CN112538260B - Glass fiber reinforced polypropylene/polyamide composite material and preparation method thereof - Google Patents
Glass fiber reinforced polypropylene/polyamide composite material and preparation method thereof Download PDFInfo
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- 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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/25—Component parts, details or accessories; Auxiliary operations
- B29C48/285—Feeding the extrusion material to the extruder
- B29C48/288—Feeding the extrusion material to the extruder in solid form, e.g. powder or granules
- B29C48/2886—Feeding the extrusion material to the extruder in solid form, e.g. powder or granules of fibrous, filamentary or filling materials, e.g. thin fibrous reinforcements or fillers
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/25—Component parts, details or accessories; Auxiliary operations
- B29C48/285—Feeding the extrusion material to the extruder
- B29C48/297—Feeding the extrusion material to the extruder at several locations, e.g. using several hoppers or using a separate additive feeding
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C2948/00—Indexing scheme relating to extrusion moulding
- B29C2948/92—Measuring, controlling or regulating
- B29C2948/92504—Controlled parameter
- B29C2948/92609—Dimensions
- B29C2948/92619—Diameter or circumference
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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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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2423/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2423/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
- C08J2423/10—Homopolymers or copolymers of propene
- C08J2423/14—Copolymers of propene
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2451/00—Characterised by the use of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives of such polymers
- C08J2451/06—Characterised by the use of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives of such polymers grafted on to homopolymers or copolymers of aliphatic hydrocarbons containing only one carbon-to-carbon double bond
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- C08J2463/00—Characterised by the use of epoxy resins; Derivatives of epoxy resins
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/16—Nitrogen-containing compounds
- C08K5/34—Heterocyclic compounds having nitrogen in the ring
- C08K5/35—Heterocyclic compounds having nitrogen in the ring having also oxygen in the ring
- C08K5/353—Five-membered rings
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Abstract
The invention discloses a glass fiber reinforced polypropylene/polyamide composite material and a preparation method thereof, belonging to the field of polypropylene/polyamide composite materials. The glass fiber reinforced polypropylene/polyamide composite material comprises the following components in parts by weight: 20-25 parts of polypropylene, 65-70 parts of polyamide, 30-35 parts of short glass fiber, 10-20 parts of compatilizer, 0.2-0.4 part of curing agent and 0.2-0.4 part of antioxidant; the compatilizer comprises PP-g-MAH, epoxy resin and oxazoline; the curing agent is one or two of diethyl tetramethyl imidazole and epoxy-imidazole compound. According to the invention, PP-g-MAH, epoxy resin and oxazoline are used as compatilizers, and imidazole compounds containing tertiary amine are used as curing agents, so that the weld mark strength of the composite material can be obviously improved by optimizing the dosage of each raw material, and can reach up to 122MPa.
Description
Technical Field
The invention relates to the field of polypropylene/polyamide composite materials, in particular to a glass fiber reinforced polypropylene/polyamide composite material and a preparation method thereof.
Background
Polyamide (PA) is a general plastic with the largest use amount, is widely used in industries such as industry and automobile, contains a large number of amide groups in a macromolecular structure, can form hydrogen bonds among molecules, has reactivity under certain conditions, is a polymer with strong polarity and crystallinity, but has high molding shrinkage rate, poor dimensional stability and easy moisture absorption.
The polypropylene (PP) and the fiber are added and blended, so that excellent processing performance and comprehensive performance can be obtained, the resin water absorption can be reduced by the glass fiber reinforcement, and the polyamide has very good affinity with the glass fiber. However, the weld line strength is reduced due to poor compatibility of the alloy, so in order to further expand the application of the PP/PA plastic alloy and reduce the cost, the weld mark strength of the PP/PA plastic alloy material is urgently required to be improved.
CN201610600601.5 discloses a polyamide-polypropylene blend and its preparation method, wherein the composition is prepared by blending 25-30 parts of polyamide, 5-10 parts of polypropylene, 2-3 parts of compatibilizer, 3-4 parts of toughening agent, and 5-7 parts of talc powder, the compatibilizer adopts monostearyl alcohol glyceryl ether and glyceryl monostearate, but the mechanism thereof is not explained.
CN201811168956.7 discloses a permeation resistant air conditioning hose. The inner liner layer is a modified polyamide nylon alloy obtained by blending polyamide and carboxyl-containing modified polyolefin, and the air hose has high permeability resistance.
Chinese patent application CN201910570451.1 discloses a modified nylon material, wherein 40-60 parts of nylon-6; 4-5 parts of a filler; the toughening agent and the compatilizer comprise 7-10 parts of styrene butadiene rubber and 3-4 parts of bisphenol A epoxy resin. Chinese patent application CN201210270214 discloses a super-tough polyamide alloy and a preparation method and application thereof, wherein the components comprise 2-81.5% of polyamide, 2-81.5% of polyester, 0.5-5% of compatilizer and 10-35% of toughening agent, and the compatilizer is polymer ionomer, polyamide-polyester block copolymer, phenyl sulfonate, epoxy resin, maleic anhydride graft copolymer or rubber phase-containing elastomer. Both of the above patent applications utilize epoxy resin as a compatibilizer for polyamide, but from the viewpoint of stretching effect, a higher compatibilizing system for improving weld mark strength of glass fiber reinforced resin is not obtained.
Disclosure of Invention
In order to overcome the above disadvantages, the present invention aims to provide a glass fiber reinforced polypropylene/polyamide composite material having high weld mark strength.
The invention also aims to provide a preparation method of the glass fiber reinforced polypropylene/polyamide composite material.
The purpose of the invention is realized by the following technical scheme.
The glass fiber reinforced polypropylene/polyamide composite material comprises the following components in parts by weight:
the compatilizer comprises PP-g-MAH, epoxy resin and oxazoline;
the curing agent is one or two of diethyl tetramethyl imidazole and epoxy-imidazole compound.
Preferably, the glass fiber reinforced polypropylene/polyamide composite material comprises the following components in parts by weight:
the compatilizer comprises 10 parts of PP-g-MAH, 1.5-2.3 parts of epoxy resin and 5 parts of oxazoline.
Preferably, the glass fiber reinforced polypropylene/polyamide composite material comprises the following components in parts by weight:
the compatilizer comprises 10 parts of PP-g-MAH, 1.8-2 parts of epoxy resin and 5 parts of oxazoline.
Preferably, the glass fiber reinforced polypropylene/polyamide composite material comprises the following components in parts by weight:
the compatilizer comprises 10 parts of PP-g-MAH (maleic anhydride grafted polypropylene), 2 parts of epoxy resin and 5 parts of oxazoline.
Preferably, the polypropylene is homo-polypropylene or co-polypropylene, the melt flow rate is 10-40 g/10min, the melt flow rate is 2.16kg/230 ℃, and the test method is GB/T3682.1-2018.
Preferably, the polyamide has a melting point of 210 ℃ or higher and an intrinsic viscosity index of 2.4.
Preferably, the epoxy resin is one or more of glycidyl ether epoxy resin, glycidyl ester epoxy resin, glycidyl amine epoxy resin, linear aliphatic epoxy resin, alicyclic epoxy resin, and bisphenol epoxy resin.
Preferably, the antioxidant is pentaerythritol tetrakis [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ].
Preferably, in order to improve the processing adjustment of the composite material, additives such as lubricants and the like can be added, and some ultraviolet resistant agents, high-temperature stabilizers and the like can be added for improving other weather resistance.
The preparation method of the glass fiber reinforced polypropylene/polyamide composite material comprises the following steps:
feeding polypropylene, polyamide, a compatilizer, a curing agent and an antioxidant from a main feeding port according to a ratio, feeding glass fiber from a side feeding port, extruding and granulating by a double-screw extruder to obtain the glass fiber reinforced polypropylene/polyamide composite material, wherein the extrusion temperature is set to 180-230 ℃, the rotation speed of a host screw is 300-600rpm, and the length-diameter ratio of the screw is 56.
The invention adopts a 56.
The compatilizer adopted in the invention is PP-g-MAH, epoxy resin (EP) and oxazoline. PP-g-MAH is matched with epoxy resin and a curing agent, and aims to modify short glass fibers, improve the compatibility of the short glass fibers in polypropylene, improve the mechanical property of a material, form higher polar group density at a weld mark, and greatly improve the intermolecular acting force at the weld mark, so that the strength of the weld mark is improved. Oxazoline can react with polymers containing amino or carboxyl, can improve the bonding tightness of polyamide/polypropylene matrix materials, can react with acid anhydride, epoxy resin and the like, can promote the dispersion of alloy components, can be tightly bonded with the matrix materials, and has good compatibilization effect.
Due to the low grafting rate of the non-polarity of the polypropylene and the PP-g-MAH, the improvement of the mechanical property is limited. The invention adopts PP-g-MAH, and epoxy resin and curing agent are matched. The epoxy group can react with the hydroxyl of the coupling agent on the surface of the fiber and the PPg-MAH anhydride group respectively, so that the compatibilization effect of the PP-g-MAH is improved.
The imidazole tertiary amine in the curing agent of the invention causes the ring opening of the epoxy group, plays a role in accelerating the reaction of EP and acid anhydride, and causes the epoxy resin to generate partial gel or curing, thus reducing the plasticizing effect.
The added epoxy resin contains epoxy functional groups with higher reactivity, can react with terminal amino groups of polyamide, and is favorable for improving the crosslinking compactness of the polyamide and the polypropylene plastic alloy. And the PP-g-MAH is matched with tertiary amine of imidazole in curing agents such as diethyl tetramethyl imidazole and the like to open the ring of an epoxy group, so that the reaction of epoxy resin and anhydride can be promoted, and the effects of modifying glass fiber and increasing PP volume are achieved.
Compared with the prior art, the invention has the following beneficial effects:
1. according to the invention, the PP-g-MAH, the epoxy resin and the curing agent are added into the glass fiber reinforced polypropylene/polyamide composite material to modify the chopped glass fiber, so that the compatibilization effect of the glass fiber in polypropylene is improved, the distribution of the glass fiber in the composite material is improved, and the intermolecular interaction force at a weld mark is improved, thereby improving the weld mark strength of the glass fiber reinforced plastic alloy.
2. The base material disclosed by the invention is matched with oxazoline for use, so that the dispersibility of the polypropylene/polyamide alloy can be improved, the tight combination of the base material is promoted, the weld mark strength of the polypropylene/polyamide composite material is improved, meanwhile, due to the lower addition amount, the influence on the mechanical strength can be reduced, and the effect of obviously improving the weld mark strength of the composite material is achieved.
3. According to the invention, the polypropylene/polyamide composite material with weld mark strength as high as 122MPa is prepared by optimizing the dosage of the compatilizer PP-g-MAH, the epoxy resin, the oxazoline and the curing agent.
4. The invention adopts a 56.
Detailed Description
Specific embodiments of the present invention will be further described below with reference to examples, but the embodiments of the present invention are not limited thereto.
The examples of the invention and the comparative examples used the following raw materials:
polypropylene: the melt flow rate of the copolymerized polypropylene is 10-40 g/10min,2.16kg/230 DEG C
Polyamide: the melting point is above 210 deg.C, and the intrinsic viscosity index is 2.4
A compatibilizer A; an epoxy resin;
a compatilizer B: PP-g-MAH;
a compatilizer C: oxazolines
Curing agent: diethyl tetramethyl imidazole 2E4MZ
Antioxidant: tetrakis [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propanoic acid ] pentaerythritol ester
The preparation methods of the glass fiber reinforced polyamide composite materials of the examples and the comparative examples are as follows: weighing raw materials according to a mass ratio, feeding auxiliary agents such as polyamide resin, polypropylene, a compatilizer, a curing agent, an antioxidant and the like from a main feeding port of a double-screw extruder, adding short glass fiber from a side feeding port, performing melt blending extrusion in the double-screw extruder, cooling, air drying and granulating to obtain the glass fiber reinforced polyamide/polypropylene alloy composite material with high weld mark strength, wherein the extrusion temperature is set to be 180-230 ℃, the rotating speed of a host screw is 300-600rpm, and the length-diameter ratio of the screw is 56.
The performance test method comprises the following steps:
(1) Strength of the weld mark: according to the test method of the national standard GB/T1040.2-2008, the test sample strip is poured into the two ends
(2) Tensile strength: testing according to the method of national standard GB/T1040.2-200.
(3) Bending strength: testing according to the method of the national standard GB/T9341-2008.
TABLE 1
TABLE 2
As is clear from examples 1 to 7, the weld mark strength is rather lowered by too high an amount of the epoxy resin, and it is understood from comparative example 1/2 that it is necessary to control the amount of the epoxy compound to be in the range of 1 to 3 parts and more effective at preferably 1.8 to 2 parts.
Within the range of the amount of the present invention, the weld mark strength of the examples was higher than that of comparative example 3, which indicates that the weld mark strength was greatly improved compared to the original tensile strength of the resin matrix. As is clear from example 5 and comparative example 6, it is preferable that the curing agent is not added to the components, and the component-compatible effect is not good, probably because the epoxy resin will not act on the maleic anhydride without ring-opening. Combining example 5 with comparative example 7, it can be seen that the addition of oxazoline can greatly improve the weld mark strength of the alloy, probably because the dispersibility of the components is improved, so that the polypropylene/polyamide components are tightly combined.
From example 5 and comparative example 4/5, it can be seen that when the epoxy resin is 2 parts, the PP-g-MAH and the curing agent have the best compatibilization effect between 10 parts and 0.2 part, which is beneficial to improving the weld mark strength of the material.
Claims (9)
1. The glass fiber reinforced polypropylene/polyamide composite material is characterized by comprising the following components in parts by weight:
20-25 parts of polypropylene
65-70 parts of polyamide
30-35 parts of short glass fiber
10 portions of PP-g-MAH
1.5-2.3 parts of epoxy resin
Oxazoline 5 parts
0.2 to 0.4 portion of curing agent
0.2-0.4 part of antioxidant;
the PP-g-MAH, the epoxy resin and the oxazoline are compatilizers;
the curing agent is one or two of diethyl tetramethyl imidazole and epoxy-imidazole compound.
2. The glass fiber reinforced polypropylene/polyamide composite material according to claim 1, comprising the following components in parts by weight:
20-25 parts of polypropylene
65-70 parts of polyamide
30-35 parts of short glass fiber
10 portions of PP-g-MAH
1.8-2 parts of epoxy resin
Oxazoline 5 parts
0.2 to 0.4 portion of curing agent
0.2-0.4 part of antioxidant;
the PP-g-MAH, the epoxy resin and the oxazoline are compatilizers.
3. The glass fiber reinforced polypropylene/polyamide composite material according to claim 2, comprising the following components in parts by weight:
20 portions of polypropylene
Polyamide 70 parts
Short glass fiber 30 parts
10 portions of PP-g-MAH
Epoxy resin 2 parts
Oxazoline 5 parts
0.2 part of curing agent
0.2 part of antioxidant;
the PP-g-MAH, the epoxy resin and the oxazoline are compatilizers.
4. The glass fiber reinforced polypropylene/polyamide composite material as claimed in any one of claims 1 to 3, wherein the polypropylene is homo-polypropylene or co-polypropylene, and the melt flow rate is 10-40 g/10min,2.16kg/230 ℃.
5. A glass fiber reinforced polypropylene/polyamide composite material according to any one of claims 1 to 3, wherein the polyamide is a polyamide having a melting point of 210 ℃ or higher and an intrinsic viscosity index of 2.4.
6. The glass fiber reinforced polypropylene/polyamide composite material according to any one of claims 1 to 3, wherein the epoxy resin is one or more of glycidyl ether type epoxy resin, glycidyl ester type epoxy resin, glycidyl amine type epoxy resin, linear aliphatic epoxy resin, alicyclic epoxy resin and bisphenol type epoxy resin.
7. The glass fiber reinforced polypropylene/polyamide composite material according to any one of claims 1 to 3, wherein the antioxidant is pentaerythritol tetrakis [ β - (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ].
8. The glass fiber reinforced polypropylene/polyamide composite material according to any one of claims 1 to 3, further comprising one or more of a lubricant, an anti-UV agent and a high temperature stabilizer.
9. A method for preparing a glass fiber reinforced polypropylene/polyamide composite material as claimed in any one of claims 1 to 3, comprising the steps of:
feeding polypropylene, polyamide, a compatilizer, a curing agent and an antioxidant from a main feeding port according to a ratio, feeding glass fiber from a side feeding port, extruding and granulating by using a double-screw extruder to obtain the glass fiber reinforced polypropylene/polyamide composite material, wherein the extrusion temperature is set to 180-230 ℃, the rotation speed of a main machine screw is 300-600rpm, and the length-diameter ratio of the screw is 56.
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| CN114573959B (en) * | 2022-03-22 | 2023-10-10 | 上海金发科技发展有限公司 | PET composition and application thereof |
| CN115612204B (en) * | 2022-09-27 | 2023-09-26 | 天津金发新材料有限公司 | Masterbatch for improving strength retention rate of polypropylene weld marks, and preparation method and application thereof |
| CN115536942B (en) * | 2022-10-25 | 2023-06-02 | 苏州旭光聚合物有限公司 | Plant fiber reinforced polypropylene composite material and preparation method thereof |
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| CN103194023B (en) * | 2013-03-19 | 2015-12-23 | 深圳市亚塑科技有限公司 | A kind of fiberglass reinforced PP/PA6 matrix material and preparation method thereof and application |
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