CN113185690B - Process for preparing high-fluidity polyamide - Google Patents
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- CN113185690B CN113185690B CN202110730705.9A CN202110730705A CN113185690B CN 113185690 B CN113185690 B CN 113185690B CN 202110730705 A CN202110730705 A CN 202110730705A CN 113185690 B CN113185690 B CN 113185690B
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- 239000004952 Polyamide Substances 0.000 title claims abstract description 56
- 229920002647 polyamide Polymers 0.000 title claims abstract description 56
- 238000004519 manufacturing process Methods 0.000 title description 3
- 239000000463 material Substances 0.000 claims abstract description 57
- 238000002360 preparation method Methods 0.000 claims abstract description 19
- 238000006243 chemical reaction Methods 0.000 claims description 46
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 43
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 24
- 229910052757 nitrogen Inorganic materials 0.000 claims description 21
- 238000001035 drying Methods 0.000 claims description 20
- VYFYYTLLBUKUHU-UHFFFAOYSA-N dopamine Chemical compound NCCC1=CC=C(O)C(O)=C1 VYFYYTLLBUKUHU-UHFFFAOYSA-N 0.000 claims description 18
- JBKVHLHDHHXQEQ-UHFFFAOYSA-N epsilon-caprolactam Chemical compound O=C1CCCCCN1 JBKVHLHDHHXQEQ-UHFFFAOYSA-N 0.000 claims description 18
- 238000001914 filtration Methods 0.000 claims description 14
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 12
- 229960003638 dopamine Drugs 0.000 claims description 9
- 238000001125 extrusion Methods 0.000 claims description 9
- 229920003209 poly(hydridosilsesquioxane) Polymers 0.000 claims description 9
- 238000009835 boiling Methods 0.000 claims description 8
- 239000012153 distilled water Substances 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 8
- 238000005406 washing Methods 0.000 claims description 8
- JHWNWJKBPDFINM-UHFFFAOYSA-N Laurolactam Chemical compound O=C1CCCCCCCCCCCN1 JHWNWJKBPDFINM-UHFFFAOYSA-N 0.000 claims description 7
- 238000005469 granulation Methods 0.000 claims description 7
- 230000003179 granulation Effects 0.000 claims description 7
- 239000002253 acid Substances 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 5
- 239000002994 raw material Substances 0.000 claims description 4
- 238000006459 hydrosilylation reaction Methods 0.000 claims description 3
- 230000006837 decompression Effects 0.000 claims description 2
- 239000000155 melt Substances 0.000 abstract description 7
- 229920006122 polyamide resin Polymers 0.000 abstract description 4
- 239000011159 matrix material Substances 0.000 abstract description 3
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 229920006130 high-performance polyamide Polymers 0.000 abstract description 2
- 230000009878 intermolecular interaction Effects 0.000 abstract description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical class [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract 1
- 239000011347 resin Substances 0.000 abstract 1
- 229920005989 resin Polymers 0.000 abstract 1
- 239000004033 plastic Substances 0.000 description 9
- 229920003023 plastic Polymers 0.000 description 9
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 6
- 229920002302 Nylon 6,6 Polymers 0.000 description 6
- 239000000203 mixture Substances 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- 239000003795 chemical substances by application Substances 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 239000000654 additive Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- LDVVTQMJQSCDMK-UHFFFAOYSA-N 1,3-dihydroxypropan-2-yl formate Chemical compound OCC(CO)OC=O LDVVTQMJQSCDMK-UHFFFAOYSA-N 0.000 description 2
- RYYXDZDBXNUPOG-UHFFFAOYSA-N 4,5,6,7-tetrahydro-1,3-benzothiazole-2,6-diamine;dihydrochloride Chemical compound Cl.Cl.C1C(N)CCC2=C1SC(N)=N2 RYYXDZDBXNUPOG-UHFFFAOYSA-N 0.000 description 2
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 description 2
- 241000208202 Linaceae Species 0.000 description 2
- 235000004431 Linum usitatissimum Nutrition 0.000 description 2
- 239000002202 Polyethylene glycol Substances 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- 239000003963 antioxidant agent Substances 0.000 description 2
- 230000003078 antioxidant effect Effects 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 229920001971 elastomer Polymers 0.000 description 2
- 239000000806 elastomer Substances 0.000 description 2
- 229920006351 engineering plastic Polymers 0.000 description 2
- 239000003822 epoxy resin Substances 0.000 description 2
- 239000000835 fiber Substances 0.000 description 2
- 239000000945 filler Substances 0.000 description 2
- 238000001746 injection moulding Methods 0.000 description 2
- 239000012948 isocyanate Substances 0.000 description 2
- 150000002513 isocyanates Chemical class 0.000 description 2
- 239000003607 modifier Substances 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 229920000647 polyepoxide Polymers 0.000 description 2
- 229920001223 polyethylene glycol Polymers 0.000 description 2
- 239000000741 silica gel Substances 0.000 description 2
- 229910002027 silica gel Inorganic materials 0.000 description 2
- 238000005160 1H NMR spectroscopy Methods 0.000 description 1
- KXDHJXZQYSOELW-UHFFFAOYSA-N Carbamic acid Chemical compound NC(O)=O KXDHJXZQYSOELW-UHFFFAOYSA-N 0.000 description 1
- 239000002656 Distearyl thiodipropionate Substances 0.000 description 1
- 229920002943 EPDM rubber Polymers 0.000 description 1
- QFHVLUABSDQCPF-UHFFFAOYSA-N N-[5-(2-aminoethyl)-1,2-dihydroxycyclohexa-2,4-dien-1-yl]-2-methylprop-2-enamide Chemical compound C(C(=C)C)(=O)NC1(CC(CCN)=CC=C1O)O QFHVLUABSDQCPF-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- PWWSSIYVTQUJQQ-UHFFFAOYSA-N distearyl thiodipropionate Chemical group CCCCCCCCCCCCCCCCCCOC(=O)CCSCCC(=O)OCCCCCCCCCCCCCCCCCC PWWSSIYVTQUJQQ-UHFFFAOYSA-N 0.000 description 1
- 235000019305 distearyl thiodipropionate Nutrition 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000005038 ethylene vinyl acetate Substances 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000003365 glass fiber Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- RKISUIUJZGSLEV-UHFFFAOYSA-N n-[2-(octadecanoylamino)ethyl]octadecanamide Chemical group CCCCCCCCCCCCCCCCCC(=O)NCCNC(=O)CCCCCCCCCCCCCCCCC RKISUIUJZGSLEV-UHFFFAOYSA-N 0.000 description 1
- 238000000655 nuclear magnetic resonance spectrum Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229920001200 poly(ethylene-vinyl acetate) Polymers 0.000 description 1
- -1 polytetrafluoroethylene Polymers 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 239000004810 polytetrafluoroethylene Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 229920006114 semi-crystalline semi-aromatic polyamide Polymers 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- 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
- C08G69/42—Polyamides containing atoms other than carbon, hydrogen, oxygen, and nitrogen
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Polyamides (AREA)
Abstract
The invention relates to the field of polyamide material preparation, in particular to a preparation method of high-fluidity polyamide, and sulfonated graphene grafted polyamide prepared under a high-temperature and high-pressure environment has better compatibility with matrix polyamide resin, thereby being beneficial to improving the mechanical property and fluidity of the polyamide material; the high-performance polyamide takes a multi-branched polyamide material as main matrix resin, the molecules of the polyamide material have smaller atom space arrangement size and symmetrical structure, the characteristics of no entanglement inside and outside the molecules and small intermolecular interaction are realized, the melt viscosity of the polyamide with the structure is much lower than that of linear polyamide with the same molecular weight, the excellent fluidity of the polyamide material widens the application range of the polyamide material, shortens the processing period and reduces the system cost.
Description
Technical Field
The invention relates to the field of preparation of polyamide materials, in particular to a preparation method of high-fluidity polyamide.
Background
With the gradual miniaturization and light weight development of parts in the industries of automobiles, electronics, electrical and the like, steel is replaced by plastic as the development trend of the current material field, and more metal materials are gradually replaced by engineering plastics such as polyamide.
CN107057333A discloses a polyamide plastic, relating to the technical field of engineering plastics. The traditional Chinese medicine is prepared from the following raw materials in parts by weight: 30 to 35 parts of polyamide, 10 to 15 parts of epoxy resin, 1 to 5 parts of polytetrafluoroethylene, 2 to 4 parts of carbon black, 5 to 10 parts of thiourea dioxide, 5 to 10 parts of silica gel, 0.5 to 1 part of monoglyceride, 1 to 5 parts of polyethylene glycol, 0.4 to 0.8 part of flax fiber, 2 to 5 parts of ethylenediamine, 1 to 5 parts of glycerol and 1 to 5 parts of isocyanate. According to the invention, the tensile strength, the wear resistance, the self-lubricating property and the impact toughness property of the polyamide plastic lining are effectively improved by adding the epoxy resin, the thiourea dioxide, the silica gel, the monoglyceride, the polyethylene glycol, the flax fiber, the ethylenediamine, the glycerol and the isocyanate.
CN102010589B discloses a polyamide blend molding compound, comprising a polyamide mixture component and at least one impact resistant component, characterized in that the polyamide mixture component comprises: (A)20 to 65% by weight of at least one semicrystalline polyamide; (B)8 to 25% by weight of at least one amorphous and/or microcrystalline polyamide; and (C)1 to 20% by weight of at least one polyamide. The impact resistant composition comprises: (D)10 to 40% by weight of a polyamide elastomer comprising hard and soft segments, wherein the hard segments are based on caprolactam and/or amino-carboxylic acid; and (E)0 to 35 weight percent of a non-polyamide elastomer. Molded parts, such as brake booster lines, formed from the polyamide blend molding compound have a modulus of elasticity at a temperature of-40 ℃ of no greater than 2400MPa, and a modulus of elasticity at a temperature of +120 ℃ of at least 180 MPa.
CN103911004A discloses a modified polyamide-66 plastic, which is prepared from a polyamide-66 plastic and an additive, wherein the additive comprises a wear-resistant agent, an impact-resistant modifier, an antioxidant, a chemical-resistant agent and a filler, the wear-resistant agent is N, N' -ethylene bis stearamide, the impact-resistant modifier is an ethylene-vinyl acetate copolymer, the antioxidant is distearyl thiodipropionate, the chemical-resistant agent is ethylene propylene diene monomer, and the filler is glass fiber. According to the modified polyamide-66 plastic disclosed by the invention, various additives are added into the polyamide-66 plastic, so that the prepared modified polyamide-66 plastic has excellent performances such as wear resistance, mechanical strength, oxidation resistance, chemical resistance, strength, hardness and the like, the performance of the polyamide-66 plastic is greatly enhanced, and the application range is widened.
The polyamide resin prepared by the invention and the prior art is of a linear structure, has chain entanglement, and has high relative viscosity and poor melt fluidity although the mechanical property is good. For injection molding and extrusion processes, uneven or even unfilled mold filling occurs, so that it is not suitable to make thin-walled and complex precision parts with the polyamide resin of the above invention.
Disclosure of Invention
In order to solve the above problems, the present invention provides a method for producing a high-fluidity polyamide.
A preparation method of high-fluidity polyamide comprises the following steps:
according to the mass parts: putting 1600 parts of caprolactam with 1500-fold, 500 parts of laurolactam with 400-fold, 50-60 parts of distilled water and 25-35 parts of intermediate A into a high-pressure reaction kettle, closing a feed inlet, vacuumizing, and replacing air in the kettle with high-purity nitrogen, and performing the operation for 3 times, and finally keeping the pressure in the kettle at-0.09 to-0.06 MPa; heating the reaction kettle to 200-300 ℃, and reacting for 240 min; opening an exhaust valve, vacuumizing for reaction for 120-180min, introducing high-purity nitrogen for protection after the reaction is finished, standing and balancing for 120min, extracting the obtained material in boiling water, filtering, washing and drying to obtain the polyamide material;
the preparation method of the intermediate A comprises the following steps:
according to the mass parts: introducing high-purity nitrogen, carrying out reduced pressure reaction at 60-70 ℃ for 90-180min on 1.2-3.5 parts of 2-chloro-4, 6-diallyl triazine, 1.8-3.7 parts of 3-methacrylamide dopamine, 5-9 parts of hydrogen silsesquioxane and 0.8-1.6 parts of isopropanol solution of chloroplatinic acid with the mass percent concentration of 0.5-1.9 percent, then carrying out pressure relief after the reaction is finished, filtering the material, introducing the filtered material into 400 parts of hot water at 80-95 ℃ of 300-one, stirring the hot water for 1-5h, taking out the material, drying the material, adding the dried material into a double-screw extruder for extrusion granulation, and drying the material after the extrusion granulation to obtain the intermediate A.
The reaction mechanism is that the 2-chloro-4, 6-diallyl triazine, the 3-methacrylamide dopamine and the hydrogen silsesquioxane are subjected to hydrosilylation reaction to generate an intermediate A.
The decompression reaction is carried out under the vacuum degree of 0.07-0.09 MPa.
The temperature of the extruder is 230-250 ℃.
The rotating speed of the extruder is 280-350 r/min.
The partial reaction equation is schematically shown as follows:
the technical effects are as follows: according to the preparation method of the high-fluidity polyamide, 2-chloro-4, 6-diallyl triazine, 3-methacrylamide dopamine and hydrogen silsesquioxane are used as raw materials to carry out hydrosilylation reaction under a high-temperature and high-pressure environment to obtain modified polyamide, and the modified polyamide has good compatibility with matrix polyamide resin and is beneficial to improvement of mechanical property and fluidity of a polyamide material; the polyamide material molecule has smaller atom space arrangement size and symmetrical structure, has the characteristics of no entanglement inside and outside the molecule and small intermolecular interaction, the melt viscosity of the polyamide with the structure is much lower than that of linear polyamide with the same molecular weight, the silicon-hydrogen addition reactant obtained by taking 2-chloro-4, 6-diallyl triazine and 3-methacrylamide dopamine as raw materials increases the fluidity of the polyamide, the melt flow speed can reach 31.9 (g/10 min), the excellent fluidity widens the application range of the polyamide material, shortens the processing period and reduces the system cost.
Drawings
FIG. 1 is a (1HNMR) NMR spectrum of 3-methacrylamidodopamine used in example 2.
Detailed Description
The invention is further illustrated by the following specific examples:
in order to quickly evaluate the flow properties of the material, the Melt Flow Rate (MFR) of the material was measured using a melt index meter. The test temperature was 235 ℃ and the load was 0.325 kg. The high-performance polyamide material prepared in the following examples is injection-molded into a standard sample by an injection molding machine, and mechanical property tests are carried out, wherein the tensile strength and the elongation at break which are used as mechanical property indexes are tested according to GB/T1040.2-2006.
Example 1
A preparation method of high-fluidity polyamide comprises the following steps:
putting 1500kg of caprolactam, 400kg of laurolactam, 50kg of distilled water and 25kg of intermediate A into a high-pressure reaction kettle, closing a feeding port, vacuumizing, and replacing air in the kettle with high-purity nitrogen, and performing the operation for 3 times, and finally keeping the pressure in the kettle to be-0.06 MPa; heating the reaction kettle to 200 ℃, and reacting for 180 min; opening an exhaust valve, vacuumizing for reaction for 120min, introducing high-purity nitrogen for protection after the reaction is finished, standing and balancing for 100min, extracting the obtained material in boiling water, filtering, washing and drying to obtain a polyamide material;
the preparation method of the intermediate A comprises the following steps:
introducing high-purity nitrogen, carrying out reduced pressure reaction at 60 ℃ for 90min on 1.2kg of 2-chloro-4, 6-diallyl triazine, 1.8kg of 3-methacrylamide dopamine, 5kg of hydrogen silsesquioxane and 0.8kg of isopropanol solution of chloroplatinic acid with the mass percent concentration of 0.5%, decompressing after completion, decompressing, filtering the material, introducing the filtered material into 300kg of 80 ℃ hot water, stirring for 1h, taking out, drying, adding the dried material into a double-screw extruder for extrusion granulation, and drying after completion to obtain the intermediate A.
Example 2
A preparation method of high-fluidity polyamide comprises the following steps:
1550kg of caprolactam, 450kg of laurolactam, 55kg of distilled water and 30kg of intermediate A are put into a high-pressure reaction kettle, a feeding port is closed, the air in the kettle is replaced by high-purity nitrogen gas through vacuumizing, the operation is carried out for 3 times, and finally the pressure in the kettle is kept to be-0.07 MPa; heating the reaction kettle to 250 ℃, and reacting for 210 min; opening an exhaust valve, vacuumizing for reaction for 150min, introducing high-purity nitrogen for protection after the reaction is finished, standing and balancing for 110min, extracting the obtained material in boiling water, filtering, washing and drying to obtain a polyamide material;
the preparation method of the intermediate A comprises the following steps:
introducing high-purity nitrogen, carrying out reduced pressure reaction at 64 ℃ for 150min on 2.4kg of 2-chloro-4, 6-diallyl triazine, 2.5kg of 3-methacrylamide dopamine, 7kg of hydrogen silsesquioxane and 1.2kg of isopropanol solution of chloroplatinic acid with the mass percent concentration of 0.7%, decompressing after completion, filtering the materials, introducing the materials into 350kg of 90 ℃ hot water, stirring for 3h, taking out, drying, adding the materials into a double-screw extruder for extrusion granulation, wherein the temperature of the extruder is 240 ℃, the rotating speed is 310r/min, and drying after completion to obtain the intermediate A.
Example 3
A preparation method of high-fluidity polyamide comprises the following steps:
putting 1600kg of caprolactam, 500kg of laurolactam, 60kg of distilled water and 35kg of intermediate A into a high-pressure reaction kettle, closing a feeding port, vacuumizing, and replacing air in the kettle with high-purity nitrogen, and performing the operation for 3 times, and finally keeping the pressure in the kettle to be-0.09 MPa; heating the reaction kettle to 300 ℃, and reacting for 240 min; opening an exhaust valve, vacuumizing for reaction for 180min, introducing high-purity nitrogen for protection after the reaction is finished, standing and balancing for 120min, extracting the obtained material in boiling water, filtering, washing and drying to obtain a polyamide material;
the preparation method of the intermediate A comprises the following steps:
introducing high-purity nitrogen, carrying out reduced pressure reaction at 70 ℃ for 180min on 3.5kg of 2-chloro-4, 6-diallyl triazine, 3.7kg of 3-methacrylamide dopamine, 9kg of hydrogen silsesquioxane and 1.6kg of isopropanol solution of chloroplatinic acid with the mass percent concentration of 1.9%, decompressing after completion, filtering the materials, introducing the materials into 400kg of 95 ℃ hot water, stirring for 5h, taking out, drying, adding the materials into a double-screw extruder for extrusion granulation, wherein the temperature of the extruder is 250 ℃, the rotating speed is 350r/min, and drying after completion to obtain the intermediate A.
The melt flow rate and mechanical strength test results for the materials prepared in the above examples are shown in the following table:
comparative example 1
A preparation method of high-fluidity polyamide comprises the following steps:
putting 1500kg of caprolactam, 400kg of laurolactam and 50kg of distilled water into a high-pressure reaction kettle, closing a feeding port, vacuumizing, and replacing air in the kettle with high-purity nitrogen, and performing the operation for 3 times, and finally keeping the pressure in the kettle to be-0.06 MPa; heating the reaction kettle to 200 ℃, and reacting for 180 min; opening an exhaust valve, vacuumizing for reaction for 120min, introducing high-purity nitrogen for protection after the reaction is finished, standing and balancing for 100min, extracting the obtained material in boiling water, filtering, washing and drying to obtain a polyamide material;
comparative example 2
A preparation method of high-fluidity polyamide comprises the following steps:
putting 1500kg of caprolactam, 50kg of distilled water and 25kg of the intermediate A into a high-pressure reaction kettle, closing a feeding port, vacuumizing, and replacing air in the kettle with high-purity nitrogen, and performing the operation for 3 times, and finally keeping the pressure in the kettle to be-0.06 MPa; heating the reaction kettle to 200 ℃, and reacting for 180 min; opening an exhaust valve, vacuumizing for reaction for 120min, introducing high-purity nitrogen for protection after the reaction is finished, standing and balancing for 100min, extracting the obtained material in boiling water, filtering, washing and drying to obtain a polyamide material;
the other technical scheme is the same as that of the embodiment 1.
Comparative example 3
A preparation method of high-fluidity polyamide comprises the following steps:
putting 1500kg of caprolactam, 400kg of laurolactam, 50kg of distilled water and 25kg of intermediate A into a high-pressure reaction kettle, closing a feeding port, vacuumizing, and replacing air in the kettle with high-purity nitrogen, and performing the operation for 3 times, and finally keeping the pressure in the kettle to be-0.06 MPa; heating the reaction kettle to 200 ℃, and reacting for 180 min; opening an exhaust valve, vacuumizing for reaction for 120min, introducing high-purity nitrogen for protection after the reaction is finished, standing and balancing for 100min, extracting the obtained material in boiling water, filtering, washing and drying to obtain a polyamide material;
the preparation method of the intermediate A comprises the following steps:
introducing high-purity nitrogen, carrying out reduced pressure reaction on 1.2kg of 2-chloro-4, 6-diallyl triazine, 5kg of hydrogen silsesquioxane and 0.8kg of isopropanol solution of chloroplatinic acid with the mass percent concentration of 0.5% at 60 ℃ for 90min, relieving pressure after the reaction is finished, filtering the materials, introducing the materials into 300kg of hot water with the temperature of 80 ℃, stirring for 1h, taking out the materials, drying, adding the materials into a double-screw extruder, extruding and granulating, and drying after the reaction is finished to obtain the intermediate A.
The melt flow rate and mechanical strength test results for the materials prepared in the above comparative examples are shown in the following table:
Claims (5)
1. a preparation method of high-fluidity polyamide is characterized in that:
according to the mass parts: putting 1600 parts of caprolactam with 1500-fold, 500 parts of laurolactam with 400-fold, 50-60 parts of distilled water and 25-35 parts of intermediate A into a high-pressure reaction kettle, closing a feed inlet, vacuumizing, and replacing air in the kettle with high-purity nitrogen, and performing the operation for 3 times, and finally keeping the pressure in the kettle at-0.09 to-0.06 MPa; heating the reaction kettle to 200-300 ℃, and reacting for 240 min; opening an exhaust valve, vacuumizing for reaction for 120-180min, introducing high-purity nitrogen for protection after the reaction is finished, standing and balancing for 120min, extracting the obtained material in boiling water, filtering, washing and drying to obtain the polyamide material;
2-chloro-4, 6-diallyl triazine, 3-methacrylamide dopamine and hydrogen silsesquioxane are used as raw materials to carry out hydrosilylation reaction to generate the intermediate A.
2. The process for producing a high-fluidity polyamide, according to claim 1, characterized in that: the preparation method of the intermediate A comprises the following steps:
according to the mass parts: introducing high-purity nitrogen, carrying out reduced pressure reaction at 60-70 ℃ for 90-180min on 1.2-3.5 parts of 2-chloro-4, 6-diallyl triazine, 1.8-3.7 parts of 3-methacrylamide dopamine, 5-9 parts of hydrogen silsesquioxane and 0.8-1.6 parts of isopropanol solution of chloroplatinic acid with the mass percent concentration of 0.5-1.9 percent, then carrying out pressure relief after the reaction is finished, filtering the material, introducing the filtered material into 400 parts of hot water at 80-95 ℃ of 300-one, stirring the hot water for 1-5h, taking out the material, drying the material, adding the dried material into a double-screw extruder for extrusion granulation, and drying the material after the extrusion granulation to obtain the intermediate A.
3. The process for producing a high-fluidity polyamide, according to claim 2, characterized in that: the decompression reaction is carried out under the vacuum degree of 0.07-0.09 MPa.
4. The process for producing a high-fluidity polyamide, according to claim 2, characterized in that: the extrusion temperature of the extruder is 230-250 ℃.
5. The process for producing a high-fluidity polyamide, according to claim 2, characterized in that: the rotating speed of the extruder is 280-350 r/min.
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| JPS63258887A (en) * | 1987-04-16 | 1988-10-26 | Toray Ind Inc | Organic silicon compound |
| TW562822B (en) * | 2002-09-03 | 2003-11-21 | Chang Chun Plastics Co Ltd | Organic-inorganic hybrid film material and its preparation |
| JP4483331B2 (en) * | 2004-02-17 | 2010-06-16 | チッソ株式会社 | Diamine having silsesquioxane skeleton and polymer using the same |
| CN104830053A (en) * | 2015-01-08 | 2015-08-12 | 杭州师范大学 | Caprolactam-laurolactam co-polymer modified by glass fiber and preparation method of powder thereof |
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