CN110698756A - High weld mark strength glass fiber reinforced polypropylene composite material and preparation method thereof - Google Patents
High weld mark strength glass fiber reinforced polypropylene composite material and preparation method thereof Download PDFInfo
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- CN110698756A CN110698756A CN201910934466.1A CN201910934466A CN110698756A CN 110698756 A CN110698756 A CN 110698756A CN 201910934466 A CN201910934466 A CN 201910934466A CN 110698756 A CN110698756 A CN 110698756A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- 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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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2323/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2323/02—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
- C08J2323/10—Homopolymers or copolymers of propene
- C08J2323/12—Polypropene
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- 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
- C08J2423/26—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers modified by chemical after-treatment
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- 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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- C—CHEMISTRY; METALLURGY
- 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
- C08K7/00—Use of ingredients characterised by shape
- C08K7/02—Fibres or whiskers
- C08K7/04—Fibres or whiskers inorganic
- C08K7/14—Glass
Abstract
The glass fiber reinforced polypropylene composite material with high weld mark strength comprises the following components in parts by weight: 100 parts of polypropylene; 0.1-2 parts of sulfonated polyolefin wax; 1-10 parts of maleic anhydride grafted polypropylene; 1-50 parts of glass fiber. According to the invention, the sulfonated polyolefin wax and the maleic anhydride grafted polypropylene are added into the glass fiber reinforced polypropylene in a compounding manner, and the sulfonated polyolefin wax is enriched at the flowing front end during injection molding, so that a higher strong polar group density is formed at a weld mark, the intermolecular interaction force at the weld mark is greatly improved, and the weld mark strength of the glass fiber reinforced polypropylene is improved.
Description
Technical Field
The invention relates to the technical field of high polymer materials, in particular to a glass fiber reinforced polypropylene composite material with high weld mark strength and a preparation method thereof.
Background
After the polypropylene is reinforced by the glass fiber, the strength, rigidity, impact strength and thermal deformation temperature of the polypropylene can be greatly improved, so that the polypropylene can be widely applied to industries such as automobiles, building materials, household appliances and the like. However, during application, weld mark locations of injection molded articles of reinforced polypropylene are often found to be the initiation points of failure of the articles. This is because the addition of glass fiber can greatly improve the strength of the material, but it is difficult to improve the weld mark strength. In general, the strength of the glass fiber reinforced weld mark is not higher than that of the matrix resin, which is mainly caused by poor compatibility between the glass fiber and the resin matrix, and even if the glass fiber is modified to improve the compatibility between the glass fiber and the resin matrix, the improvement on the strength of the weld line is insufficient; furthermore, the weld mark strength is difficult to be improved by merely adding maleic anhydride grafted polypropylene to increase the compatibility. The glass fiber reinforced polypropylene material with high weld mark strength can be used for preparing lighter and lower-cost parts, so that the weld mark strength of the glass fiber reinforced polypropylene material is urgently required to be improved in order to further expand the application of the glass fiber reinforced polypropylene material and reduce the cost.
CN200810218925.8 discloses a high weld mark strength reinforced polypropylene material and a preparation method thereof, in the patent, the weld mark strength is improved by reducing the orientation of glass fibers to improve the bridging level of the glass fibers to an interface.
Chinese patent application CN109535620A discloses an impact-resistant pedal plate material for a sanitation garbage can, which comprises 10-20 parts of a polypropylene/calcined kaolin compound, 25-35 parts of an acetic acid-ethylene-acetic acid copolymer, 20-30 parts of chlorosulfonated polyethylene, 10-20 parts of polycarbonate, 2-4 parts of a cross-linking agent, 8-16 parts of a maleic anhydride grafted ethylene-acrylic acid copolymer, 4-8 parts of medical stone, 2-4 parts of glass fiber, 2-3.5 parts of fly ash, 8-10 parts of nano titanium dioxide and 1-2 parts of acetyl tributyl citrate. Chinese patent application CN109337248A discloses a thermal aging resistant polyvinyl chloride resin, comprising the following components: polyvinyl chloride resin, chlorosulfonated polyethylene, polypropylene resin, maleic anhydride grafted compatilizer, heat-resistant modified filler, aluminum alloy micro powder and the like. Both of the above two patent applications use chlorosulfonated polyethylene, which has the functions of toughening and improving impact strength, is a high molecular substance, and has a much higher molecular weight than sulfonated polyolefin wax, and although chlorosulfonated polyethylene has a polar group and can also have the function of improving polarity in a composite material, the improvement of polarity is very limited because of its higher molecular weight. Therefore, the improvement of weld mark strength by chlorosulfonated polyethylene is very limited, and only toughness and impact strength can be improved.
Disclosure of Invention
The invention aims to provide a glass fiber reinforced polypropylene composite material which has high weld mark strength.
The invention also aims to provide a preparation method of the glass fiber reinforced polypropylene composite material with high weld mark strength.
The invention is realized by the following technical scheme:
the glass fiber reinforced polypropylene composite material with high weld mark strength comprises the following components in parts by weight:
100 parts of polypropylene;
0.1-2 parts of sulfonated polyolefin wax;
1-10 parts of maleic anhydride grafted polypropylene;
1-50 parts of glass fiber;
the grafting ratio of the maleic anhydride grafted polypropylene ranged from 0.7 ~ 2%.
Preferably, the composition comprises the following components in parts by weight:
100 parts of polypropylene;
0.2-1 part of sulfonated polyolefin wax;
2.5-6 parts of maleic anhydride grafted polypropylene;
1-50 parts of glass fiber;
the grafting ratio of the maleic anhydride grafted polypropylene ranged from 0.7 ~ 2%.
Preferably, the polypropylene resin has a melt flow rate of 10 ~ 40g/10min, 2.16kg/230 ℃ and a test method of GB/T3682.1-2018.
The polypropylene resin may be homo-polypropylene or co-polypropylene.
Generally, the melt flow rate of a polypropylene resin reflects its molecular weight size and uniformity of molecular weight distribution, which is reflected by the microstructure within the polypropylene resin.
In the invention, the purpose of adding a certain amount of maleic anhydride for grafting is to improve the compatibility of the glass fiber and the PP resin; the purpose of adding a certain amount of sulfonated polyolefin wax is to improve intermolecular acting force at the weld mark, and under the mutual synergistic effect of the two effects, the sulfonated polyolefin wax is enriched at the flowing front end during injection molding, so that higher strong polar group density is formed at the weld mark, the intermolecular acting force at the weld mark is greatly improved, and the weld mark strength of the glass fiber reinforced polypropylene is improved.
The sulfonated polyolefin wax is selected from at least one or a combination of more of sulfonated polyethylene wax, sulfonated polypropylene wax and sulfonated polybutylene wax.
Preferably, the sulfonated polyolefin wax has a sulfonation degree of 0.5 ~ 0.8.8 mmol/g and a number average molecular weight of 1000 ~ 10000, wherein the sulfonation degree has a great influence on the weld mark strength, and the weld mark strength is reduced by over-high or under-low.
According to the invention, the grafting rate range of the maleic anhydride grafted polypropylene is 0.7 ~ 2%, the melt flow rate is 50 ~ 200g/10min, 2.13kg/230 ℃, and the test method is GB/T3682.1-2018. generally, the grafting rate range of the common maleic anhydride grafted polypropylene is 0.3-3.5%, and the grafting rate is over 5% and even up to 10% by customization, however, experiments show that the improvement of the weld line strength of the glass fiber reinforced polypropylene material is only obvious if the grafting rate is in a small range of 0.7-2%.
0-3 parts of antioxidant is also included according to the parts by weight.
Antioxidants include primary antioxidants or stabilizers (e.g., hindered phenols and/or secondary arylamines). Suitable antioxidants include alkylated monophenols or polyphenols; alkylation reaction products of polyhydric phenols with dienes such as tetrakis [ methylene (3, 5-di-tert-butyl-4-hydroxyhydrocinnamate) ] methane and the like; butylated reaction products of p-cresol or dicyclopentadiene; alkylated hydroquinones; hydroxylated thiodiphenyl ether; alkylidene bisphenols; a benzyl compound; esters of beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) -propionic acid with mono-or polyhydric alcohols; esters of beta- (5-tert-butyl-4-hydroxy-3-methylphenyl) -propionic acid with mono-or polyhydric alcohols; esters of thioalkyl or thioaryl compounds such as distearylthiopropionate, dilaurylthiopropionate, ditridecylthiopropionate, octadecyl-3- (3, 5-di-t-butyl-4-hydroxyphenyl) propionate, pentaerythritol-tetrakis [3- (3, 5-di-t-butyl-4-hydroxyphenyl) ] propionate and the like; amides of beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) -propionic acid and the like; or combinations comprising at least one of the foregoing antioxidants.
Of course, auxiliary agents such as lubricants and the like can be added for improving the processing adjustment of the composite material, and some ultraviolet resistant agents, high-temperature stabilizers and the like can be added for improving other weather resistance.
The preparation method of the high-weld mark strength glass fiber reinforced polypropylene composite material comprises the following steps of feeding polypropylene, maleic anhydride grafted polypropylene, sulfonated polyolefin wax and an antioxidant from a main feeding port and feeding glass fiber from a side feeding port according to a ratio, extruding and granulating by a double-screw extruder to obtain the high-weld mark strength glass fiber reinforced polypropylene composite material, wherein the extrusion temperature is set to be 180 ~ 230 ℃, the rotating speed of a main machine screw is 300 ~ 600rpm, and the length-diameter ratio of the screw is 40: 1.
The invention has the following beneficial effects:
according to the invention, two key components, namely maleic anhydride grafted polypropylene and sulfonated polyolefin wax, are added into the glass fiber reinforced polypropylene, so that the weld mark strength of the material can be improved under the synergistic effect. The sulfonation value of the sulfonated polyolefin wax is optimized, the grafting rate of the maleic anhydride grafted polypropylene is optimized, and the weld mark strength is greatly improved.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following claims and specific examples. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The examples of the invention and the comparative examples used the following raw materials:
polypropylene: the metallocene petrochemical N-Z30S has MFR of 25g/10 min;
sulfonated polyolefin wax a: the sulfonation degree is 0.6mmol/g, and the number average molecular weight is about 6000;
sulfonated polyolefin wax B: the sulfonation degree is 0.3mmol/g, and the number average molecular weight is about 5600;
sulfonated polyolefin wax C: the degree of sulfonation was 1.0mmol/g, and the number average molecular weight was about 5800.
Maleic anhydride-grafted polypropylene a: the grafting rate is 1.8 percent, and the melt flow rate is 80g/10 min;
maleic anhydride grafted polypropylene B: the grafting rate is 0.8 percent, and the melt flow rate is 89g/10 min;
maleic anhydride-grafted polypropylene C: the grafting rate is 0.3 percent, and the melt flow rate is 102g/10 min;
maleic anhydride-grafted polypropylene D: the grafting rate is 3.5 percent, and the melt flow rate is 72g/10 min;
maleic anhydride grafted polyethylene: the grafting rate was 1.3%, and the melt flow rate was 98g/10 min.
Glass fiber: CPIC ECS 305K;
antioxidant: hindered phenol antioxidants.
The preparation method of the glass fiber reinforced polypropylene composite material comprises the steps of feeding polypropylene, maleic anhydride grafted polypropylene (or maleic anhydride grafted polyethylene), sulfonated polyolefin wax and an antioxidant from a main feeding port and feeding glass fiber from a side feeding port according to the proportion, extruding and granulating by a double-screw extruder to obtain the glass fiber reinforced polypropylene composite material with high weld mark strength, wherein the extrusion temperature is set to be 180 ~ 230 ℃, the rotation speed of a main machine screw is 450rpm, and the length-diameter ratio of the screw is 40: 1.
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: examples 1-7 component ratios and Performance test results of glass fiber reinforced Polypropylene composite materials
| Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | Example 6 | |
| Polypropylene | 100 | 100 | 100 | 100 | 100 | 100 |
| Sulfonated polyolefin wax A | 0.8 | 0.1 | 0.2 | 2 | ||
| Sulfonated polyolefin wax B | 0.8 | |||||
| Sulfonated polyolefin wax C | 0.8 | |||||
| Maleic anhydride grafted Polypropylene A | 5 | 5 | 5 | 5 | 5 | 5 |
| Glass fiber | 30 | 30 | 30 | 30 | 30 | 30 |
| Antioxidant agent | 0.2 | 0.2 | 0.2 | 0.2 | 0.2 | 0.2 |
| Weld mark strength Mpa | 36 | 32 | 31 | 30 | 35 | 31 |
| Tensile strength, Mpa | 92 | 89 | 88 | 93 | 91 | 81 |
| Flexural strength, Mpa | 130 | 123 | 119 | 134 | 128 | 117 |
As can be seen from example 1/2/3, the preferred sulfonated polyolefin waxes have a degree of sulfonation in the range of preferably 0.5 ~ 0.8.8 mmol/g.
As can be seen from example 1/4/5/6, the use of sulfonated polyolefin wax in the preferred range gives a high weld mark strength, and is slightly too high or too low.
Table 2: examples 8-12 proportions of Components of glass fiber reinforced Polypropylene composite Material and results of Performance test
| Example 7 | Example 8 | Example 9 | Example 10 | Example 11 | |
| Polypropylene | 100 | 100 | 100 | 100 | 100 |
| Sulfonated polyolefin wax A | 0.8 | 0.8 | 0.1 | 2 | 0.8 |
| Maleic anhydride grafted Polypropylene A | 2 | 8 | 10 | 1 | |
| Maleic anhydride grafted Polypropylene B | 5 | ||||
| Glass fiber | 30 | 30 | 30 | 30 | 30 |
| Antioxidant agent | 0.2 | 0.2 | 0.2 | 0.2 | 0.2 |
| Weld mark strength Mpa | 32 | 30 | 31 | 32 | 36 |
| Tensile strength, Mpa | 80 | 85 | 83 | 73 | 92 |
| Flexural strength, Mpa | 112 | 122 | 117 | 101 | 129 |
As can be seen from example 1/7/8/9, the preferred range of the amount of maleic anhydride-grafted polypropylene is such that the weld mark strength is improved to a high level, and when the amount exceeds 8 parts to 10 parts, the tensile strength and flexural strength are reduced although the weld mark strength is slightly increased.
Table 3: the components of the glass fiber reinforced polypropylene composite material of the comparative example are proportioned and the performance test results
| Comparative example 1 | Comparative example 2 | Comparative example 3 | Comparative example 4 | Comparative example 5 | Comparative example 6 | |
| Polypropylene A | 100 | 100 | 100 | 100 | 100 | 100 |
| Sulfonated polyolefin wax A | 0.8 | 0.8 | 0.8 | 0.8 | 3 | |
| Maleic anhydride grafted Polypropylene A | 5 | 5 | ||||
| Maleic anhydride grafted Polypropylene C | 5 | |||||
| Maleic anhydride grafted Polypropylene D | 5 | |||||
| Maleic anhydride grafted polyethylene | 5 | |||||
| Glass fiber | 30 | 30 | 30 | 30 | 30 | 30 |
| Antioxidant agent | 0.2 | 0.2 | 0.2 | 0.2 | 0.2 | 0.2 |
| Weld mark strength Mpa | 27 | 28 | 28 | 27 | 25 | 23 |
| Tensile strength, Mpa | 64 | 76 | 75 | 74 | 71 | 68 |
| Flexural strength, Mpa | 88 | 103 | 107 | 101 | 96 | 97 |
From comparative examples 1 and 5, it can be seen that only maleic anhydride grafted polypropylene is required to obtain high tensile strength and flexural strength; however, in order to achieve high weld line strength, high tensile strength and high flexural strength at the same time, it is necessary to add suitable sulfonated polyolefin waxes.
From comparative example 2/3/4/5, it is clear that the graft ratio of maleic anhydride-grafted polypropylene must be within the range of the present invention, and maleic anhydride-grafted polyethylene has no corresponding effect.
As is clear from the comparative examples, the excessive amount of the sulfonated polyolefin wax rather greatly reduced the weld mark strength and other strengths.
Claims (8)
1. The glass fiber reinforced polypropylene composite material with high weld mark strength is characterized by comprising the following components in parts by weight:
100 parts of polypropylene;
0.1-2 parts of sulfonated polyolefin wax;
1-10 parts of maleic anhydride grafted polypropylene;
1-50 parts of glass fiber;
the grafting ratio of the maleic anhydride grafted polypropylene ranged from 0.7 ~ 2%.
2. The high weld mark strength glass fiber reinforced polypropylene composite material as claimed in claim 1, which comprises the following components in parts by weight:
100 parts of polypropylene;
0.2-1 part of sulfonated polyolefin wax;
2.5-6 parts of maleic anhydride grafted polypropylene;
1-50 parts of glass fiber;
the grafting ratio of the maleic anhydride grafted polypropylene ranged from 0.7 ~ 2%.
3. The high weld mark strength glass fiber reinforced polypropylene composite material of claim 1, wherein the polypropylene resin has a melt flow rate of 10 ~ 40g/10min, 2.16kg/230 ℃, as measured by GB/T3682.1-2018.
4. The high weld mark strength glass fiber reinforced polypropylene composite material of claim 1, wherein the sulfonated polyolefin wax is selected from at least one or a combination of sulfonated polyethylene wax, sulfonated polypropylene wax and sulfonated polybutylene wax.
5. The high weld mark strength glass fiber reinforced polypropylene composite material of claim 4, wherein the sulfonated polyolefin wax has a sulfonation degree of 0.5 ~ 0.8.8 mmol/g and a number average molecular weight of 1000 ~ 10000.
6. The high weld mark strength glass fiber reinforced polypropylene composite material of claim 1, wherein the melt flow rate of the maleic anhydride grafted polypropylene is 50 ~ 200g/10min, 2.16kg/230 ℃, as measured by GB/T3682.1-2018.
7. The high weld mark strength glass fiber reinforced polypropylene composite material as claimed in claim 1, further comprising 0-3 parts by weight of an antioxidant.
8. The preparation method of the high weld mark strength glass fiber reinforced polypropylene composite material as claimed in any one of claims 1 to 7, which is characterized by comprising the following steps of feeding polypropylene, maleic anhydride grafted polypropylene, sulfonated polyolefin wax and an antioxidant from a main feeding port, feeding glass fiber from a side feeding port, extruding and granulating by a double-screw extruder to obtain the high weld mark strength glass fiber reinforced polypropylene composite material, wherein the extrusion temperature is set to be 180 ~ 230 ℃, the rotation speed of a main machine screw is 300 ~ 600rpm, and the length-diameter ratio of the screw is 40: 1.
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Application publication date: 20200117 |
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