CN114806005A - Super-tough scratch-resistant polypropylene composite material and preparation method thereof - Google Patents
Super-tough scratch-resistant polypropylene composite material and preparation method thereof Download PDFInfo
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- CN114806005A CN114806005A CN202111263688.9A CN202111263688A CN114806005A CN 114806005 A CN114806005 A CN 114806005A CN 202111263688 A CN202111263688 A CN 202111263688A CN 114806005 A CN114806005 A CN 114806005A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/10—Homopolymers or copolymers of propene
- C08L23/12—Polypropene
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
Abstract
The invention discloses a super-tough scratch-resistant polypropylene composite material and a preparation method thereof. The super-tough scratch-resistant polypropylene composite material is prepared from polypropylene, a flame retardant, a toughening-scratch-resistant composite auxiliary agent, a flame retardant synergist, an antioxidant and a copper aging resistant agent; the toughening-scraping resistant composite auxiliary agent is prepared from the following raw materials: ethylene-octene copolymer (POE), compatilizer, coupling agent, nano talcum powder and magnesium carbonate whisker with micropores on the surface. The super-tough scratch-resistant polypropylene composite material and the preparation method thereof overcome the technical problems of fiber floating and mold damage caused by modification of glass fiber and uneven dispersion easily caused by addition of inorganic minerals, nano talcum powder can be uniformly dispersed in microporous magnesium carbonate whiskers, and can be well combined with POE (polyolefin elastomer) and PP (polypropylene) resin under the action of a compatilizer after being soaked by a coupling agent.
Description
Technical Field
The invention relates to the technical field of chemical materials, in particular to a super-tough scratch-resistant polypropylene composite material and a preparation method thereof.
Background
Polypropylene improves the toughness of the material by adding a toughening agent, such as POE (copolymer of ethylene and octene), but the toughness is improved while the heat deformation temperature of the material is reduced, and the material is easy to scratch when in contact. The reduction of the heat distortion temperature makes the material safe for use in products with heat generation. The material surface becomes soft in macroscopic view and is easy to scratch to cause scratches, so that the use experience of a user is reduced, and the market competitiveness of the product is influenced.
In order to solve the problem, glass fiber or inorganic mineral is commonly used for filling and modifying the material so as to improve the heat distortion temperature and the scratch resistance of the material. The problem of fiber floating is easy to occur in the appearance of a product after the glass fiber reinforced material is subjected to injection molding, the glass fiber reinforced material is used, the damage to an injection mold is large, the mold needs to be made of high-hardness steel, and a frequent polishing mold is needed in the production process. The risk is two-sided, firstly, the high-hardness steel mould is used, and the mould cavity is easy to crack due to long-time production under the condition of rapid cooling and rapid heating of injection molding; second, frequent polishing of the mold may cause deformation of the mold, which affects the machining accuracy of the product. If inorganic mineral is used for filling modification, the problems can be solved, but the inorganic mineral is difficult to be uniformly combined with a resin base material even in the presence of a coupling agent, and agglomeration and uneven dispersion are easy to occur in blending modification of materials, so that the stability of the performance of injection molding products is poor.
Disclosure of Invention
The invention aims to provide a super-tough scratch-resistant polypropylene composite material with high notch impact strength, high heat deformation temperature and high scratch resistance and a preparation method thereof.
According to one aspect of the invention, the super-tough scratch-resistant polypropylene composite material is prepared from the following raw materials: polypropylene, a flame retardant, a toughening-scraping resistant composite auxiliary agent, a flame retardant synergist, an antioxidant and a copper aging resistant agent; the toughening-scraping resistant composite auxiliary agent is prepared from the following raw materials: ethylene-octene copolymer (POE), compatilizer, coupling agent, nano talcum powder and magnesium carbonate whisker with micropores on the surface. The super-tough scratch-resistant polypropylene composite material has the beneficial effects that the nano talcum powder can be uniformly dispersed in the microporous magnesium carbonate whisker, and can be well combined with POE and PP resin under the action of the compatilizer after being soaked by the coupling agent, so that the material scheme disclosed by the invention has the advantages of high notch impact strength, high heat resistance, high flame retardance, high scratch resistance and the like, and the technical problems that the glass fiber is used for modifying floating fibers and a mold is damaged and the inorganic mineral is added so as to cause uneven dispersion are solved.
In some embodiments, the particle size of the nano talc powder is 25-50nm, the diameter of the magnesium carbonate whisker is 10-15 μm, the length-diameter ratio is 30-50, and the surface micropore size of the magnesium carbonate whisker is 150-300 nm. The magnesium carbonate crystal whisker carrier has the beneficial effect that micropores of the magnesium carbonate crystal whisker can be used as a carrier for carrying the nano talcum powder.
The aspect ratio referred to in this application refers to the ratio of length to diameter.
In some embodiments, the coupling agent is one or a mixture of two of vinyltriethoxysilane (YDH-151) and Y-aminopropyltriethoxysilane (KH-550) in a mass ratio of 1-3:1, preferably 2:1, when used together. The beneficial effect is that the coupling agent soaks the magnesium carbonate crystal whisker carrying the nano talcum powder, and the bonding force between the coupling agent and the POE toughening agent can be improved.
In some embodiments, the compatibilizing agent is maleic anhydride. The magnesium carbonate whisker modified polyolefin injection molding agent has the beneficial effects that the magnesium carbonate whisker modified polyolefin injection molding agent can react with a hydrophilic group of the magnesium carbonate whisker soaked by the coupling agent, so that the bonding capability between the magnesium carbonate whisker and POE is improved, the bonding capability between the POE and PP substrate resin can also be improved, the dispersion is uniform, and the performance stability of an injection molding product is good.
The melt index of the polypropylene is 14-40g/10min, the flame retardant is a commercial hypophosphite flame retardant, the flame retardant synergist is Melamine Cyanurate (MCA), the antioxidant is tetra [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid ] pentaerythritol ester (antioxidant 1010) and bis (2, 4-di-tert-butylphenyl) pentaerythritol diphosphite (antioxidant 626), and the mass ratio of the antioxidant to the flame retardant is (1-1.6): 1, and the copper aging resistant agent is a hindered phenol non-polluting copper resistant agent.
According to another aspect of the invention, a preparation method of the super-tough scratch-resistant polypropylene composite material is provided, wherein the raw materials of the super-tough scratch-resistant polypropylene composite material are adopted, and the preparation method comprises the following specific steps:
(1) preparing a toughening-scraping resistant composite auxiliary agent: baking nano talcum powder and magnesium carbonate whisker with micropores on the surface at 80 ℃ for 4h, mixing the nano talcum powder and the magnesium carbonate whisker in a high-speed mixer until the nano talcum powder is uniformly distributed in the micropores of the magnesium carbonate whisker, soaking the magnesium carbonate whisker carrying the nano talcum powder in a coupling agent for 25-30min, and then uniformly mixing the magnesium carbonate whisker, ethylene-octene copolymer (POE) and a compatilizer in the high-speed mixer to obtain a toughening-scraping resistant composite auxiliary agent;
(2) the polypropylene, the flame retardant synergist, the antioxidant and the copper aging resistant agent in the formula amount are uniformly mixed in a high-speed mixer, and then the mixture is plasticized with the toughening-scraping resistant composite auxiliary agent through a double-screw extruder, cooled and granulated to obtain the super-tough scraping resistant polypropylene composite material.
Wherein the weight parts of the raw materials are as follows: 41-61 parts of polypropylene, 5-15 parts of flame retardant, 20-40 parts of toughening-scraping resistant composite auxiliary agent, 5-15 parts of flame retardant synergist, 0.3 part of antioxidant and 0.4 part of copper aging resistant agent, 10-15 parts of ethylene-octene copolymer (POE), 3 parts of compatilizer, 1-2 parts of coupling agent, 5-10 parts of nano talcum powder and 5-10 parts of magnesium carbonate whisker with micropores on the surface.
The length-diameter ratio of the screw of the double-screw extruder is 37-45, and the temperature and the rotating speed of each section are shown in the following table:
TABLE 1 values of temperature and speed parameters of each section of the twin-screw extruder
The preparation method of the magnesium carbonate whisker with micropores on the surface comprises the following steps: corroding the magnesium carbonate whisker by using dilute sulfuric acid containing a corrosion inhibitor with the mass concentration of 0.15%, wherein the treatment time is 20-35 s, and after the corrosion is finished, washing away the dilute sulfuric acid and the corrosion inhibitor on the surface of the magnesium carbonate whisker by using deionized water to obtain the magnesium carbonate whisker with micropores on the surface, wherein the mass concentration of the dilute sulfuric acid is 1-3%, and the corrosion inhibitor is corrosion inhibitor LAN-826. The method has the beneficial effects that under the action of the corrosion system, the corrosion speed can be well controlled, and the pore diameter of the surface micropores of the magnesium carbonate whisker is controlled at 150-300 nm.
Compared with the prior art, the invention has the advantages that: the invention discloses a super-tough scratch-resistant polypropylene composite material and a preparation method thereof for the first time, and solves the technical problems that glass fiber is used for modifying floating fiber and a mold is damaged, and inorganic minerals are added to easily cause uneven dispersion.
Detailed Description
The present invention will be described in further detail with reference to examples.
Detailed description of the preferred embodiments
Example 1
The super-tough scratch-resistant polypropylene composite material is prepared from the following raw materials in parts by weight: 41 parts of polypropylene, 15 parts of flame retardant, 24 parts of toughening-scraping resistant composite assistant, 15 parts of flame retardant synergist, 0.3 part of antioxidant and 0.4 part of copper aging resistant agent, wherein the toughening-scraping resistant composite assistant is prepared from the following raw materials in parts by weight: 10 parts of ethylene-octene copolymer (POE), 3 parts of compatilizer, 1 part of coupling agent, 5 parts of nano talcum powder and 5 parts of magnesium carbonate whisker with micropores on the surface, and the preparation method comprises the following specific steps:
(1) preparing micropores on the surface of the magnesium carbonate whisker: corroding the magnesium carbonate whisker by using dilute sulfuric acid containing a corrosion inhibitor LAN-826 with the mass concentration of 0.15%, wherein the treatment time is 20-35 s, and after the corrosion is finished, washing away the dilute sulfuric acid and the corrosion inhibitor on the surface of the magnesium carbonate whisker by using deionized water to obtain the magnesium carbonate whisker with micropores on the surface, wherein the mass concentration of the dilute sulfuric acid is 1-3%; the pore diameter of the surface micropores of the obtained magnesium carbonate crystal whisker is 150-300 nm;
(2) preparing a toughening-scraping resistant composite auxiliary agent: baking nano talcum powder and magnesium carbonate whisker with micropores on the surface at 80 ℃ for 4h, mixing the nano talcum powder and the magnesium carbonate whisker in a high-speed mixer until the nano talcum powder is uniformly distributed in the micropores of the magnesium carbonate whisker, soaking the magnesium carbonate whisker carrying the nano talcum powder in a coupling agent for 25-30min, and then uniformly mixing the magnesium carbonate whisker, ethylene-octene copolymer (POE) and a compatilizer in the high-speed mixer to obtain a toughening-scraping resistant composite auxiliary agent;
(3) the polypropylene, the flame retardant synergist, the antioxidant and the copper aging resistant agent in the formula amount are uniformly mixed in a high-speed mixer, and then the mixture is plasticized with the toughening-scraping resistant composite auxiliary agent through a double-screw extruder, cooled and granulated to obtain the super-tough scraping resistant polypropylene composite material.
In the specific embodiment, the particle size of the nano talcum powder is 25-50nm, the diameter of the magnesium carbonate whisker is 10-15 μm, and the length-diameter ratio is 30-50.
In this embodiment, the coupling agent is a mixture of vinyltriethoxysilane (YDH-151) and Y-aminopropyltriethoxysilane (KH-550) in a mass ratio of 2: 1. The compatilizer is maleic anhydride. The polypropylene has a melt index of 14-40g/10min, the flame retardant is a commercial hypophosphite flame retardant, the flame-retardant synergist is Melamine Cyanurate (MCA), the antioxidant is tetra [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid ] pentaerythritol ester (antioxidant 1010) and bis (2, 4-di-tert-butylphenyl) pentaerythritol diphosphite (antioxidant 626) which are mixed according to the mass ratio of 1.5:1, and the copper aging resistant agent is a hindered phenol non-pollution copper resistant agent.
The length-diameter ratio of the screw of the double-screw extruder in the preparation process is 37-45, and the temperature and the rotating speed of each section are shown in table 1.
Example 2
The difference from the above example 1 is that: the super-tough scratch-resistant polypropylene composite material is prepared from the following raw materials in parts by weight: 46 parts of polypropylene, 10 parts of flame retardant, 30 parts of toughening-scraping resistant composite auxiliary agent, 10 parts of flame retardant synergist, 0.3 part of antioxidant and 0.4 part of copper aging resistant agent, wherein the toughening-scraping resistant composite auxiliary agent comprises the following raw materials in parts by weight: 11 parts of ethylene-octene copolymer (POE), 3 parts of compatilizer, 2 parts of coupling agent, 7 parts of nano talcum powder and 7 parts of magnesium carbonate whisker with micropores on the surface.
Example 3
The difference from the above example 1 is that: the super-tough scratch-resistant polypropylene composite material is prepared from the following raw materials in parts by weight: 55 parts of polypropylene, 7 parts of flame retardant, 31 parts of toughening-scraping resistant composite assistant, 7 parts of flame retardant synergist, 0.3 part of antioxidant and 0.4 part of copper aging resistant agent, wherein the toughening-scraping resistant composite assistant is prepared from the following raw materials in parts by weight: 12 parts of ethylene-octene copolymer (POE), 3 parts of compatilizer, 2 parts of coupling agent, 7 parts of nano talcum powder and 7 parts of magnesium carbonate whisker with micropores on the surface.
Example 4
The difference from the above example 1 is that: the super-tough scratch-resistant polypropylene composite material is prepared from the following raw materials in parts by weight: 61 parts of polypropylene, 5 parts of flame retardant, 40 parts of toughening-scraping resistant composite auxiliary agent, 5 parts of flame retardant synergist, 0.3 part of antioxidant and 0.4 part of copper aging resistant agent, wherein the toughening-scraping resistant composite auxiliary agent comprises the following raw materials in parts by weight: 15 parts of ethylene-octene copolymer (POE), 3 parts of compatilizer, 2 parts of coupling agent, 10 parts of nano talcum powder and 10 parts of magnesium carbonate whisker with micropores on the surface.
Comparative test
The raw material formulations of comparative examples 1-3 and examples 1-4 are shown in table 2 below:
TABLE 2 Polypropylene composite formulations
Note: the magnesium carbonate whiskers of comparative example 4 were not microporous, and the magnesium carbonate whiskers of comparative examples 1-3 and examples 1-4 were microporous.
The comparative examples 1 to 4 were prepared in the same manner as in example 1, except that the formulation of each raw material was different. Injection molded samples of the materials prepared in the comparative examples and examples were tested according to the following standards, wherein the scratch resistance test was performed according to GMW14688, parallel straight lines are drawn on the surface of the material, the L value is changed according to the color difference test, the larger the Delta L is, the less the material is scratched, and the opposite is. The results are shown in table 3 below:
TABLE 3 Performance test results for various polypropylene composites
As can be seen from the above table, comparative example 1 of the present invention does not contain POE component, and the notched impact strength and toughness of the material are low. Comparative example 2 does not add magnesium carbonate whisker, but because the addition of POE component, has played the effect of toughening to the material, the breach impact strength ratio of material 1 has promoted, simultaneously because the addition of POE component, the material is able to bear or endure scraping test back delta L value grow, macroscopically the reaction goes out the material and is able to bear or endure scraping. The reason is that the nano talcum powder can not be well coupled with the coupling agent due to no magnesium carbonate crystal whisker as a carrier to carry the nano talcum powder, and the nano talcum powder is agglomerated when dispersed in the base material, so that the polymer chain can be microscopically isolated, the toughening effect of POE on the material is reduced, and the scratch resistance of the material is improved. Comparative example 3 does not add nanometer talcum powder, but because the reinforcing of magnesium carbonate whisker and POE toughening dual function, the breach impact strength of material increases, toughness reinforcing, but because the addition of POE, do not have nanometer talcum powder simultaneously and promote the scraping resistant performance of material, the material is able to bear or endure scraping resistant test back delta L and obviously increase, and the material is able to bear or endure scraping resistant performance is poor. And because POE component has poor heat resistance, the heat distortion temperature of the modified material is obviously reduced. The magnesium carbonate added in the comparative example 4 is not subjected to micropore treatment, so that the nano talcum powder is unevenly distributed in the modified material, agglomeration occurs, and the mechanical property of the material is poor. In examples 1 to 4, due to the existence of the POE component, the notch impact strength of the material is high, and the toughness of the material is obviously improved. As shown in comparative example test data, although the thermal deformation temperature of the material is reduced and the scratch resistance of the surface of the material is reduced by increasing the POE component, the toughening-scratch resistance composite additive is prepared by compounding the coupling agent and the POE by carrying the nano talcum powder on the magnesium carbonate whisker, so that the influence of the addition of the POE component on the thermal deformation temperature and the scratch resistance of the material is effectively solved. Thus, examples 1-4 have the advantages of high toughness, high heat distortion temperature, and high scratch resistance.
What has been described above are merely some embodiments of the present invention. It will be apparent to those skilled in the art that various changes and modifications can be made without departing from the inventive concept thereof, and these changes and modifications can be made without departing from the spirit and scope of the invention.
Claims (10)
1. The super-tough scratch-resistant polypropylene composite material is characterized by comprising the following raw materials: polypropylene, a flame retardant, a toughening-scraping resistant composite auxiliary agent, a flame retardant synergist, an antioxidant and a copper aging resistant agent; the toughening-scraping resistant composite auxiliary agent is prepared from the following raw materials: ethylene-octene copolymer (POE), compatilizer, coupling agent, nano talcum powder and magnesium carbonate whisker with micropores on the surface.
2. The super-tough scratch-resistant polypropylene composite material as claimed in claim 1, wherein the particle size of the nano talc powder is 25-50nm, the diameter of the magnesium carbonate whisker is 10-15 μm, the aspect ratio is 30-50, and the surface micropore size of the magnesium carbonate whisker is 150-300 nm.
3. The ultra-tough scratch-resistant polypropylene composite material according to claim 1, wherein the coupling agent is one of vinyltriethoxysilane (YDH-151) and Y-aminopropyltriethoxysilane (KH-550) or a mixture of the two in a mass ratio of 1-3: 1.
4. The super tough scratch resistant polypropylene composite material according to claim 3, wherein the coupling agent is a mixture of vinyltriethoxysilane (YDH-151) and Y-aminopropyltriethoxysilane (KH-550) in a mass ratio of 2: 1.
5. The super tough scratch resistant polypropylene composite material according to claim 1, wherein the compatilizer is maleic anhydride, the flame retardant is a commercially available hypophosphite flame retardant, the flame retardant synergist is Melamine Cyanurate (MCA), the antioxidant is pentaerythritol tetrakis [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ] (antioxidant 1010) and bis (2, 4-di-tert-butylphenyl) pentaerythritol diphosphite (antioxidant 626) in a mass ratio of (1-1.6): 1, and the copper aging resistant agent is a hindered phenol non-polluting copper resistant agent.
6. The super-tough scratch-resistant polypropylene composite material according to claim 1, wherein the raw materials comprise, by weight: 41-61 parts of polypropylene, 5-15 parts of flame retardant, 20-40 parts of toughening-scraping resistant composite auxiliary agent, 5-15 parts of flame retardant synergist, 0.3 part of antioxidant and 0.4 part of copper aging resistant agent, wherein the toughening-scraping resistant composite auxiliary agent comprises the following raw materials in parts by weight: 10-15 parts of ethylene-octene copolymer (POE), 3 parts of compatilizer, 1-2 parts of coupling agent, 5-10 parts of nano talcum powder and 5-10 parts of magnesium carbonate whisker with micropores on the surface.
7. A preparation method of the super-tough scratch-resistant polypropylene composite material is characterized by adopting the raw materials of the super-tough scratch-resistant polypropylene composite material as claimed in any one of claims 1 to 6, and comprises the following specific steps:
(1) preparing a toughening-scraping resistant composite auxiliary agent: baking nano talcum powder and magnesium carbonate whisker with micropores on the surface at 80 ℃ for 4h, mixing the nano talcum powder and the magnesium carbonate whisker in a high-speed mixer until the nano talcum powder is uniformly distributed in the micropores of the magnesium carbonate whisker, soaking the magnesium carbonate whisker carrying the nano talcum powder in a coupling agent for 25-30min, and then uniformly mixing the magnesium carbonate whisker, ethylene-octene copolymer (POE) and a compatilizer in the high-speed mixer to obtain a toughening-scraping resistant composite auxiliary agent;
(2) the polypropylene, the flame retardant synergist, the antioxidant and the copper aging resistant agent in the formula amount are uniformly mixed in a high-speed mixer, and then the mixture is plasticized with the toughening-scraping resistant composite auxiliary agent through a double-screw extruder, cooled and granulated to obtain the super-tough scraping resistant polypropylene composite material.
8. The method for preparing the super tough scratch and tear resistant polypropylene composite material according to claim 7, wherein the length-diameter ratio of the screws of the twin-screw extruder is 37-45, and the temperature and the rotating speed of each section are shown in the following table:
9. the preparation method of the super-tough scratch-resistant polypropylene composite material as claimed in claim 7, wherein the preparation method of the magnesium carbonate whisker with micropores on the surface comprises the following steps: and (2) corroding the magnesium carbonate whisker by using dilute sulfuric acid containing a corrosion inhibitor with the mass concentration of 0.15%, wherein the treatment time is 20-35 s, and after the corrosion is finished, washing away the dilute sulfuric acid and the corrosion inhibitor on the surface of the magnesium carbonate whisker by using deionized water to obtain the magnesium carbonate whisker with micropores on the surface.
10. The preparation method of the super-tough scratch-resistant polypropylene composite material as claimed in claim 9, wherein the mass concentration of the dilute sulfuric acid is 1% -3%, and the corrosion inhibitor is a corrosion inhibitor LAN-826.
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| CN107880393A (en) * | 2017-12-07 | 2018-04-06 | 公牛集团有限公司 | A kind of socket ultra-toughness scratch-resistant PP composite material and preparation method |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107880393A (en) * | 2017-12-07 | 2018-04-06 | 公牛集团有限公司 | A kind of socket ultra-toughness scratch-resistant PP composite material and preparation method |
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