CN104497304A - High-liquidity and high-temperature nylon resin, fiber-reinforced nylon and preparation method of nylon resin - Google Patents
High-liquidity and high-temperature nylon resin, fiber-reinforced nylon and preparation method of nylon resin Download PDFInfo
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Abstract
The invention discloses a high-liquidity and high-temperature nylon resin, a fiber-reinforced nylon and a preparation method of the nylon resin. The nylon is prepared from the following components in percentage by weight: 45%-90% of high-liquidity and high-temperature nylon, 5%-50% of fiber, 0.05%-5% of a fiber processing agent, 0.05%-3% of an antioxidant, 0.05%-3% of a plasticizer, 0.05%-3% of a coupling reagent and 0.15%-5% of an assistant. The high-liquidity and high-temperature nylon is modified by adding the fiber; the liquidity of the obtained modified high-liquidity and high-temperature nylon does not change; the mechanical strength is improved; other excellent properties such as high temperature resistance and wear-resisting property are kept; and meanwhile, the preparation method disclosed by the invention is simple in process and excellent in effect.
Description
Technical field
The present invention relates to high-temperature nylon field, be specifically related to a kind of high workability high-temperature nylon resin, and fibre-reinforced high workability high-temperature nylon and preparation method.
Background technology
Under high-tech promotion, plastics technology obtains and develops rapidly, and researchist constantly works out type material and comes alternative traditional metal and timber.In recent years, along with the development in market, the performance of structural elements to metal substitute material (plastics) of automobile, engineering machinery, power tool and sport-goods trade is had higher requirement.Not only the requirement mechanical property that will have, also will improve its dimensional stability and low molding shrinkage.Polymeric amide is positioned at first of five large-engineering plastics (PA, POM, PC, PPO, PBT) always, current domestic and international application the most a kind of engineering plastics, there is tough wear-resisting, shock-resistant, antifatigue, corrosion-resistant, resistance to wet goods excellent specific property, can physics and chemistry modification be carried out.
Wherein high-temperature nylon due to can resistance to 180 DEG C be even greater than the continuous high temperature of 180 DEG C, good resistance to elevated temperatures can be brought for some parts, therefore more and more welcomed by the people, be used widely, for meeting the needs of different field, usually further modification is carried out to it, to improve high-temperature nylon performance in a certain respect, as mechanical property etc., but usually the membership that adds of properties-correcting agent makes its mobility be deteriorated, and easily causes high-temperature nylon orientation, anisotropy, when making machine-shaping, internal stress is large, easy contraction, and product size is not easy to control.
As the performance in order to improve high-temperature nylon, patent CN10176006A, CN102344671A, CN102344666A, CN102344664A, CN101704996A, CN103788624A, CN104072982A improve the mechanical strength of high-temperature nylon by various toughener, weighting material and the mixture of the two, maintain its high-temperature stability simultaneously, but the interpolation of these materials greatly reduces the mobility of high-temperature nylon, be unfavorable for injection moulding or extrude.Patent CN103788624A utilizes situ aggregation method to carry out modification to high-temperature nylon, the orientation of the uncontrollable toughener of this method of modifying in high-temperature nylon, and the orientation of toughener in high-temperature nylon directly affects its performance, also can cause the discharging difficulty of modification high-temperature nylon simultaneously.
From the above mentioned, its flowing property must be ensured when improving other performances of high-temperature nylon, otherwise the use field of high-temperature nylon can be limited.
Summary of the invention
The technical problem to be solved in the present invention is: provide a kind of high workability high-temperature nylon resin, fibre-reinforced high workability high-temperature nylon and preparation method thereof, the fiber reinforced nylon obtained not only has excellent mechanical property but also have good mobility.
The solution that the present invention solves its technical problem is: a kind of high workability high-temperature nylon resin, add in deionized water by the amorphous nylon salt of 40-60 weight part high-temperature nylon salt, 20-60 weight part, 0.5-10 weight part polyamines, then corresponding auxiliary agent is added, after nitrogen purging, improving reaction system pressure is 1 ~ 4MPa; Be warming up to 200 ~ 250 DEG C, then keep 1 ~ 10h, carry out copolymerization, obtain prepolymer; Then by prepolymer in a nitrogen atmosphere or under vacuum condition, 180 ~ 250 DEG C, reaction 3 ~ 15h obtains.
Preferably, the relative viscosity of described high workability high-temperature nylon resin is 2.0 ~ 3.0, and fusing point is 270 DEG C ~ 330 DEG C.
Preferably, described high-temperature nylon salt is one or more in nylon 6T salt, nylon 7T salt, nylon 8 T salt, nylon 9 T salt, nylon 10T salt, nylon 11 T salt, nylon 12T salt, nylon 6I salt, nylon 7I salt, nylon 8 I salt, nylon 9 I salt, nylon 10I salt, nylon 11 I salt and nylon 12I salt, is further preferably the one or more than one in nylon 6T salt, nylon 7T salt, nylon 8 T salt, nylon 9 T salt, nylon 10T salt, nylon 11 T salt and nylon 12T salt.
Preferably, described amorphous nylon salt is the one or more than one in nylon 46 salt, nylon 6 salt, nylon salt, NYLON610 salt, nylon 612 salt, nylon 9 salt, Nylon-1010 Salt, Nylon 1012 salt, nylon 11 salt, nylon 12 salt and nylon 1212 salt.
Preferably, described polyamines is triaminotriphenyl methylmethane, polymine, diethylenetriamine, triethylene tetramine, polyamide-amide or polyetheramine, further preferably, is polymine or polyetheramine.
Present invention also offers and a kind of the nylon that fiber reinforcement obtains is carried out to above-mentioned high temperature height fluidity nylon resin, be made up of the component of following weight percent: high workability high-temperature nylon resin: 45% ~ 90%, fiber: 5% ~ 50%, fibre finish: 0.05% ~ 5%; Oxidation inhibitor: 0.05% ~ 3%, softening agent: 0.05% ~ 3%, coupling agent: 0.05% ~ 3%, auxiliary agent 0.15% ~ 5%.
Preferably, described fiber is glass fibre, carbon fiber, aramid fiber or whisker.
Preferably, described oxidation inhibitor to be described oxidation inhibitor be in mantoquita, potassiumiodide compound, hindered phenol compound, phosphorous acid lipid and hindered amine compound one or more; Further preferably, be the composite antioxidant of hindered phenol compound and phosphorous acid ester.
Preferably, described auxiliary agent is the one or more than one in thermo-stabilizer, end-capping reagent, molecular weight regulator and catalyzer.
Present invention also offers a kind of preparation method of fiber reinforcement high workability high-temperature nylon, comprise the following steps:
By high workability high-temperature nylon resin 80 DEG C ~ 120 DEG C bakings more than 8 hours;
Fiber fibre finish is carried out pre-treatment, then dries more than 4h at 60 DEG C;
High workability high-temperature nylon resin, pretreated fiber, oxidation inhibitor, softening agent, coupling agent and auxiliary agent after drying are mixed in proportion, then twin screw extruder is added, controlled working temperature is at 290-320 DEG C, and screw speed, at 80-150rpm, melt extrudes granulation;
Pellet 80 DEG C ~ 100 DEG C will be obtained and dry more than 8h, obtain described fiber reinforcement high workability high-temperature nylon.
The invention has the beneficial effects as follows: high workability high-temperature nylon resin of the present invention is by after interpolation fiber reinforcement, the good fluidity of the modification high workability high-temperature nylon obtained, and mechanical strength is improved, other excellent properties such as the performance such as high temperature resistant, wear-resisting have also been obtained maintenance; Preparation method's technique of the present invention is simple simultaneously, excellent effect.
Embodiment
Clear, complete description is carried out, to understand object of the present invention, characteristic sum effect fully below with reference to the technique effect of embodiment to design of the present invention and generation.Obviously; described embodiment is a part of embodiment of the present invention, instead of whole embodiment, based on embodiments of the invention; other embodiments that those skilled in the art obtains under the prerequisite not paying creative work, all belong to the scope of protection of the invention.
A kind of high workability high-temperature nylon resin of the present invention, add in deionized water by the amorphous nylon salt of 40-60 weight part high-temperature nylon salt, 20-60 weight part, 0.5-10 weight part polyamines, then add corresponding auxiliary agent, after nitrogen purging, improving reaction system pressure is 1 ~ 4MPa; Be warming up to 200 ~ 250 DEG C, then keep 1 ~ 10h, carry out copolymerization, obtain prepolymer; Then by prepolymer in a nitrogen atmosphere or under vacuum condition, 180 ~ 250 DEG C, reaction 3 ~ 15h, carries out solid state reaction thickening, thus obtain.Preferably, the relative viscosity of described high workability high-temperature nylon resin is 2.0 ~ 3.0, and fusing point is 270 DEG C ~ 330 DEG C.
The high-temperature nylon salt that wherein synthesis high workability high-temperature nylon resin is used can be the high-temperature nylon salt known by those skilled in that art, be preferably, nylon 6T salt, nylon 7T salt, nylon 8 T salt, nylon 9 T salt, nylon 10T salt, nylon 11 T salt, nylon 12T salt, nylon 6I salt, nylon 7I salt, nylon 8 I salt, nylon 9 I salt, nylon 10I salt, one or more in nylon 11 I salt and nylon 12I salt, be further preferably nylon 6T salt, nylon 7T salt, nylon 8 T salt, nylon 9 T salt, nylon 10T salt, one or more than one in nylon 11 T salt and nylon 12T salt.
Synthesis high workability high-temperature nylon resin amorphous nylon salt used can be the amorphous nylon salt known by those skilled in that art, is preferably one or more in nylon 46 salt, nylon 6 salt, nylon salt, NYLON610 salt, nylon 612 salt, nylon 9 salt, Nylon-1010 Salt, Nylon 1012 salt, nylon 11 salt, nylon 12 salt and nylon 1212 salt.
The polyamines synthesizing high workability high-temperature nylon resin used is preferably, and triaminotriphenyl methylmethane, polymine, diethylenetriamine, triethylene tetramine, polyamide-amide or polyetheramine further preferably, are polymine or polyetheramine.
Auxiliary agent, as catalyzer, end-capping reagent etc., optionally adds one or more auxiliary agents by those skilled in the art according to reaction needed.
Of the present inventionly strengthen by above-mentioned high workability high-temperature nylon resin fibre the nylon obtained, be made up of the component of following weight percent: high workability high-temperature nylon resin: 45% ~ 90%, fiber: 5% ~ 50%, fibre finish: 0.05% ~ 5%; Oxidation inhibitor: 0.05% ~ 3%, softening agent: 0.05% ~ 3%, coupling agent: 0.05% ~ 3%, auxiliary agent 0.15% ~ 5%.
The fiber added is preferably glass fibre, carbon fiber, aramid fiber or whisker.Used fibre finish is fibre finish conventional in this area, as silicane fibre finish etc.
Oxidation inhibitor be preferably in mantoquita, potassiumiodide compound, hindered phenol compound, phosphorous acid lipid and hindered amine compound one or more; Further preferably, be the composite antioxidant of hindered phenol compound and phosphorous acid ester.
Wherein mantoquita is selected from neutralized verdigris, cupric iodide or its composition; Hindered phenol compound is selected from oxidation inhibitor 1098, antioxidant 1010, antioxidant 2246, antioxidant 1076 or its combination; Phosphorous acid lipid is selected from irgasfos 168, oxidation inhibitor 626, oxidation inhibitor 439, oxidation inhibitor H10 or its combination; Hindered amine compound is selected from N, N '-hexa-methylene-bis--3-(3,5-di-tert-butyl-hydroxy phenyl) acetone amine, oxidation inhibitor DNP, oxidation inhibitor 4010 or its combination.
Described auxiliary agent is the one or more than one in thermo-stabilizer, end-capping reagent, molecular weight regulator and catalyzer.According to reaction needed, select to add wherein one or more.
Of the present inventionly additionally provide a kind of fiber reinforcement high workability high-temperature nylon preparation method, comprise the following steps:
By high workability high-temperature nylon resin 80 DEG C ~ 120 DEG C bakings more than 8 hours;
Fiber fibre finish is carried out pre-treatment, then dries more than 4h at 60 DEG C;
High workability high-temperature nylon resin, pretreated fiber, oxidation inhibitor, softening agent, coupling agent and auxiliary agent after drying are mixed in proportion, then twin screw extruder is added, controlled working temperature is at 290-320 DEG C, screw speed is at 80-150rpm, melt extrude granulation, pellet 80 DEG C ~ 100 DEG C will be obtained again and dry more than 8h, obtain described fiber reinforcement high workability high-temperature nylon.
Embodiment 1
1) synthesis of high workability high-temperature nylon resin
Particularly, by 45 portions of nylon 6T salt and, 55 parts of nylon salts, 2 parts of triaminotriphenyl methylmethanes add in deionized water, then add end-capping reagent 2 parts, after nitrogen purging, improving reaction system pressure is 3.0MPa; Heat up 230 DEG C, then keep 5h, carry out copolymerization, obtain prepolymer; Then in a nitrogen atmosphere or under vacuum condition, temperature is 180 DEG C, reaction 15h, carry out solid state reaction thickening, thus obtain described high workability high-temperature nylon resin, the relative viscosity of described high workability high-temperature nylon resin is 2.2; Fusing point is 285 DEG C.
2) preparation of fiber reinforcement high workability high-temperature nylon
2.1 by step 1) in the high workability high-temperature nylon resin that obtains 80 DEG C of bakings 12 hours.
35 parts of glass fibre, 3 portions of fibre finishs are carried out pre-treatment by 2.2, then dry more than 4h at 60 DEG C.
High workability high-temperature nylon resin, pretreated glass fibre, the neutralized verdigris oxidation inhibitor of 0.8 part, the softening agent of 1 part, 0.05 part of coupling agent, 0.15 part of end-capping reagent after the drying of 60 parts mix by 2.3, then twin screw extruder is added, controlled working temperature is at 290-320 DEG C, screw speed, at 80rpm, melt extrudes granulation.
2.4 will obtain pellet 80 DEG C dries more than 10h, obtains described fiber reinforcement high workability high-temperature nylon.
The processing parameter melt extruded is as shown in table 1.
Embodiment 2
1) synthesis of high workability high-temperature nylon resin
Particularly, add in deionized water, then add end-capping reagent 2 parts by 50 portions of nylon 6T salt, 50 parts of nylon salts, 1 part of diethylenetriamine, after nitrogen purging, improving reaction system pressure is 1MPa; Heat up 240 DEG C, then keep 4h, carry out copolymerization, obtain prepolymer; Then in a nitrogen atmosphere or under vacuum condition, temperature is 250 DEG C, reaction 4h, carry out solid state reaction thickening, thus obtain described high workability high-temperature nylon resin, the relative viscosity of described high workability high-temperature nylon resin is 2.4; Fusing point is 280 DEG C.
2) preparation of fiber reinforcement high workability high-temperature nylon
2.1 by step 1) in the high workability high-temperature nylon resin that obtains 100 DEG C of bakings 10 hours.
10 parts of carbon fibers, 1 portion of fibre finish is carried out pre-treatment by 2.2, then dries more than 4h at 60 DEG C.
High workability high-temperature nylon resin, pretreated carbon fiber, oxidation inhibitor 1098,1 part of coupling agent of 1 part, the molecular weight regulator of 0.5 part after the drying of 86.5 parts mix by 2.3, then twin screw extruder is added, controlled working temperature is at 290-320 DEG C, screw speed, at 120rpm, melt extrudes granulation.
2.4 will obtain pellet 85 DEG C dries 13h, obtains described fiber reinforcement high workability high-temperature nylon.
The processing parameter melt extruded is as shown in table 1.
Embodiment 3
1) synthesis of high workability high-temperature nylon resin
Particularly, by 40 portions of nylon 6T salt, 10 parts of nylon 12 salt, 20 parts of nylon salts, 0.5 part of triethylene tetramine adds in deionized water, then adds catalyzer 2 parts, and after nitrogen purging, improving reaction system pressure is 3.8MPa; Heat up 250 DEG C, then keep 8h, carry out copolymerization, obtain prepolymer; Then in a nitrogen atmosphere or under vacuum condition, temperature is 200 DEG C, reaction 10h, carry out solid state reaction thickening, thus obtain described high workability high-temperature nylon resin, the relative viscosity of described high workability high-temperature nylon resin is 2.5; Fusing point is 290 DEG C.
2) preparation of fiber reinforcement high workability high-temperature nylon
2.1 by step 1) in the high workability high-temperature nylon resin that obtains 110 DEG C of bakings 12 hours.
30 parts of aramid fibers, 3 portions of fibre finishs are carried out pre-treatment by 2.2, then dry more than 4h at 60 DEG C.
High workability high-temperature nylon resin after the drying of 61 parts, pretreated aramid fiber, oxidation inhibitor 1098,1 part of irgasfos 168 of 1 part, the softening agent of 3 parts, 0.5 part of coupling agent, the molecular weight regulator of 0.5 part mix by 2.3, then twin screw extruder is added, controlled working temperature is at 290-320 DEG C, screw speed, at 100rpm, melt extrudes granulation.
2.4 will obtain pellet 80 DEG C dries 8.5h, obtains described fiber reinforcement high workability high-temperature nylon.
The processing parameter melt extruded is as shown in table 1.
Embodiment 4
1) synthesis of high workability high-temperature nylon resin
Particularly, add in deionized water, then add end-capping reagent 2 parts by 50 portions of nylon 6T salt and 10 parts of nylon 6I salt, 20 parts of Nylon 1012 salt, 4 parts of polymines and 4 parts of polyetheramines, after nitrogen purging, improving reaction system pressure is 3MPa; Heat up 230 DEG C, then keep 3h, carry out copolymerization, obtain prepolymer; Then in a nitrogen atmosphere or under vacuum condition, temperature is 220 DEG C, reaction 8h, carry out solid state reaction thickening, thus obtain described high workability high-temperature nylon resin, the relative viscosity of described high workability high-temperature nylon resin is 2.2; Fusing point is 310 DEG C.
2) preparation of fiber reinforcement high workability high-temperature nylon
2.1 by step 1) in the high workability high-temperature nylon resin that obtains 95 DEG C of bakings 15 hours.
50 parts of whiskers, 3.5 portions of fibre finishs are carried out pre-treatment by 2.2, then dry more than 4h at 60 DEG C.
High workability high-temperature nylon resin after the drying of 45 parts, pretreated filler, the oxidation inhibitor DNP of 0.05 part, the softening agent of 0.05 part, 1.2 parts of coupling agents, the end-capping reagent of 0.2 part mix by 2.3, then twin screw extruder is added, controlled working temperature is at 290-320 DEG C, screw speed, at 150rpm, melt extrudes granulation.
2.4 will obtain pellet 95 DEG C dries 10h, obtains described fiber reinforcement high workability high-temperature nylon.
The processing parameter melt extruded is as shown in table 1.
Comparative example:
Carrying out drying by synthesizing the high workability high-temperature nylon resin obtained in embodiment 1, not carrying out fiberfill fibers modification, directly according to the procession parameters of embodiment 1, extruding melt pelletization.
To the nylon pellet implementing to obtain in 1-3 and comparative example 1, adopt condition as shown in table 2 to carry out injection moulding and obtain standard test specimen, carry out performance test by GB/T 1040-1992 and GB/T 9341-2008, the results are shown in Table 3.
Table 1 twin screw extruder processing condition
Table 2 precise injection machine processing condition
The performance test results of table 3 fiber reinforcement height flowing high-temperature nylon
Above better embodiment of the present invention is illustrated, but the invention is not limited to described embodiment, those of ordinary skill in the art also can make all equivalent modifications or replacement under the prerequisite without prejudice to spirit of the present invention, and these equivalent modification or replacement are all included in the application's claim limited range.
Claims (10)
1. a high workability high-temperature nylon resin, it is characterized in that: be add in deionized water by the amorphous nylon salt of 40-60 weight part high-temperature nylon salt, 20-60 weight part, 0.5-10 weight part polyamines, then corresponding auxiliary agent is added, after nitrogen purging, improving reaction system pressure is 1 ~ 4MPa; Be warming up to 200 ~ 250 DEG C, then keep 1 ~ 10h, carry out copolymerization, obtain prepolymer; Then by prepolymer in a nitrogen atmosphere or under vacuum condition, 180 ~ 250 DEG C, reaction 3 ~ 15h obtains.
2. high workability high-temperature nylon resin according to claim 1, is characterized in that, relative viscosity is 2.0 ~ 3.0, and fusing point is 270 DEG C ~ 330 DEG C.
3. high workability high-temperature nylon resin according to claim 1, it is characterized in that, described high-temperature nylon salt is one or more in nylon 6T salt, nylon 7T salt, nylon 8 T salt, nylon 9 T salt, nylon 10T salt, nylon 11 T salt, nylon 12T salt, nylon 6I salt, nylon 7I salt, nylon 8 I salt, nylon 9 I salt, nylon 10I salt, nylon 11 I salt and nylon 12I salt.
4. high workability high-temperature nylon resin according to claim 1, it is characterized in that, described amorphous nylon salt is one or more in nylon 46 salt, nylon 6 salt, nylon salt, NYLON610 salt, nylon 612 salt, nylon 9 salt, Nylon-1010 Salt, Nylon 1012 salt, nylon 11 salt, nylon 12 salt and nylon 1212 salt.
5. high workability high-temperature nylon resin according to claim 1, is characterized in that, described polyamines is triaminotriphenyl methylmethane, polymine, diethylenetriamine, triethylene tetramine, polyamide-amide or polyetheramine.
6. a fiber reinforcement high workability high-temperature nylon, is characterized in that: be made up of the component of following weight percent: high workability high-temperature nylon resin: 45% ~ 90%, fiber: 5% ~ 50%, fibre finish: 0.05% ~ 5%; Oxidation inhibitor: 0.05% ~ 3%, softening agent: 0.05% ~ 3%, coupling agent: 0.05% ~ 3%, auxiliary agent 0.15% ~ 5%;
Described high workability high-temperature nylon resin is the high workability high-temperature nylon resin described in any one of claim 1-5.
7. fiber reinforcement high workability high-temperature nylon according to claim 6, is characterized in that,
Described fiber is glass fibre, carbon fiber, aramid fiber or whisker.
8. fiber reinforcement high workability high-temperature nylon according to claim 6, is characterized in that,
Described oxidation inhibitor is one or more in mantoquita, potassiumiodide compound, hindered phenol compound, phosphorous acid lipid and hindered amine compound.
9. fiber reinforcement high workability high-temperature nylon according to claim 6, is characterized in that,
Described auxiliary agent is the one or more than one in thermo-stabilizer, end-capping reagent, molecular weight regulator, toughner and catalyzer.
10. a preparation method for fiber reinforcement high workability high-temperature nylon, is characterized in that: comprise the following steps:
By high workability high-temperature nylon resin 80 DEG C ~ 120 DEG C bakings more than 8 hours;
Fiber fibre finish is carried out pre-treatment, then dries more than 4h at 60 DEG C;
High workability high-temperature nylon resin, pretreated fiber, oxidation inhibitor, softening agent, coupling agent and auxiliary agent after drying are mixed in proportion, then twin screw extruder is added, controlled working temperature is at 290-320 DEG C, and screw speed, at 80-150rpm, melt extrudes granulation;
Pellet 80 DEG C ~ 100 DEG C will be obtained and dry more than 8h, obtain described fiber reinforcement high workability high-temperature nylon.
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| CN104817831A (en) * | 2015-05-21 | 2015-08-05 | 国网智能电网研究院 | Electric-insulation thermoplastic resin composition and preparation method thereof |
| CN107629205A (en) * | 2017-10-20 | 2018-01-26 | 广州市万佳成塑料有限公司 | A kind of production method of the low molecule amount nylon 46 powder synthesis resin of high molecular weight nylon 46 |
| EP3290459A4 (en) * | 2015-04-29 | 2019-01-02 | Lotte Advanced Materials Co., Ltd. | Polyamide resin, polyamide resin composition containing same, preparation method therefor, and molded product including same |
| CN113308112A (en) * | 2021-06-17 | 2021-08-27 | 东莞市鑫塑源塑胶科技有限公司 | Yellowing-resistant PA6 reinforced material and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| EP3290459A4 (en) * | 2015-04-29 | 2019-01-02 | Lotte Advanced Materials Co., Ltd. | Polyamide resin, polyamide resin composition containing same, preparation method therefor, and molded product including same |
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| CN113308112A (en) * | 2021-06-17 | 2021-08-27 | 东莞市鑫塑源塑胶科技有限公司 | Yellowing-resistant PA6 reinforced material and preparation method and application thereof |
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