CN109535563B - Environment-friendly composite material and preparation method and application thereof - Google Patents
Environment-friendly composite material and preparation method and application thereof Download PDFInfo
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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
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2217—Oxides; Hydroxides of metals of magnesium
- C08K2003/2224—Magnesium hydroxide
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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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2296—Oxides; Hydroxides of metals of zinc
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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Abstract
The invention provides an environment-friendly composite material which is prepared from the following components in parts by weight: 100 parts of PP, 3-4 parts of toughening agent, 0.5-1 part of antioxidant, 8-12 parts of flame retardant, 1-1.5 parts of lubricant, 1-2 parts of PAMAM and 10-15 parts of zinc-silicon composite oxide. The invention also discloses a preparation method of the environment-friendly composite material. The environment-friendly composite material provided by the invention has the advantages of low VOC content, strong wear resistance, low temperature resistance and aging resistance.
Description
Technical Field
The invention relates to a composite material, in particular to an environment-friendly composite material and a preparation method and application thereof.
Background
Resin-based composite materials are fiber-reinforced materials using organic polymers as a matrix, and usually, fiber reinforcements such as glass fibers, carbon fibers, basalt fibers, or aramid fibers are used, and commonly used matrices include polyethylene, polypropylene, polyvinyl chloride, epoxy resins, phenol resins, and the like. Among them, polypropylene (abbreviated as PP in english) is a thermoplastic general-purpose plastic with very excellent comprehensive properties, and has the characteristics of easy processing, low density, low production cost and the like, so polypropylene has wide application in the industries of household appliances, packaging materials of daily necessities, automobile industry and the like, and becomes one of the plastics with the fastest growth rate in recent years. However, polypropylene also has some disadvantages, such as: the creep resistance is poor, the melting point is low, the dimensional stability is poor, the thermal deformation temperature is low, the low-temperature brittleness is limited, and the application of the polypropylene as an engineering stressed material is restricted, so that the performance improvement by filling the polypropylene with inorganic substances is a common enhancement mode at present, but the common inorganic substances can react with a polypropylene matrix and an auxiliary agent to generate micromolecular volatile organic substances, so that the VOC content is higher, and the defect of insufficient environmental protection exists.
Chinese patent with application number CN201810341775.3 discloses a modified polypropylene composite material and a preparation method thereof, wherein the modified polypropylene composite material comprises the following components in parts by weight: 30-50 parts of polypropylene, 10-30 parts of filling reinforcing agent, 15-25 parts of flame retardant, 5-15 parts of toughening agent, 1-5 parts of antioxidant and 1-4 parts of black matrix. The composite material also has the problems of higher VOC content and insufficient environmental protection, and has poor wear resistance, low temperature resistance and aging resistance.
Disclosure of Invention
The invention aims to provide an environment-friendly composite material which is low in VOC content and has high wear resistance, low temperature resistance and ageing resistance.
In order to solve the technical problems, the technical scheme of the invention is as follows:
an environment-friendly composite material is prepared from the following components in parts by weight: 100 parts of PP, 3-4 parts of toughening agent, 0.5-1 part of antioxidant, 8-12 parts of flame retardant, 1-1.5 parts of lubricant, 1-2 parts of PAMAM and 10-15 parts of zinc-silicon composite oxide.
Further, the melt index of the PP provided by the invention is 5-10g/10 min.
Further, the toughening agent is POE.
Furthermore, the antioxidant is antioxidant 1010 or antioxidant DSTP.
Further, the flame retardant is magnesium hydroxide.
Further, the lubricant of the present invention is ethylene bis stearamide.
Further, the preparation steps of the PAMAM of the invention are as follows:
A1. adding anhydrous methanol and ethylenediamine into a reaction bottle, placing the reaction bottle in an ice-water bath, stirring for 1 hour, dropwise adding methyl acrylate into the reaction bottle, heating to 30 ℃, stirring for reaction for 24 hours, vacuumizing, and removing the anhydrous methanol and unreacted methyl acrylate to obtain PAMAM-0.5G;
A2. adding absolute methanol and PAMAM-0.5G into a reaction bottle A, placing the reaction bottle A in an ice-water bath, stirring, adding absolute ethanol and ethylenediamine into the reaction bottle B, placing the reaction bottle B in the ice-water bath, stirring for 1 hour to obtain an ethylenediamine solution, dropwise adding the ethylenediamine solution into the reaction bottle A, heating to 25 ℃, stirring for 24 hours, adding n-butyl alcohol, vacuumizing at 80 ℃, and removing the absolute methanol and the excessive ethylenediamine to obtain the PAMAM.
Further, in the step A1, the weight ratio of the anhydrous methanol to the ethylenediamine to the methyl acrylate is 15:1: 8.7; in the step A2, the weight ratio of the anhydrous methanol to the PAMAM-0.5G in the reaction bottle A is 1:1, the mass fraction of the ethylenediamine solution is 68.9%, and the weight ratio of the PAMAM-0.5G to the ethylenediamine solution is 1: 3.4.
Further, the preparation steps of the zinc-silicon composite oxide of the invention are as follows:
adding zinc oxide into deionized water with the weight of 5 times of that of the zinc oxide, carrying out ultrasonic oscillation for 30 minutes, carrying out magnetic stirring for 1 hour, dropwise adding 10% of sodium silicate solution with mass fraction, adjusting the pH value to 9, heating to 90 ℃, continuing carrying out magnetic stirring for 1 hour, then aging for 2 hours, filtering and washing the obtained product, and drying at 90 ℃ to obtain the zinc-silicon composite oxide, wherein the weight ratio of the sodium silicate solution to the zinc oxide is 1: 2.
The invention also provides a preparation method of the environment-friendly composite material.
In order to solve the technical problems, the technical scheme is as follows:
a preparation method of an environment-friendly composite material comprises the following steps:
B1. weighing the components according to the parts by weight, adding the flame retardant, the PAMAM and the zinc-silicon composite oxide into a mixer, and mixing for 40 minutes at the rotating speed of 800 revolutions per minute to obtain a mixture;
B2. and B1, uniformly mixing the mixture obtained in the step B with other components, transferring the mixture into a double-screw extruder to extrude to obtain an extruded material, granulating the extruded material by using a granulator, and cooling the granulated material to room temperature by water to obtain the environment-friendly composite material, wherein the extrusion temperature of the double-screw extruder is 180-220 ℃, and the rotating speed of a screw is 40 rpm.
Therefore, compared with the prior art, the invention has the following beneficial effects:
1) the zinc oxide has good ultraviolet absorption performance, but the mechanical property and the thermal stability of the zinc oxide are not good, and the silicon dioxide has good mechanical property, wear resistance and thermal stability.
2) The flame retardant and the zinc-silicon composite oxide used in the invention both belong to inorganic substances and also have the defect of higher VOC content, so the dendritic macromolecular PAMAM is prepared, the molecular surface of the PAMAM has high-density active group-amino, the PAMAM can be coated on the surfaces of the flame retardant and the zinc-silicon composite oxide during blending, the flame retardant, the zinc-silicon composite oxide and a polypropylene matrix are separated, and the PAMAM and the polypropylene matrix have better compatibility, so that the flame retardant and the zinc-silicon composite oxide are not easy to separate out, the reaction between the flame retardant and the zinc-silicon composite oxide and the polypropylene matrix is effectively reduced, and low-molecular volatile organic matters are generated, thereby the VOC content of the composite material is effectively reduced, and the environmental protection performance of the composite material is improved; in addition, the PAMAM can also improve the dispersibility of the flame retardant and the zinc-silicon composite oxide in a polypropylene matrix, so that the wear resistance, the low temperature resistance and the aging resistance of the composite material are further improved.
Detailed Description
The present invention will be described in detail with reference to specific embodiments, which are illustrative of the invention and are not to be construed as limiting the invention.
Example 1
The environment-friendly composite material is prepared from the following components in parts by weight: 100 parts of PP with the melt index of 5-10g/10min, 3 parts of POE, 10101 parts of antioxidant, 11 parts of magnesium hydroxide, 1.2 parts of ethylene bis stearamide, 1 part of PAMAM and 15 parts of zinc-silicon composite oxide.
The preparation method comprises the following steps:
(1) adding anhydrous methanol and ethylenediamine into a reaction bottle, placing the reaction bottle in an ice-water bath, stirring for 1 hour, dropwise adding methyl acrylate into the reaction bottle, heating to 30 ℃, stirring for reaction for 24 hours, vacuumizing, and removing the anhydrous methanol and unreacted methyl acrylate to obtain PAMAM-0.5G, wherein the weight ratio of the anhydrous methanol to the ethylenediamine to the methyl acrylate is 15:1: 8.7;
(2) adding absolute methanol and PAMAM-0.5G into a reaction bottle A, placing the reaction bottle A in an ice-water bath, stirring, adding absolute ethanol and ethylenediamine into a reaction bottle B, placing the reaction bottle B in the ice-water bath, stirring for 1 hour to obtain an ethylenediamine solution, dropwise adding the ethylenediamine solution into the reaction bottle A, heating to 25 ℃, stirring for 24 hours, adding n-butyl alcohol, vacuumizing at 80 ℃, removing the absolute methanol and the excessive ethylenediamine to obtain the PAMAM, wherein the weight ratio of the absolute methanol to the PAMAM-0.5G in the reaction bottle A is 1:1, the mass fraction of the ethylenediamine solution is 68.9%, and the weight ratio of the PAMAM-0.5G to the ethylenediamine solution is 1: 3.4;
(3) adding zinc oxide into deionized water with the weight of 5 times, performing ultrasonic oscillation for 30 minutes, performing magnetic stirring for 1 hour, dropwise adding 10% sodium silicate solution with mass fraction, adjusting the pH value to 9, heating to 90 ℃, continuing to perform magnetic stirring for 1 hour, then aging for 2 hours, filtering and washing the obtained product, and drying at 90 ℃ to obtain a zinc-silicon composite oxide, wherein the weight ratio of the sodium silicate solution to the zinc oxide is 1: 2;
(4) weighing the components according to the parts by weight, adding the flame retardant, the PAMAM and the zinc-silicon composite oxide into a mixer, and mixing for 40 minutes at the rotating speed of 800 revolutions per minute to obtain a mixture;
(5) and (3) uniformly mixing the mixture obtained in the step (4) with other components, transferring the mixture into a double-screw extruder to extrude to obtain an extruded material, granulating the extruded material by using a granulator, and cooling the granulated material to room temperature by water to obtain the environment-friendly composite material, wherein the extrusion temperature of the double-screw extruder is 180-220 ℃, and the rotating speed of a screw is 40 rpm.
Example 2
The environment-friendly composite material is prepared from the following components in parts by weight: 100 parts of PP with the melt index of 5-10g/10min, 4 parts of POE, 0.5 part of antioxidant DSTP, 9 parts of magnesium hydroxide, 1.1 part of ethylene bis-stearamide, 1.6 parts of PAMAM and 11 parts of zinc-silicon composite oxide.
The preparation method is the same as that of example 1.
Example 3
The environment-friendly composite material is prepared from the following components in parts by weight: 100 parts of PP with the melt index of 5-10g/10min, 3.5 parts of POE, 0.8 part of antioxidant DSTP, 10 parts of magnesium hydroxide, 1.4 parts of ethylene bis stearamide, 1.5 parts of PAMAM and 12 parts of zinc-silicon composite oxide.
The preparation method is the same as that of example 1.
Example 4
The environment-friendly composite material is prepared from the following components in parts by weight: 100 parts of PP with the melt index of 5-10g/10min, 3.2 parts of POE, 10100.9 parts of antioxidant, 8 parts of magnesium hydroxide, 1.5 parts of ethylene bis stearamide, 1.2 parts of PAMAM and 14 parts of zinc-silicon composite oxide.
The preparation method is the same as that of example 1.
Example 5
The environment-friendly composite material is prepared from the following components in parts by weight: 100 parts of PP with the melt index of 5-10g/10min, 3.6 parts of POE, 0.6 part of antioxidant DSTP, 12 parts of magnesium hydroxide, 1 part of ethylene bis-stearamide, 2 parts of PAMAM and 10 parts of zinc-silicon composite oxide.
The preparation method is the same as that of example 1.
Reference example 1
The components do not include PAMAM, and other components and preparation methods are the same as those of example 3.
Reference example 2
The components do not include the zinc-silicon composite oxide, and other components and the preparation method are the same as those of the embodiment 3.
Comparative example
The comparative example is example 1 of the chinese invention having application number CN 201810341775.3.
The first experimental example: VOC content testing
The VOC content of each composite was tested with reference to the PV3341 standard. The test results are shown in table 1:
| VOC content (μ gC/g) | |
| Example 1 | 23 |
| Example 2 | 28 |
| Example 3 | 21 |
| Example 4 | 30 |
| Example 5 | 26 |
| Reference example 1 | 95 |
| Reference example 2 | 29 |
| Comparative example | 107 |
TABLE 1
As can be seen from Table 1, the VOC content of inventive examples 1-5 is significantly lower than that of the comparative examples. The compositions of reference examples 1 and 2 are different from those of examples 1 to 5, wherein the VOC content of reference example 1 is increased greatly, which shows that the VOC content of the composite material can be greatly reduced by PAMAM; the VOC content of reference example 2 was almost the same as that of examples 1 to 5, showing that the zinc-silicon composite oxide had little effect on the VOC content.
Experiment example two: abrasion resistance test
The abrasion tester is used for testing the friction mass loss of each composite material by referring to GB/T3960-. The test results are shown in table 2:
| loss of friction mass (mg) | |
| Example 1 | 101.3 |
| Example 2 | 101.9 |
| Example 3 | 101.0 |
| Example 4 | 102.1 |
| Example 5 | 102.4 |
| Reference example 1 | 148.7 |
| Reference example 2 | 322.5 |
| Comparative example | 456.6 |
TABLE 2
As can be seen from Table 2, the wear quality loss of examples 1 to 5 of the present invention is significantly less than that of the comparative examples, indicating that the present invention has a strong wear resistance. The components of reference examples 1 and 2 are different from those of examples 1 to 5, wherein the loss of wear quality of reference example 2 is increased greatly, which shows that the zinc-silicon composite oxide can greatly improve the wear resistance of the composite material; the abrasion mass loss of reference example 1 is increased a little, and shows that PAMAM can effectively improve the dispersibility of the zinc-silicon composite oxide in the polypropylene matrix.
Experiment example three: low temperature resistance test
The notched impact strength of each composite material at 25 ℃ and-30 ℃ is measured by referring to the GB/T1043-93 standard, the notched impact strength reduction rate is calculated, the notched impact strength reduction rate = (25 ℃ notched impact strength-30 ℃ notched impact strength)/25 ℃ notched impact strength is multiplied by 100%, the lower the notched impact strength reduction rate is, the stronger the low temperature resistance is, and the test results are shown in Table 3:
| notched impact strength reduction (%) | |
| Example 1 | 48.7 |
| Example 2 | 48.9 |
| Example 3 | 48.3 |
| Example 4 | 49.0 |
| Example 5 | 48.6 |
| Reference example 1 | 52.8 |
| Reference example 2 | 54.4 |
| Comparative example | 56.2 |
TABLE 3
As can be seen from Table 3, the notched impact strength of examples 1 to 5 of the present invention was significantly lower than that of the comparative examples, indicating that the present invention has high low-temperature resistance. The compositions of reference examples 1 and 2 are different from those of examples 1 to 5, wherein the rate of decrease in notched impact strength of reference example 2 is increased a lot, which shows that the zinc-silicon composite oxide is effective in improving the low temperature resistance of the composite material; the decrease rate of the notched impact strength of reference example 1 is increased to some extent, which shows that PAMAM can effectively improve the dispersibility of the zinc-silicon composite oxide in the polypropylene matrix.
Experimental example four: light aging resistance test
The test is carried out in an artificial ultraviolet accelerated aging box, the aging time is 960 hours, the ultraviolet wavelength is 340nm, the irradiation intensity is 0.89W/m, the static bending strength of the composite material before and after aging is determined by referring to GB/T23137-:
| static bending Strength Retention (%) | |
| Example 1 | 91.8 |
| Example 2 | 91.5 |
| Example 3 | 92.1 |
| Example 4 | 91.6 |
| Example 5 | 91.7 |
| Reference example 1 | 85.4 |
| Reference example 2 | 80.3 |
| Comparative example | 75.9 |
TABLE 4
As can be seen from Table 4, the static bending strength retention rates of the examples 1 to 5 of the present invention are significantly higher than those of the comparative examples, indicating that the present invention has strong light aging resistance. The components of reference examples 1 and 2 are different from those of examples 1 to 5, wherein the static bending strength retention rate of the reference example 2 is greatly reduced, which shows that the zinc-silicon composite oxide can effectively improve the light aging resistance of the composite material; the static bending strength retention rate of the reference example 1 is reduced a little, and the PAMAM can effectively improve the dispersibility of the zinc-silicon composite oxide in the polypropylene matrix.
The foregoing embodiments are merely illustrative of the principles and utilities of the present invention and are not intended to limit the invention. Any person skilled in the art can modify or change the above-mentioned embodiments without departing from the spirit and scope of the present invention. Accordingly, it is intended that all equivalent modifications or changes which can be made by those skilled in the art without departing from the spirit and technical spirit of the present invention be covered by the claims of the present invention.
Claims (8)
1. An environment-friendly composite material, which is characterized in that: the composition is prepared from the following components in parts by weight: 100 parts of PP, 3-4 parts of toughening agent, 0.5-1 part of antioxidant, 8-12 parts of flame retardant, 1-1.5 parts of lubricant, 1-2 parts of PAMAM and 10-15 parts of zinc-silicon composite oxide;
the preparation steps of the zinc-silicon composite oxide are as follows:
adding zinc oxide into deionized water with the weight of 5 times, performing ultrasonic oscillation for 30 minutes, performing magnetic stirring for 1 hour, dropwise adding 10% sodium silicate solution with mass fraction, adjusting the pH value to 9, heating to 90 ℃, continuing to perform magnetic stirring for 1 hour, then aging for 2 hours, filtering and washing the obtained product, and drying at 90 ℃ to obtain a zinc-silicon composite oxide, wherein the weight ratio of the sodium silicate solution to the zinc oxide is 1: 2;
the preparation steps of the PAMAM are as follows:
A1. adding anhydrous methanol and ethylenediamine into a reaction bottle, placing the reaction bottle in an ice-water bath, stirring for 1 hour, dropwise adding methyl acrylate into the reaction bottle, heating to 30 ℃, stirring for reaction for 24 hours, vacuumizing, and removing the anhydrous methanol and unreacted methyl acrylate to obtain PAMAM-0.5G;
A2. adding absolute methanol and PAMAM-0.5G into a reaction bottle A, placing the reaction bottle A in an ice-water bath, stirring, adding absolute ethanol and ethylenediamine into the reaction bottle B, placing the reaction bottle B in the ice-water bath, stirring for 1 hour to obtain an ethylenediamine solution, dropwise adding the ethylenediamine solution into the reaction bottle A, heating to 25 ℃, stirring for 24 hours, adding n-butyl alcohol, vacuumizing at 80 ℃, and removing the absolute methanol and the excessive ethylenediamine to obtain the PAMAM;
the preparation steps of the environment-friendly composite material are as follows:
B1. weighing the components according to the parts by weight, adding the flame retardant, the PAMAM and the zinc-silicon composite oxide into a mixer, and mixing for 40 minutes at the rotating speed of 800 revolutions per minute to obtain a mixture;
B2. and B1, uniformly mixing the mixture obtained in the step B with other components, transferring the mixture into a double-screw extruder to extrude to obtain an extruded material, granulating the extruded material by using a granulator, and cooling the granulated material to room temperature by water to obtain the environment-friendly composite material, wherein the extrusion temperature of the double-screw extruder is 180-220 ℃, and the rotating speed of a screw is 40 rpm.
2. The environmentally friendly composite material of claim 1, wherein: the melt index of the PP is 5-10g/10 min.
3. The environmentally friendly composite material of claim 1, wherein: the toughening agent is POE.
4. The environmentally friendly composite material of claim 1, wherein: the antioxidant is antioxidant 1010 or antioxidant DSTP.
5. The environmentally friendly composite material of claim 1, wherein: the flame retardant is magnesium hydroxide.
6. The environmentally friendly composite material of claim 5, wherein: the lubricant is ethylene bis stearamide.
7. The environmentally friendly composite material of claim 1, wherein: in the step A1, the weight ratio of the anhydrous methanol to the ethylenediamine to the methyl acrylate is 15:1: 8.7; in the step A2, the weight ratio of the anhydrous methanol to the PAMAM-0.5G in the reaction bottle A is 1:1, the mass fraction of the ethylenediamine solution is 68.9%, and the weight ratio of the PAMAM-0.5G to the ethylenediamine solution is 1: 3.4.
8. The method for preparing the environment-friendly composite material according to any one of claims 1 to 7, wherein: the method comprises the following steps:
B1. weighing the components according to the parts by weight, adding the flame retardant, the PAMAM and the zinc-silicon composite oxide into a mixer, and mixing for 40 minutes at the rotating speed of 800 revolutions per minute to obtain a mixture;
B2. and B1, uniformly mixing the mixture obtained in the step B with other components, transferring the mixture into a double-screw extruder to extrude to obtain an extruded material, granulating the extruded material by using a granulator, and cooling the granulated material to room temperature by water to obtain the environment-friendly composite material, wherein the extrusion temperature of the double-screw extruder is 180-220 ℃, and the rotating speed of a screw is 40 rpm.
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