CN101121818A - High-performance hydrolysis-resistance reinforced nylon 6 and preparation method thereof - Google Patents
High-performance hydrolysis-resistance reinforced nylon 6 and preparation method thereof Download PDFInfo
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- CN101121818A CN101121818A CNA2006100298514A CN200610029851A CN101121818A CN 101121818 A CN101121818 A CN 101121818A CN A2006100298514 A CNA2006100298514 A CN A2006100298514A CN 200610029851 A CN200610029851 A CN 200610029851A CN 101121818 A CN101121818 A CN 101121818A
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Abstract
The present invention discloses a high-performance anti-hydrolysis reinforced nylon 6 and the preparation method. The components and weight shares include: 40 to 88 shares of nylon-6 resin, 5 to 50 shares of non-absorbent composite elastomer activated toughener, and 10 to 50 shares of glass fiber. The non-absorbent composite elastomer toughener is the composite made by the activated reaction of the poly olefin compound of different chemical structures. The product of the present invention is inspected with the national standards. The test results show that each performance of the high-performance anti-hydrolysis reinforced nylon 6 all reach or surpass the preset requirements, solving the problem that the rigidness of the material will be greatly reduced after being dipped in water and boiled; the material is made to have the excellent anti-hydrolysis performance; the bending strength of the material can still maintain above 65 percent after being boiled in water for 100 hours.
Description
Technical field
The present invention relates to a kind of high-performance hydrolysis-resistance reinforced nylon 6 dragon 6 and preparation method thereof.
Background technology
Nylon 6 is the extremely wide engineering plastics of a kind of purposes, is made by caprolactam polymerization, and its fusing point is 215～225 ℃, and its fusing point, rigidity, wear resistance all are lower than PA66, and water absorbability and toughness all are better than PA66, are the cost performance best materials.
Amide group in the PA6 molecular chain has polarity, can form hydrogen bond, so the mechanical property excellence, and as tensile strength height, good toughness, ability repeated stock vibrations are tough and tensile engineering plastics; PA6 belongs to crystalline material, fusing point is obvious; Surface hardness is big, abrasion performance, frictional coefficient are little, self lubricity and noise reduction are arranged.The use temperature scope is at-40 ℃～150 ℃; Electrical insulation capability is good, anti-electric arc, but be subject to Temperature Influence; Be easy to painted and nontoxic; Organic solvents such as oil resistant, hydro carbons, ester class, anti-weak base, but not acidproof and oxygenant, not water-fast, alcohols isopolarity solvent; Be easy to machine-shaping.Weak point is that water-intake rate is higher, and dimensional stability is relatively poor.Generally can by strengthen, method of modifying such as toughness reinforcing, filling overcomes its weak point, and other performance is greatly improved.
Reinforced Nylon 6 kind in the market is a lot, and there is very big-difference in Reinforced Nylon 6 rerum naturas of different manufacturers production.In general, external manufacturer such as DUPONT, ASAHI, DSM, BASF etc. have a lot of different grades, as high rigidity, high tenacity, heat-proof aging etc., but fail to satisfy the demand of the high-performance hydrolysis-resistance material of some special dimensions development, must research and development novel high-performance hydrolysis-resistant reinforced nylon 6.
Summary of the invention
The technical issues that need to address of the present invention are to disclose a kind of high-performance hydrolysis-resistance reinforced nylon 6 dragon 6 and preparation method thereof, to overcome the above-mentioned defective that prior art exists, satisfy the demand of some special dimension development.
For this reason, the contriver has proposed following technical scheme:
Said high-performance hydrolysis-resistance reinforced nylon 6 dragon 6, its component and parts by weight comprise:
40～88 parts of Nylon 6s
5～50 parts of non-water-absorbent composite elastic body activation toughner
10～50 parts in glass fibre
Said non-water-absorbent composite elastic body toughner is that to have a polyolefine of different chemical structures and component compound, the mixture that the process priming reaction makes, this mixture promptly has excellent polarity and has good toughness and rigidity again, thereby played extraordinary compatibilization effect between nylon 6 and glass, simultaneously because this composite elastic body activation toughner is non-water-absorbent mixture, its adding can effectively reduce the water-intake rate of system, and weakened the destructiveness of water greatly, thereby inflexible keeps having played positive effect after making material immersion and boiling to nylon 6 and glass interface;
Polyolefine with different chemical structures and molecular weight is to adopt the feedstock production comprise following parts by weight:
10～90 parts of ethylene-octene copolymer POE
20～90 parts of propylene diene three component system multipolymer EPDM
10～30 parts of polypropylene PP
5～40 parts of polythene PEs
Catalyzer 0.1-5 part
Activator 0.5-10 part
Said catalyzer is selected from two (tert-butyl peroxide) diisopropylbenzene(DIPB)s, dicumyl peroxide, 2,5-dimethyl-2, two (tert-butyl hydroperoxide) hexanes of 5-, di-t-butyl peroxide, 2,5-dimethyl-2, two (tert-butyl hydroperoxide) hexin benzene of 5-, tert-butyl peroxide trimethyl silane, right-isopropyl methyl cyclohexyl hydroperoxidation benzene or two-tertiary butyl-one or more mixtures such as diperoxy benzoic ether;
Activator is selected from ethylene/methyl acrylate/toxilic acid-ethyl ester, Ethylene/vinyl acetate/maleic anhydride, ethyl propenoate/rich horse calculation-ethyl ester, ethyl propenoate/maleic anhydride, glycidyl ester, glycine acrylate, maleimide (as N, a N '-benzene bismaleimides) etc. and uses separately or compound use;
Said glass fibre can adopt conventional glass fibre; the preferred glass fibre that adopts the combined polarity collecting agent to handle; the glass fibre that said combined polarity collecting agent is handled is a kind of commercially available prod; the trade mark as the preparation of Chongqing matrix material company limited is the glass fibre of SRW-1000TEX; the present invention most preferably adopts glass fibre of handling through composite coupler or the glass fibre of handling through composite coupler processing and combined polarity collecting agent; can play extraordinary enhancement to material; make material have high strength and high-modulus; because the effect of composite coupler and combined polarity collecting agent; make between glass fibre and Nylon 6 and non-water-absorbent composite elastic body toughner and formed firm bonding interface; suppress water molecules and entered interfacial layer; good protective action has been played at the interface, thereby can keep favorable rigidity after making material immersion and boiling.
Adopt composite coupler to handle the method for the glass fibre of combined polarity collecting agent processing, report is all arranged on many documents;
Said composite coupler parts by weight are:
Being 100 parts with water is benchmark, 1～15 part of phosphate coupling agent, 1～10 part of silane coupling agent, 0.5～10 part of Resins, epoxy, 1～15 part of glycidyl ester;
The chemical name of phosphate coupling agent is single siloxy pyrophosphate coupling agent, and can adopt the trade mark is the product of PN-179;
The chemical general formula of silane coupling agent is Y (CH2) nSIX3, organo-functional groups such as Y-alkyl, phenyl, epoxy group(ing), amino, and can adopt the trade mark is sulfydryl-β (3, the 4-epoxycyclohexyl) ethyl-trimethyl silane or Y-glycidoxypropyltrimewasxysilane.
The method for preparing above-mentioned high-performance hydrolysis-resistance reinforced nylon 6 dragon 6 comprises the steps:
Earlier catalyzer, activator and dispersion agent are used ball milling mixing machine premix, polyolefine with different chemical structures and molecular weight mixes through high mixer again, enter into twin screw extruder then, frit reaction under 170～260 ℃ temperature, extruding pelletization promptly obtain required non-water-absorbent composite elastic body activation toughner;
Dispersion agent is selected low molecule lipid for use, and the mixture of preferred stearylamide or group photo resin acid calcium, the consumption of dispersion agent are 0.3～5.0 part of polyolefine gross weight umber of different chemical structures;
After will obtaining non-water-absorbent composite elastic body activation toughner and Nylon 6 consolute then, with the glass fibre extruding pelletization, melt extruding temperature range is 220～280 ℃, promptly obtains high-performance hydrolysis-resistance reinforced nylon 6 dragon 6 of the present invention.
Product of the present invention can adopt national standard, detects.Test sample, by CJ80NC type injection moulding machine 260 ℃ of following injection mouldings.
The testing method of physical and mechanical properties:
1). tensile strength
Press the GB1040 test
Pulling experiment machine model: LJ-1000 speed: 10mm/min
2). elongation at break
Press the GB1040 test
Pulling experiment machine model: LJ-1000 speed: 10mm/min
3). the socle girder notched Izod impact strength
Press the GB1843 test
Impact experiment machine model: XJU-22
4). melt flow rate (MFR)
Press the GB3682 test
Melt flow rate (MFR) instrument model: XNR-400250 ℃/2.16Kg standard mouth mould internal diameter 2.095mm
5). flexural strength
Press the GB9341 test
Pulling experiment machine model: LJ-1000 speed: 2mm/min
6). flame retardant properties testing level combustion method
Press the test of UL 94 horizontal firing methods
Burning instrument model: ATLAS-HVUL
7). heat-drawn wire
Press the GB1634 test
8). proportion
Press the GB1033-86 test
9). content of glass fiber
Press the ISO3451/1 test
10). resistance to hydrolysis
Boil 100h in the boiling water, test flexural strength conservation rate.
Adopt the aforesaid method detected result to show, every performance of said high-performance hydrolysis-resistance reinforced nylon 6 dragon 6 materials all meets or exceeds the expectation index requirement, has solved the problem that rigidity descends significantly behind material immersion and the poach.Make material have excellent resistance to hydrolysis energy, and in boiling water behind the boiling 100h flexural strength of material still can remain on more than 65%.
Embodiment
The major equipment of the production product that adopts has:
High-speed mixer: rotating speed 350-1300 rev/min
Twin screw extruder: engine speed 250-500rpm
Barrel zone temperature: 220-280 ℃
Tank: water temperature 20-60 ℃
Dicing machine: rotating speed 400-700rpm.
Embodiment 1
With 35 kilograms of ethylene-octene copolymer POE elastomericss, 25 kilograms of propylene diene three component system multipolymer EPDM rubber, 20 kilograms of polypropylene PP resins, 17 kilograms of polythene PE resins, the mixture of 1 kilogram of two (tert-butyl peroxide) diisopropylbenzene(DIPB) and tert-butyl peroxide trimethyl silane, 2 kilograms of glycidyl esters and maleimide are (as N, a N '-benzene bismaleimides) mixture elder generation premix mixes through high mixer again, enter into twin screw extruder then, under 170～260 ℃ temperature, each section temperature is followed successively by: 170 ± 10 ℃, and 190 ± 10 ℃, 210 ± 10 ℃, 240 ± 10 ℃, 220 ± 10 ℃, 220 ± 10 ℃, 210 ± 10 ℃, 210 ± 10 ℃, 210 ± 10 ℃, 210 ± 10 ℃, frit reaction, extruding pelletization promptly obtains required non-water-absorbent composite elastic body activation toughner.
With 64 kilograms of Nylon 6s, 5 kilograms of non-water-absorbent composite elastic body activation toughner, glass fibre that 30 kilograms of phosphoric acid ester and silane composite coupler and Resins, epoxy and glycidyl ester combined polarity collecting agent are handled and 1 kilogram the compound low molecule lipid of dispersion agent, commodity are called MTJ2045, in the forcing machine of screw combinations, melt extrude granulation, melt extruding temperature is 220～270 ℃, each section temperature is followed successively by: 230 ± 10 ℃, and 240 ± 10 ℃, 250 ± 10 ℃, 250 ± 10 ℃, 260 ± 10 ℃, 260 ± 10 ℃, 250 ± 10 ℃, 250 ± 10 ℃, 240 ± 10 ℃, 240 ± 10 ℃, promptly obtain high-performance hydrolysis-resistance reinforced nylon 6 dragon 6 of the present invention.
Above-mentioned product is detected its result such as following table:
| Performance | Testing method | Unit | Embodiment 1 | ||
| Proportion | GB1033 | g/cm3 | 1.35 | ||
| Melt index | GB3682 | g/10min. | 16.3 | ||
| Tensile strength | GB1040 | MPa | 165 | ||
| Elongation at break | GB1040 | ％ | 3.5 | ||
| Flexural strength | GB9341 | MPa | 245 | ||
| Modulus in flexure | GB9341 | MPa | 8000 | ||
| Notched Izod impact strength | GB1843 | KJ/m 2 | 18.5 | ||
| Heat-drawn wire (1.82MPa) | GB1634 | ℃ | 210 | ||
| Flame retardant resistance | UL 94 | 1.6mm | HB | ||
| 3.0mm | HB | ||||
| Resistance to hydrolysis energy 1 | Flexural strength | GB9341 | 50 hours | ％ | 77.5 |
| 100 hours | 68.1 | ||||
| Resistance to hydrolysis energy 2 | Modulus in flexure | GB9341 | 50 hours | ％ | 73.6 |
| 100 hours | 65.8 | ||||
Embodiment 2
With 35 kilograms of ethylene-octene copolymer POE elastomericss, 25 kilograms of propylene diene three component system multipolymer EPDM rubber, 20 kilograms of polypropylene PP resins, 17 kilograms of polythene PE resins, the mixture of 1 kilogram of two (tert-butyl peroxide) diisopropylbenzene(DIPB) and tert-butyl peroxide trimethyl silane, 2 kilograms of glycidyl esters and maleimide are (as N, a N '-benzene bismaleimides) mixture elder generation premix mixes through high mixer again, enter into twin screw extruder then, under 170～260 ℃ temperature, each section temperature is followed successively by: 170 ± 10 ℃, and 190 ± 10 ℃, 210 ± 10 ℃, 240 ± 10 ℃, 220 ± 10 ℃, 220 ± 10 ℃, 210 ± 10 ℃, 210 ± 10 ℃, 210 ± 10 ℃, 210 ± 10 ℃, frit reaction, extruding pelletization promptly obtains required non-water-absorbent composite elastic body activation toughner.
15 kilograms of non-water-absorbent composite elastic body activation toughner, 53 kilograms of Nylon 6s mix, join blend in the twin screw extruder of specific screw combinations, the glass fibre that 30 kilograms of composite couplers and combined polarity collecting agent are handled and 2 kilograms of dispersion agents are in screw extrusion press, melt extrude granulation, melt extruding temperature is 220～280 ℃, each section temperature is followed successively by: 230 ± 10 ℃, and 240 ± 10 ℃, 240 ± 10 ℃, 250 ± 10 ℃, 250 ± 10 ℃, 260 ± 10 ℃, 270 ± 10 ℃, 260 ± 10 ℃, 250 ± 10 ℃, 250 ± 10 ℃, promptly obtain high-performance hydrolysis-resistance reinforced nylon 6 dragon 6 of the present invention.
Above-mentioned product is detected its result such as following table:
| Performance | Testing method | Unit | Embodiment 2 | |
| Proportion | GB1033 | g/cm3 | 1.35 | |
| Melt index | GB3682 | g/10min. | 14.5 | |
| Tensile strength | GB1040 | MPa | 145 | |
| Elongation at break | GB1040 | ％ | 4.0 | |
| Flexural strength | GB9341 | MPa | 190 | |
| Modulus in flexure | GB9341 | MPa | 7000 | |
| Notched Izod impact strength | GB1843 | KJ/m 2 | 27.5 | |
| Heat-drawn wire | GB1634 | ℃ | 200 | |
| Flame retardant resistance | UL 94 | 1.6mm | HB | |
| 3.0mm | HB | |||
| Resistance to hydrolysis can 1 flexural strength | GB9341 | 50 hours | ％ | 83.5 |
| 100 hours | 74.8 | |||
| Resistance to hydrolysis can 2 modulus in flexurees | GB9341 | 50 hours | 79.7 | |
| 100 hours | 71.1 | |||
Claims (5)
1. a high-performance hydrolysis-resistance reinforced nylon 6 dragon 6 is characterized in that, component and parts by weight comprise:
40～88 parts of Nylon 6s
5～50 parts of non-water-absorbent composite elastic body activation toughner
10～50 parts in glass fibre
Said non-water-absorbent composite elastic body toughner is that to have a polyolefine of different chemical structures and component compound, the mixture that makes through priming reaction.
2. high-performance hydrolysis-resistance reinforced nylon 6 dragon 6 according to claim 1 is characterized in that, the polyolefine with different chemical structures and molecular weight is to adopt the feedstock production comprise following parts by weight:
10～90 parts of ethylene-octene copolymer POE
20～90 parts of propylene diene three component system multipolymer EPDM
10～30 parts of polypropylene PP
5～40 parts of polythene PEs
Catalyzer 0.1-5 part
Activator 0.5-10 part
Said catalyzer is selected from two (tert-butyl peroxide) diisopropylbenzene(DIPB)s, dicumyl peroxide, 2,5-dimethyl-2, two (tert-butyl hydroperoxide) hexanes of 5-, di-t-butyl peroxide, 2,5-dimethyl-2, one or more mixtures in two (tert-butyl hydroperoxide) hexin benzene of 5-, tert-butyl peroxide trimethyl silane, right-isopropyl methyl cyclohexyl hydroperoxidation benzene or the two-tertiary butyl-diperoxy benzoic ether;
Activator is selected from one or more mixtures in ethylene/methyl acrylate/toxilic acid-ethyl ester, Ethylene/vinyl acetate/maleic anhydride, ethyl propenoate/rich horse calculation-ethyl ester, ethyl propenoate/maleic anhydride, glycidyl ester, glycine acrylate or the maleimide.
3. high-performance hydrolysis-resistance reinforced nylon 6 dragon 6 according to claim 1, it is characterized in that said glass fibre adopts the glass fibre of combined polarity collecting agent processing or adopts the glass fibre of handling through composite coupler or the glass fibre of handling through composite coupler processing and combined polarity collecting agent.
4. high-performance hydrolysis-resistance reinforced nylon 6 dragon 6 according to claim 1 is characterized in that, said composite coupler parts by weight are:
Being 100 parts with water is benchmark, 1～15 part of phosphate coupling agent, 1～10 part of silane coupling agent, 0.5～10 part of Resins, epoxy, 1～15 part of glycidyl ester.
5. prepare the method for each described high-performance hydrolysis-resistance reinforced nylon 6 dragon 6 of claim 1～4, it is characterized in that, comprise the steps:
Earlier catalyzer, activator and dispersion agent are used ball milling mixing machine premix, polyolefine with different chemical structures and molecular weight mixes through high mixer again, enter into twin screw extruder then, frit reaction under 170～260 ℃ temperature, extruding pelletization promptly obtain required non-water-absorbent composite elastic body activation toughner;
Dispersion agent is selected low molecule lipid for use, and the consumption of dispersion agent is 0.3～5.0 part of polyolefine gross weight umber of different chemical structures;
After will obtaining non-water-absorbent composite elastic body activation toughner and Nylon 6 consolute then, with the glass fibre extruding pelletization, melt extruding temperature range is 220～280 ℃, promptly obtains high-performance hydrolysis-resistance reinforced nylon 6 dragon 6 of the present invention.
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| Application Number | Priority Date | Filing Date | Title |
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| CNA2006100298514A CN101121818A (en) | 2006-08-09 | 2006-08-09 | High-performance hydrolysis-resistance reinforced nylon 6 and preparation method thereof |
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|---|---|---|---|
| CNA2006100298514A CN101121818A (en) | 2006-08-09 | 2006-08-09 | High-performance hydrolysis-resistance reinforced nylon 6 and preparation method thereof |
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| CN102558837A (en) * | 2010-12-21 | 2012-07-11 | 上海日之升新技术发展有限公司 | Low temperature impact resistant nylon flexibilizer and preparation method of low temperature impact resistant nylon flexibilizer |
| CN103641958A (en) * | 2013-11-22 | 2014-03-19 | 江苏恒峰线缆有限公司 | Low water absorption nylon 66 and preparation method thereof |
| CN101875778B (en) * | 2009-04-28 | 2014-05-14 | 上海金发科技发展有限公司 | Super-toughened nylon alloy and preparation process thereof |
| CN104177825A (en) * | 2014-08-27 | 2014-12-03 | 东莞市卡尔文塑胶科技有限公司 | Polyamide toughening agent as well as preparation method and use thereof |
| CN104292821A (en) * | 2014-09-26 | 2015-01-21 | 宁波能之光新材料科技有限公司 | Nylon toughening masterbatch and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101875778B (en) * | 2009-04-28 | 2014-05-14 | 上海金发科技发展有限公司 | Super-toughened nylon alloy and preparation process thereof |
| CN102558837A (en) * | 2010-12-21 | 2012-07-11 | 上海日之升新技术发展有限公司 | Low temperature impact resistant nylon flexibilizer and preparation method of low temperature impact resistant nylon flexibilizer |
| CN103641958A (en) * | 2013-11-22 | 2014-03-19 | 江苏恒峰线缆有限公司 | Low water absorption nylon 66 and preparation method thereof |
| CN103641958B (en) * | 2013-11-22 | 2016-05-18 | 江苏恒峰线缆有限公司 | A kind of low water absorption nylon 66 and preparation method thereof |
| CN104177825A (en) * | 2014-08-27 | 2014-12-03 | 东莞市卡尔文塑胶科技有限公司 | Polyamide toughening agent as well as preparation method and use thereof |
| CN104292821A (en) * | 2014-09-26 | 2015-01-21 | 宁波能之光新材料科技有限公司 | Nylon toughening masterbatch and preparation method thereof |
| CN107090177A (en) * | 2017-06-12 | 2017-08-25 | 中车石家庄车辆有限公司 | A kind of tank car nylon saddle pad |
| CN107090177B (en) * | 2017-06-12 | 2020-06-12 | 中车石家庄车辆有限公司 | Nylon saddle cushion of railway tank car |
| CN109504080A (en) * | 2018-12-13 | 2019-03-22 | 沈阳科通塑胶有限公司 | A kind of enhancing nylon of hydrolysis and preparation method thereof |
| CN115073917A (en) * | 2022-06-30 | 2022-09-20 | 金旸（厦门）新材料科技有限公司 | Nylon fishing net composite material and preparation method thereof |
| CN115073917B (en) * | 2022-06-30 | 2023-05-09 | 金旸（厦门）新材料科技有限公司 | Nylon fishing net composite material and preparation method thereof |
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Application publication date: 20080213 |