CN112812550A - High-glossiness glass fiber reinforced polyamide composite material and preparation method thereof - Google Patents
High-glossiness glass fiber reinforced polyamide composite material and preparation method thereof Download PDFInfo
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/20—Compounding polymers with additives, e.g. colouring
- C08J3/22—Compounding polymers with additives, e.g. colouring using masterbatch techniques
- C08J3/226—Compounding polymers with additives, e.g. colouring using masterbatch techniques using a polymer as a carrier
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- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/04—Reinforcing macromolecular compounds with loose or coherent fibrous material
- C08J5/0405—Reinforcing macromolecular compounds with loose or coherent fibrous material with inorganic fibres
- C08J5/043—Reinforcing macromolecular compounds with loose or coherent fibrous material with inorganic fibres with glass fibres
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- C08J2377/00—Characterised by the use of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Derivatives of such polymers
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- C08J2477/00—Characterised by the use of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Derivatives of such polymers
- C08J2477/06—Polyamides derived from polyamines and polycarboxylic acids
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- C08K5/0041—Optical brightening agents, organic pigments
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Abstract
The invention discloses a high-glossiness glass fiber reinforced polyamide composite material and a preparation method thereof, wherein the high-glossiness glass fiber reinforced polyamide composite material comprises the following raw materials in parts by mass: 55-90 parts of polyamide, 5-40 parts of glass fiber, 3-6 parts of aniline black master batch, 0.2-1 part of coupling agent, 0.2-0.8 part of antioxidant and 1-2 parts of dispersing agent, wherein the aniline black master batch and the dispersing agent are sequentially mixed and added into a first side feeding port of a double-screw extruder, the polyamide, the coupling agent and the antioxidant are mixed and then added into a main feeding port, the glass fiber is added into a second side feeding port, and the polyamide, the coupling agent and the antioxidant are melted, blended, extruded, cooled and granulated to obtain the aniline black master batch. The functional aniline black master batch and the dispersing agent are added into the polyamide resin, so that the problem of fiber floating leakage on the surface of a polyamide product is solved, the polyamide product has a high-blackness brightness effect, and an injection molding part is smooth and attractive in appearance.
Description
Technical Field
The invention belongs to the technical field of modification of high polymer materials, and particularly relates to a high-glossiness glass fiber reinforced polyamide composite material and a preparation method thereof.
Background
At present, the strength of Glass Fiber (GF) reinforced Polyamide (PA) products is high, but the surface of the products has floating fibers or the floating fibers leak seriously, the PA materials have low gloss and are not beautiful enough, and black products, especially appearance parts, have grey phases and are not black enough, so that the application field of the glass fiber reinforced PA materials is limited, and the problems of serious appearance floating fibers and low gloss of the products are urgently needed to be solved when the strength of the materials is ensured.
Disclosure of Invention
In order to overcome the technical defects, the invention aims to provide the high-glossiness glass fiber reinforced polyamide composite material and the preparation method thereof.
The above object of the present invention is achieved by the following technical solutions:
the invention provides aniline black master batch which is prepared from 85-90 wt% of nylon 6(PA6), 9-13 wt% of oil-soluble aniline black and 1-2 wt% of dispersing agent through mixing, melt extrusion at the temperature of 280 ℃ by a double-screw extruder, cooling and granulating.
Preferably, the dispersant is selected from vinyl bis stearamide or PE wax.
Preferably, the raw materials are proportionally mixed in a high-speed mixer for 5-10min, and are added into a double-screw extruder to be blended, melted and extruded under the conditions that the screw rotating speed is 400-1200r/min and the processing temperature is 180-280 ℃.
The invention provides a high-glossiness glass fiber reinforced polyamide composite material which comprises the following raw materials in parts by mass: 55-90 parts of polyamide, 5-40 parts of glass fiber, 3-6 parts of aniline black master batch, 0.2-1 part of coupling agent, 0.2-0.8 part of antioxidant and 1-2 parts of dispersing agent.
Preferably, the coupling agent is selected from the group consisting of gamma-aminopropyltrimethoxysilane, gamma-aminopropyltriethoxysilane, gamma-glycidoxypropyltrimethoxysilane, gamma-glycidoxypropyltriethoxysilane, N- (beta-aminoethyl) -gamma-aminopropyltrimethoxysilane, N-beta- (aminoethyl) -gamma-aminopropylmethyldimethoxysilane, gamma-ureidopropyltriethoxysilane, N-aminoethyl-gamma-aminopropyltriethoxysilane, gamma-aminopropylmethyldiethoxysilane, N- (beta-aminoethyl) -gamma-aminopropyltriethoxysilane, polyaminoalkyltrialkoxysilanes, anilinomethyltrimethoxysilane, tris (dioctylphosphoryloxy) isopropyl titanate, gamma-glycidyloxy-N-propyltrimethoxysilane, gamma-glycidyloxy-N-propyltriethoxysilane, gamma-glycidyloxy-N-beta-aminopropyltriethoxysilane, poly (aminoalkyltrialkoxysilane, anilinomethyltrimethoxysilane, tris (dioctylphosphoryloxy) isopropyl titanate, gamma-glycidyloxy-N-propyltrimethoxysilane, gamma-glycidyloxy-N-propyltrimethoxysilane, Isopropyl triisostearate, isopropyldioleacyloxy (dioctylphosphatoxy) titanate, isopropyltris (dioctylphosphatoxy) titanate, isopropyltrioleyloxy titanate, isopropyltris (dioctylphosphatoxy) titanate, bis (dioctyloxypyrophosphate) ethylene titanate, a chelate of bis (dioctyloxypyrophosphate) ethylene titanate and triethanolamine, tetraisopropylbis (dioctylphosphatoxy) titanate, one or a combination of two or more of distearoyloxyisopropyl aluminate, isopropoxydistearoyloxyaluminate, trimethyl aluminate, triisopropyl aluminate, tribenzyl aluminate, alkoxytris (vinyl-ethoxy) zirconate, alkoxytris (p-aminophenoxy) zirconate, bis (diethyl citrate) dipropyloxyzirconium chelate or tetra (triethanolamine) zirconate.
Preferably, the antioxidant is selected from tris (2, 4-di-tert-butylphenyl) phosphite, pentaerythrityl tetrakis [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ], N' -bis- (3- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionyl) hexanediamine, bis (2, 4-di-tert-butylphenyl) pentaerythritol diphosphite, N-octadecyl beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate, tris (2, 4-di-tert-butyl) phosphite, octadecyl hindered phenol (3, 5-dibutyl-4-hydroxy-phenylpropionate), octadecyl 1,3, 5-tris (3, 5-di-tert-butyl, 4-hydroxybenzyl) s-triazine, 2,4,6- (1H,3H,5H) trione, N' -bis- (3- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionyl) hexanediamine, diethylene glycol bis [ beta- (3-tert-butyl-4-hydroxy-5-methylphenyl) propionate ] or pentaerythritol distearyl diphosphite.
Preferably, the dispersant is selected from the group consisting of vinyl bis stearamide, Glyceryl Monostearate (GMS) or glyceryl tristearate (HTG).
The invention also provides a preparation method of the glass fiber reinforced polyamide composite material, which comprises the following steps: the aniline black master batch and the dispersing agent are pre-dispersed and mixed according to the proportion, then the mixture is added into a first side feeding port of a double-screw extruder, the polyamide, the coupling agent and the antioxidant are mixed for 5-10min in a high-speed mixer according to the proportion, the mixture is added into a main feeding port of the double-screw extruder, and the glass fiber is added into a second side feeding port of the double-screw extruder; the raw materials are melted, blended and extruded at the processing temperature of 180-280 ℃, and then are cooled by a water tank, dried and cut into particles; wherein:
the main feeding rotating speed of the double-screw extruder is 400-1200r/min, and the side feeding rotating speed is 300-600 r/min;
the mass ratio of the main feeding port, the first side feeding port and the second side feeding port of the double-screw extruder is 7: 5-7: 1.
compared with the prior art, the invention has the beneficial effects that:
(1) according to the invention, the aniline black master batch is added into the glass fiber reinforced polyamide composite material, so that the product has good blackness and high-gloss black and bright effect, and the strength of the polyamide is ensured.
(2) According to the invention, on one hand, the raw material premixing and double-screw extrusion process is optimized, and on the other hand, the high polymer PA and the inorganic substance glass fiber are better combined together through the coupling agent, so that the matrix resin, the glass fiber and the black master batch are well compatible and dispersed, the color blackness and the glossiness are high, and the serious problem of fiber floating of the glass fiber reinforced polyamide composite material injection molding is effectively solved.
Detailed Description
The present invention is further illustrated by the following specific examples.
The starting materials used in the following examples are all conventional choices in the art as not illustrated.
The aniline black master batch consists of 85-90 wt% of nylon 6, 9-13 wt% of oil-soluble aniline black and 1-2 wt% of dispersing agent, and is obtained by mixing the raw materials in a high-speed mixer for 5-10min in proportion, adding the mixture into a double-screw extruder, and blending, melting and extruding the mixture under the conditions that the screw rotating speed is 400-1200r/min and the processing temperature is 180-280 ℃; wherein the dispersant is selected from vinyl bis stearamide or PE wax.
The coupling agent is selected from gamma-aminopropyltrimethoxysilane, gamma-aminopropyltriethoxysilane, gamma-glycidoxypropyltrimethoxysilane, gamma-glycidoxypropyltriethoxysilane, N- (beta-aminoethyl) -gamma-aminopropyltrimethoxysilane, N-beta- (aminoethyl) -gamma-aminopropylmethyldimethoxysilane, gamma-ureidopropyltriethoxysilane, N-aminoethyl-gamma-aminopropyltriethoxysilane, gamma-aminopropylmethyldiethoxysilane, N- (beta-aminoethyl) -gamma-aminopropyltriethoxysilane, polyaminoalkyltrialkoxysilanes, anilinomethyltrimethoxysilane, tri (dioctylphosphoryloxy) isopropyl titanate, isopropyl triisostearate, Isopropyldioleacyloxy (dioctylphosphatoxy) titanate, isopropyltris (dioctylphosphatoxy) titanate, isopropyltriolatoxy titanate, isopropyltris (dioctylphosphatoxy) titanate, bis (dioctyloxypyrophosphate) ethylene titanate, the chelate of bis (dioctyloxypyrophosphate) ethylene titanate and triethanolamine, tetraisopropylbis (dioctylphosphatoxy) titanate, distearoyloxyisopropyl aluminate, one or the combination of more than two of isopropoxy distearoyl acyloxy aluminate, trimethyl aluminate, triisopropyl aluminate, tribenzyl aluminate, alkoxy tri (vinyl-ethoxy) zirconate, alkoxy tri (p-aminophenoxy) zirconate, bis (diethyl citrate) dipropoxy zirconium chelate or tetra (triethanolamine) zirconate.
The antioxidant is selected from tris (2, 4-di-tert-butylphenyl) phosphite, pentaerythrityl tetrakis [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ], N' -bis- (3- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionyl) hexanediamine, bis (2, 4-di-tert-butylphenyl) pentaerythritol diphosphite, N-octadecyl beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate, tris (2, 4-di-tert-butyl) phosphite, octadecyl hindered phenol (3, 5-di-butyl-4-hydroxy-phenylpropionate), 1,3, 5-tris (3, 5-di-tert-butyl, 4-hydroxybenzyl) s-triazine, 2,4,6- (1H,3H,5H) trione, N' -bis- (3- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionyl) hexanediamine, diethylene glycol bis [ beta- (3-tert-butyl-4-hydroxy-5-methylphenyl) propionate ] or pentaerythritol distearyl diphosphite.
The dispersant is selected from vinyl bis stearamide, glyceryl monostearate or glyceryl tristearate.
Preparation method
Preparing aniline black color master batch: the nylon 6, the oil-soluble aniline black and the dispersing agent are proportionally mixed in a high-speed mixer for 5-10min, and then are added into a double-screw extruder to be blended, melted and extruded under the conditions that the screw rotating speed is 400-1200r/min and the processing temperature is 180-280 ℃.
Preparing a glass fiber reinforced polyamide composite material: pre-dispersing and mixing the aniline black master batch and the dispersing agent according to a ratio, adding the mixture into a first side feeding port of a double-screw extruder, proportionally mixing the polyamide, the coupling agent and the antioxidant in a high-speed mixer for 5-10min, adding the mixture into a main feeding port of the double-screw extruder, and adding the glass fiber into a second side feeding port of the double-screw extruder; the raw materials are melted, blended and extruded at the processing temperature of 180-280 ℃, and then are cooled by a water tank, dried and cut into particles; wherein the main feeding rotating speed of the double-screw extruder is 400-1200r/min, the side feeding rotating speed is 300-600r/min, and the mass ratio of the main feeding port to the first side feeding port to the second side feeding port is 7: 6: 1.
examples 1 to 3 and comparative examples 1 and 2 glass fiber reinforced polyamide composite materials were prepared according to the above-described preparation methods, and the weight compositions of the respective raw material components are shown in table 1.
Performance testing
(1) Color jetness is expressed as L value and measured according to KONICA MINOLTA Konica MINOLTA spectrocolorimeter CM-2500 c.
(2) The surface gloss measuring instrument measures according to the german BYK gloss meter.
(3) The condition of fiber floating on the surface is directly observed whether the glass fiber on the surface of the material product is exposed or not.
TABLE 1
The test results in table 1 show that the glass fiber reinforced polyamide composite material can effectively avoid the problems of serious fiber floating and low glossiness of the product while ensuring the strength of the material, and the aniline black master batch is added to enable the product to be molded once so as to achieve high blackness and high glossiness.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. It will be readily apparent to those skilled in the art that various modifications to these embodiments and the generic principles defined herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above-described embodiments. Those skilled in the art should appreciate that many modifications and variations are possible in light of the above teaching without departing from the scope of the invention.
Claims (8)
1. The aniline black master batch is characterized by comprising 85-90 wt% of nylon 6, 9-13 wt% of oil-soluble aniline black and 1-2 wt% of dispersing agent, and is obtained by mixing the raw materials, performing melt extrusion at the temperature of 180 ℃ and 280 ℃ through a double-screw extruder, cooling and granulating.
2. Nigrosine masterbatch according to claim 1, characterised in that the dispersant is selected from vinyl bis stearamide or PE wax.
3. The aniline black master batch according to claim 1, wherein the raw materials are proportionally mixed in a high-speed mixer for 5-10min, and are added into a double-screw extruder to be blended and melt extruded under the conditions of a screw rotating speed of 400-1200r/min and a processing temperature of 180-280 ℃.
4. The high-glossiness glass fiber reinforced polyamide composite material is characterized by comprising the following raw materials in parts by mass: 55-90 parts of polyamide, 5-40 parts of glass fiber, 3-6 parts of aniline black master batch according to any one of claims 1 to 3, 0.2-1 part of coupling agent, 0.2-0.8 part of antioxidant and 1-2 parts of dispersing agent.
5. The high gloss fiberglass reinforced polyamide composite material of claim 4, wherein said coupling agent is selected from the group consisting of gamma-aminopropyltrimethoxysilane, gamma-aminopropyltriethoxysilane, gamma-glycidoxypropyltrimethoxysilane, gamma-glycidoxypropyltriethoxysilane, N- (beta-aminoethyl) -gamma-aminopropyltrimethoxysilane, N-beta- (aminoethyl) -gamma-aminopropylmethyldimethoxysilane, gamma-ureidopropyltriethoxysilane, N-aminoethyl-gamma-aminopropyltriethoxysilane, gamma-aminopropylmethyldiethoxysilane, N- (beta-aminoethyl) -gamma-aminopropyltriethoxysilane, polyaminoalkyltrialkoxysilanes, polyaminotrialkoxysilanes, gamma-glycidoxypropyltrimethoxysilane, and mixtures thereof, Anilinomethyltrimethoxysilane, isopropyl tris (dioctylphosphoryloxy) titanate, isopropyl triisostearate, isopropyl dioleate acyloxy (dioctylphosphate) titanate, isopropyl tris (dioctylphosphate) titanate, isopropyl trioleate acyloxy titanate, isopropyl tris (dioctylphosphate) titanate, bis (dioctylphosphate) ethylene titanate, a chelate of bis (dioctylphosphate) ethylene titanate and triethanolamine, tetraisopropyl bis (dioctylphosphite acyloxy) titanate, distearoyloxyisopropylaluminate, isopropoxydistearoyloxyaluminate, trimethyl aluminate, triisopropyl aluminate, tribenzyl aluminate, alkoxytris (vinyl-ethoxy) zirconate, alkoxytris (p-aminophenoxy) zirconate, triisopropyl aluminate, and mixtures thereof, One or the combination of more than two of bis (diethyl citrate) dipropoxy zirconium chelate or tetra (triethanolamine) zirconate.
6. The high gloss glass fiber reinforced polyamide composite material according to claim 4, wherein the antioxidant is selected from the group consisting of tris (2, 4-di-t-butylphenyl) phosphite, pentaerythrityl tetrakis [ β - (3, 5-di-t-butyl-4-hydroxyphenyl) propionate ], hexanediamine N, N' -bis- (3- (3, 5-di-t-butyl-4-hydroxyphenyl) propionyl) hexanediamine, bis (2, 4-di-t-butylphenyl) pentaerythritol diphosphite, N-octadecyl β - (3, 5-di-t-butyl-4-hydroxyphenyl) propionate, tris (2, 4-di-t-butyl) phosphite, octadecyl hindered phenol (3, 5-dibutyl-4-hydroxy-phenyl propionate), octadecyl phosphite, 1,3, 5-tris (3, 5-di-tert-butyl, 4-hydroxybenzyl) s-triazine, 2,4,6- (1H,3H,5H) trione, N' -bis- (3- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionyl) hexanediamine, diethyleneglycol bis [ beta- (3-tert-butyl-4-hydroxy-5-methylphenyl) propionate ] or pentaerythritol distearyl diphosphite.
7. The high gloss glass fiber reinforced polyamide composite material according to claim 4, wherein the dispersant is selected from the group consisting of vinyl bis stearamide, glyceryl monostearate or glyceryl tristearate.
8. A process for the preparation of a glass fiber reinforced polyamide composite material according to any one of claims 4 to 7, comprising: the aniline black master batch and the dispersing agent are pre-dispersed and mixed according to the proportion, then the mixture is added into a first side feeding port of a double-screw extruder, the polyamide, the coupling agent and the antioxidant are mixed for 5-10min in a high-speed mixer according to the proportion, the mixture is added into a main feeding port of the double-screw extruder, and the glass fiber is added into a second side feeding port of the double-screw extruder; the raw materials are melted, blended and extruded at the processing temperature of 180-280 ℃, and then are cooled by a water tank, dried and cut into particles; wherein:
the main feeding rotating speed of the double-screw extruder is 400-1200r/min, and the side feeding rotating speed is 300-600 r/min;
the mass ratio of the main feeding port, the first side feeding port and the second side feeding port of the double-screw extruder is 7: 5-7: 1.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114163799A (en) * | 2021-12-20 | 2022-03-11 | 上海中镭新材料科技有限公司 | Polycarbonate material and preparation method and application thereof |
| CN115785655A (en) * | 2022-12-16 | 2023-03-14 | 上海中镭新材料科技有限公司 | Extra-black weather-resistant polyamide material and preparation method and application thereof |
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| CN102786793A (en) * | 2012-07-25 | 2012-11-21 | 金发科技股份有限公司 | Modified nylon material and its preparation method |
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Application publication date: 20210518 |