, then adding all the modified mesoporous silica nanorods obtained in the step S3, continuing stirring for 18h, and after the stirring is finished, centrifuging, washing and drying to obtain the functionalized mesoporous silica nanorods.
The preparation method of the functional compound comprises the following steps: adding 2 parts by weight of metformin hydrochloride and 1.6 parts by weight of 2, 2-bipyridine into 70 parts by weight of acetone, stirring at the rotating speed of 800rpm for 20min, adding 5 parts by weight of copper chloride dihydrate, continuing stirring for 10min, heating and refluxing at 50 ℃ for 2h, finally centrifuging the obtained mixed solution, taking the bottom precipitate, and drying to obtain the functional compound.
The preparation method of the high-temperature nylon comprises the following steps:
drying nylon 6T, nylon 12T and the elastomer in an air drying oven at 80 ℃ for 12 hours according to the formula, then adding the nylon 6T, the nylon 12T, the elastomer, the antioxidant 1098 and the functionalized mesoporous silica nanorods into an internal mixer for internal mixing, discharging the internally mixed materials into a screw extruder, and carrying out melt blending extrusion granulation to obtain the high-temperature nylon.
The banburying temperature of the banbury mixer is 305 ℃, and the banburying reaction time is 10 min.
The extrusion process conditions of the screw extruder are that the first zone is 280 ℃, the second zone is 300 ℃, the third zone is 320 ℃, the fourth zone is 320 ℃, the fifth zone is 320 ℃, and the rotating speed of the screw is 46 r/min.
Example 4
The high-temperature nylon is prepared from the following raw materials in parts by weight: 40 parts of nylon 6T, 40 parts of nylon 12T, 14 parts of elastomer, 1 part of antioxidant 1098 and 5 parts of functionalized mesoporous silica nanorods.
The elastomer is a maleic anhydride grafted ethylene-octene copolymer.
The preparation method of the functionalized mesoporous silica nanorod comprises the following steps:
s1, adding 3.5 parts by weight of hexadecyl trimethyl ammonium bromide into 25 parts by weight of water, uniformly dispersing by ultrasonic, adding 0.4 part by weight of phosphatidylcholine, stirring at room temperature at the rotating speed of 1200rpm for 30min, then adding 25 parts by weight of 25 wt% ammonia water, continuing stirring for 2h, then adding 15 parts by weight of tetraethyl orthosilicate, continuing stirring for 4h, and after the stirring is finished, centrifuging, washing and drying to obtain a silicon dioxide nanorod;
s2, adding 7.5 parts by weight of (3-mercaptopropyl) trimethoxysilane into 300 parts by weight of absolute ethyl alcohol, stirring at the rotating speed of 1200rpm for 15min at room temperature, then adding all the silica nanorods obtained in the step S1, stirring at the rotating speed of 500rpm at the temperature of 70 ℃ for reaction for 12h, and after the reaction is finished, centrifuging, washing and drying to obtain modified silica nanorods;
s3, adding all the modified silicon dioxide nanorods obtained in the step S2 into 50 parts by weight of hydrochloric acid ethanol solution with volume fraction of 13%, stirring and reacting at 75 ℃ for 12 hours at a rotating speed of 500rpm, centrifuging, washing and drying after the reaction is finished, so as to obtain modified mesoporous silicon dioxide nanorods;
s4, adding 5 parts by weight of functional compound into 20 parts by weight of acetone, stirring at the room temperature at the rotating speed of 1500rpm for 30min, then adding all the modified mesoporous silica nanorods obtained in the step S3, continuing stirring for 18h, and after the stirring is finished, centrifuging, washing and drying to obtain the functionalized mesoporous silica nanorods.
The preparation method of the functional compound comprises the following steps: adding 2 parts by weight of metformin hydrochloride and 1.6 parts by weight of 2, 2-bipyridine into 70 parts by weight of acetone, stirring at the rotating speed of 800rpm for 20min, adding 5 parts by weight of zirconium oxychloride octahydrate, continuing stirring for 10min, heating and refluxing at 50 ℃ for 2h, finally centrifuging the obtained mixed solution, taking the bottom precipitate, and drying to obtain the functional compound.
The preparation method of the high-temperature nylon comprises the following steps:
drying nylon 6T, nylon 12T and the elastomer in an air drying oven at 80 ℃ for 12 hours according to the formula, then adding the nylon 6T, the nylon 12T, the elastomer, the antioxidant 1098 and the functionalized mesoporous silica nanorods into an internal mixer for internal mixing, discharging the internally mixed materials into a screw extruder, and carrying out melt blending extrusion granulation to obtain the high-temperature nylon.
The banburying temperature of the banbury mixer is 305 ℃, and the banburying reaction time is 10 min.
The extrusion process conditions of the screw extruder are that the first zone is 280 ℃, the second zone is 300 ℃, the third zone is 320 ℃, the fourth zone is 320 ℃, the fifth zone is 320 ℃, and the rotating speed of the screw is 46 r/min.
Example 5
The high-temperature nylon is prepared from the following raw materials in parts by weight: 40 parts of nylon 6T, 40 parts of nylon 12T, 14 parts of elastomer, 1 part of antioxidant 1098 and 5 parts of functionalized mesoporous silica nanorods.
The elastomer is a maleic anhydride grafted ethylene-octene copolymer.
The preparation method of the functionalized mesoporous silica nanorod comprises the following steps:
s1, adding 3.5 parts by weight of hexadecyl trimethyl ammonium bromide into 25 parts by weight of water, uniformly dispersing by ultrasonic, adding 0.4 part by weight of phosphatidylcholine, stirring at room temperature at the rotating speed of 1200rpm for 30min, then adding 25 parts by weight of 25 wt% ammonia water, continuing stirring for 2h, then adding 15 parts by weight of tetraethyl orthosilicate, continuing stirring for 4h, and after the stirring is finished, centrifuging, washing and drying to obtain a silicon dioxide nanorod;
s2, adding 7.5 parts by weight of (3-mercaptopropyl) trimethoxysilane into 300 parts by weight of absolute ethyl alcohol, stirring at the rotating speed of 1200rpm for 15min at room temperature, then adding all the silica nanorods obtained in the step S1, stirring at the rotating speed of 500rpm at the temperature of 70 ℃ for reaction for 12h, and after the reaction is finished, centrifuging, washing and drying to obtain modified silica nanorods;
s3, adding all the modified silicon dioxide nanorods obtained in the step S2 into 50 parts by weight of hydrochloric acid ethanol solution with volume fraction of 13%, stirring and reacting at 75 ℃ for 12 hours at a rotating speed of 500rpm, centrifuging, washing and drying after the reaction is finished, so as to obtain modified mesoporous silicon dioxide nanorods;
s4, adding 5 parts by weight of functional compound into 20 parts by weight of acetone, stirring at the room temperature at the rotating speed of 1500rpm for 30min, then adding all the modified mesoporous silica nanorods obtained in the step S3, continuing stirring for 18h, and after the stirring is finished, centrifuging, washing and drying to obtain the functionalized mesoporous silica nanorods.
The preparation method of the functional compound comprises the following steps: adding 2 parts by weight of metformin hydrochloride and 1.6 parts by weight of 2, 2-bipyridine into 70 parts by weight of acetone, stirring at the rotating speed of 800rpm for 20min, adding 5 parts by weight of metal salt, continuing stirring for 10min, heating and refluxing at 50 ℃ for 2h, finally centrifuging the obtained mixed solution, taking the bottom precipitate, and drying to obtain the functional compound.
The metal salt is a mixture of copper chloride dihydrate and zirconium oxychloride octahydrate, wherein the mass ratio of the copper chloride dihydrate to the zirconium oxychloride octahydrate is 1: 2.
The preparation method of the high-temperature nylon comprises the following steps:
drying nylon 6T, nylon 12T and the elastomer in an air drying oven at 80 ℃ for 12 hours according to the formula, then adding the nylon 6T, the nylon 12T, the elastomer, the antioxidant 1098 and the functionalized mesoporous silica nanorods into an internal mixer for internal mixing, discharging the internally mixed materials into a screw extruder, and carrying out melt blending extrusion granulation to obtain the high-temperature nylon.
The banburying temperature of the banbury mixer is 305 ℃, and the banburying reaction time is 10 min.
The extrusion process conditions of the screw extruder are that the first zone is 280 ℃, the second zone is 300 ℃, the third zone is 320 ℃, the fourth zone is 320 ℃, the fifth zone is 320 ℃, and the rotating speed of the screw is 46 r/min.
Test example 1
And (3) testing thermal oxidation aging resistance: determination of tensile Properties of plastics according to the national Standard GB/T1040.2-2006 part 2: test conditions for molded and extruded plastics A CMT-5104 type universal tester was used to test the tensile properties of test specimens before and after thermo-oxidative ageing. The high temperature nylon prepared in the examples was injection molded into small 1BA specimens 75mm in total length, 25mm in gauge length, 10mm in end width, 2mm in thickness and 5mm in middle parallel portion width. Tensile test conditions: the drawing speed was 20 mm/min. Thermal-oxidative aging conditions: and (3) placing the test sample into a thermo-oxidative aging experimental box, setting the experimental temperature to be 160 ℃, ventilating once every minute, setting the rotating speed to be 30r/min, and aging for 50 d. Each set of 5 samples, the test results were averaged over the 5 sample data. The thermal oxidative aging resistance of nylon is expressed by tensile strength retention rate, and the greater the retention rate, the better the thermal oxidative aging resistance.
Tensile strength retention (%) tensile strength after sample aging/tensile strength without sample aging × 100%
TABLE 1 thermo-oxidative aging resistance test results
Retention rate of tensile strength% | |
Example 1 | 71.7 |
Example 2 | 81.9 |
Example 3 | 88.3 |
Example 4 | 88.1 |
Example 5 | 92.4 |
The above results show that the thermal oxidative aging resistance of example 2 is significantly improved compared to example 1, which is probably because the mesoporous silica nanorods are firstly used as the nanocarriers, and then the functional compound is loaded on the mesoporous silica nanorods, so that the migration of the functional compound molecules in the matrix can be effectively limited, and meanwhile, the effective active molecules in the functional compound are continuously released, thereby promoting the improvement of the thermal oxidative aging resistance. The tensile strength retention rate of example 3 is significantly higher than that of example 2, which may be because in example 3, when the mesoporous silica nanorod is prepared, the silica nanorod is first subjected to silanization modification, on one hand, a methoxy group in the coupling agent and a silicon hydroxyl hydrogen on the surface of the silica nanorod are subjected to elimination reaction to form a firm chemical bond, so that a mercapto functional group is connected to the surface of the silica nanorod in a chemical bonding manner, and an effective reactive center is provided for the combination of functional compounds; on the other hand, the silicon hydroxyl content on the surface of the silicon dioxide nano rod and the interface compatibility between the nano carrier and the polymer matrix are also improved, so that the dispersibility of the functionalized mesoporous silicon dioxide nano rod in the matrix is improved, and the performance is promoted to be improved.
Test example 2
Chemical resistance performance test: determination of tensile Properties of plastics according to the national Standard GB/T1040.2-2006 part 2: test conditions for molded and extruded plastics the tensile properties of the test specimens before and after chemical corrosion were tested using a CMT-5104 model universal tester. The high temperature nylon prepared in the examples was injection molded into small 1BA specimens 75mm in total length, 25mm in gauge length, 10mm in end width, 2mm in thickness and 5mm in middle parallel portion width. Tensile test conditions: the drawing speed was 50mm/min, the temperature was 15 ℃ and the humidity was 10% RH. Chemical corrosion conditions are as follows: and respectively putting the test samples into beakers filled with 1000mL of ethylene glycol, standing at 25 ℃ for 7 days, taking out, treating the medium on the surfaces of the test samples with gauze, and testing the tensile strength of the test samples. Each set of 5 samples, the test results were averaged over the 5 sample data. Chemical resistance performance of nylon is expressed by tensile strength retention, and the greater the retention, the better the chemical resistance performance.
Tensile strength retention (%) tensile strength after sample corrosion/tensile strength without sample corrosion × 100%
TABLE 2 chemical resistance test results
Retention rate of tensile strength% | |
Example 1 | 70.5 |
Example 2 | 78.8 |
Example 3 | 85.2 |
Example 4 | 85.0 |
Example 5 | 89.3 |
The results show that the high-temperature nylon prepared by the technical scheme of the invention has good chemical corrosion resistance. In example 5, the copper chloride dihydrate and the zirconium oxychloride octahydrate are compounded to serve as the metal salt in the functional compound, and the tensile strength retention rate of the metal salt is superior to that of example 3 or 4 using a single metal salt, probably because the compound formed by the octahedral zirconium ions with high atomic weight has higher chemical reactivity, the binding effect between the functional compound and the modified mesoporous silica nanorods is enhanced, and the crosslinking strength is improved; the compound formed by copper ions with a distorted octahedral structure with high-efficiency dipole moment has high electron affinity, occupies partial mesoporous channels of the silicon dioxide nanorods, increases the chemical bond density, reduces free volume crosslinking, and induces the crosslinking strength in the matrix; the two have synergistic effect, and the crosslinking strength of the matrix is improved together, so that the chemical resistance of the nylon is improved.
Claims (8)
1. The high-temperature nylon is characterized by comprising the following raw materials: nylon 6T, nylon 12T, an elastomer, an antioxidant and a functionalized mesoporous silica nanorod.
2. The high-temperature nylon is characterized by comprising the following raw materials in parts by weight: 35-50 parts of nylon 6T, 35-50 parts of nylon 12T, 10-20 parts of elastomer, 0.5-1.5 parts of antioxidant and 3-8 parts of functionalized mesoporous silica nano-rod.
3. The high temperature nylon of claim 1 or 2, wherein the preparation method of the functionalized mesoporous silica nanorods comprises the following steps:
s1, adding 3-5 parts by weight of hexadecyl trimethyl ammonium bromide into 20-30 parts by weight of water, uniformly dispersing by ultrasonic, adding 0.3-0.5 part by weight of phosphatidylcholine, stirring at the room temperature at the rotation speed of 1000-1500rpm for 20-40min, then adding 20-30 parts by weight of 20-30 wt% ammonia water, continuously stirring for 1-3h, then adding 10-20 parts by weight of tetraethyl orthosilicate, continuously stirring for 3-5h, and after the stirring is finished, centrifuging, washing and drying to obtain silicon dioxide nanorods;
s2, adding all the silicon dioxide nanorods obtained in the step S1 into 40-60 parts by weight of 10-15% hydrochloric acid ethanol solution, stirring and reacting at 70-80 ℃ at the rotating speed of 400-800rpm for 8-16h, and centrifuging, washing and drying after the reaction is finished to obtain mesoporous silicon dioxide nanorods;
s3, adding 4-6 parts by weight of functional compound into 15-30 parts by weight of acetone, stirring at the rotation speed of 1200-1800rpm for 20-40min at room temperature, then adding all the mesoporous silica nanorods obtained in the step S2, continuously stirring for 12-24h, centrifuging after finishing stirring, washing, and drying to obtain the functionalized mesoporous silica nanorods.
4. The high temperature nylon of claim 3, wherein the preparation method of the functionalized mesoporous silica nanorods comprises the following steps:
s1, adding 3-5 parts by weight of hexadecyl trimethyl ammonium bromide into 20-30 parts by weight of water, uniformly dispersing by ultrasonic, adding 0.3-0.5 part by weight of phosphatidylcholine, stirring at the room temperature at the rotation speed of 1000-1500rpm for 20-40min, then adding 20-30 parts by weight of 20-30 wt% ammonia water, continuously stirring for 1-3h, then adding 10-20 parts by weight of tetraethyl orthosilicate, continuously stirring for 3-5h, and after the stirring is finished, centrifuging, washing and drying to obtain silicon dioxide nanorods;
s2, adding 6-10 parts by weight of (3-mercaptopropyl) trimethoxysilane into 310 parts by weight of 250-310 parts by weight of anhydrous ethanol, stirring at the rotation speed of 1000-1500rpm at room temperature for 10-20min, then adding all the silica nanorods obtained in the step S1, stirring at the rotation speed of 300-600rpm at the temperature of 65-75 ℃ for reaction for 8-15h, centrifuging after the reaction is finished, washing, and drying to obtain modified silica nanorods;
s3, adding all the modified silicon dioxide nanorods obtained in the step S2 into 40-60 parts by weight of 10-15% hydrochloric acid ethanol solution, stirring and reacting at 70-80 ℃ at the rotating speed of 400-800rpm for 8-16h, and centrifuging, washing and drying after the reaction is finished to obtain the modified mesoporous silicon dioxide nanorods;
s4, adding 4-6 parts by weight of functional compound into 15-30 parts by weight of acetone, stirring at the rotation speed of 1200-1800rpm for 20-40min at room temperature, then adding all the modified mesoporous silica nanorods obtained in the step S3, continuously stirring for 12-24h, and centrifuging, washing and drying after the stirring is finished to obtain the functionalized mesoporous silica nanorods.
5. A high temperature nylon as claimed in claim 1 or 2 wherein the elastomer is any one of maleic anhydride grafted ethylene-octene copolymer, maleic anhydride grafted hydrogenated styrene-butadiene-styrene triblock copolymer, maleic anhydride grafted ethylene propylene diene monomer.
6. The high temperature nylon of claim 1 or 2, wherein the antioxidant is any one of antioxidant 1098, antioxidant KY2468 and antioxidant 1520.
7. A high temperature nylon as claimed in claim 3 or 4 wherein the functional compound is prepared by the following process: adding 1-3 parts by weight of metformin hydrochloride and 1-3 parts by weight of 2, 2-bipyridine into 50-80 parts by weight of acetone, stirring at the rotation speed of 1000rpm of 600-.
8. A process for preparing a high temperature nylon as claimed in any of claims 1 to 7 comprising the steps of:
drying nylon 6T, nylon 12T and the elastomer in a blast drying oven at 75-85 ℃ for 8-15h according to the formula, then adding the nylon 6T, the nylon 12T, the elastomer, the antioxidant and the functionalized mesoporous silica nanorods into an internal mixer for internal mixing, discharging the internal mixed materials into a screw extruder, and carrying out melt blending extrusion granulation to obtain the high-temperature nylon.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202111367583.8A CN114031938B (en) | 2021-11-18 | 2021-11-18 | High-temperature nylon and preparation method thereof |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202111367583.8A CN114031938B (en) | 2021-11-18 | 2021-11-18 | High-temperature nylon and preparation method thereof |
Publications (2)
Publication Number | Publication Date |
---|---|
CN114031938A true CN114031938A (en) | 2022-02-11 |
CN114031938B CN114031938B (en) | 2024-02-23 |
Family
ID=80138081
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN202111367583.8A Active CN114031938B (en) | 2021-11-18 | 2021-11-18 | High-temperature nylon and preparation method thereof |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN114031938B (en) |
Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN111117220A (en) * | 2019-12-31 | 2020-05-08 | 会通新材料(上海)有限公司 | Polyamide composition with permanent static dissipation function and application thereof |
-
2021
- 2021-11-18 CN CN202111367583.8A patent/CN114031938B/en active Active
Patent Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN111117220A (en) * | 2019-12-31 | 2020-05-08 | 会通新材料(上海)有限公司 | Polyamide composition with permanent static dissipation function and application thereof |
Also Published As
Publication number | Publication date |
---|---|
CN114031938B (en) | 2024-02-23 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
US3379792A (en) | Polymer blend of a polyphenylene oxide and a polyamide | |
JP7045462B2 (en) | Polyamide composite material with high strength and easy electroplating and its manufacturing method | |
EP2895552B1 (en) | Heat aging resistant ethylene vinyl acetate copolymer composition and process for its production | |
KR101940418B1 (en) | Polyamide resin composition and article comprising the same | |
KR20120004834A (en) | Blend composition comprising polyketone and nylon 6 and manufacturing method of composite using it | |
KR102082420B1 (en) | Polyamide resin composition with improved long term heat resistance | |
CN104788932B (en) | The antistatic PC of excellent heat stability/ASA alloy materials and preparation method thereof | |
WO2023097771A1 (en) | Epoxy molding compound of modified silicon dioxide grafted epoxy resin, and preparation method therefor | |
CN114573981B (en) | Halogen-free flame-retardant PA/PPO composite material and preparation method thereof | |
KR101806005B1 (en) | Modified poly(arylene ether) resin composition, method for preparing the resin composition, and molded article produced thereof | |
CN111087808A (en) | Hydrolysis-resistant high-toughness polyamide resin composite material and preparation method thereof | |
CN114031938B (en) | High-temperature nylon and preparation method thereof | |
CN115678264B (en) | Antistatic flame-retardant composite material and preparation method and application thereof | |
CN112029276A (en) | Special material for low-temperature toughened polyamide cable tie with high water absorption rate, cable tie and preparation method | |
KR20140086737A (en) | Thermoplastic resin composition and article including same | |
KR20190078066A (en) | Polyamide resin composition, method for preparating the same and article produced therefrom | |
KR102083231B1 (en) | Reinforced polyphthalamide/poly(phenylene ether) composition | |
CN117683346B (en) | Low-water-absorption glass fiber reinforced PA/PPO alloy and preparation method thereof | |
US9803073B2 (en) | Heat resistant ethylene vinyl acetate copolymer composition and process for its production | |
KR101756514B1 (en) | Polyphenylene sulfide resin composition and molded article produced therefrom | |
KR960006628B1 (en) | Thermoplastic resin compositions | |
CN117844167B (en) | ABS antistatic plastic based on graphene modification and preparation process thereof | |
CN116285336A (en) | Long-term cold-resistant ribbon material and preparation method thereof | |
KR20220169607A (en) | Thermoplastic resin composition, method for preparing the same and article prepared therefrom | |
EP3077456B1 (en) | Heat resistant ethylene vinyl acetate copolymer composition and process for its production |
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 | ||
GR01 | Patent grant | ||
GR01 | Patent grant |