CN111748150A - Recycled polypropylene material for vehicles and preparation method thereof - Google Patents
Recycled polypropylene material for vehicles and preparation method thereof Download PDFInfo
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- 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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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F255/00—Macromolecular compounds obtained by polymerising monomers on to polymers of hydrocarbons as defined in group C08F10/00
- C08F255/02—Macromolecular compounds obtained by polymerising monomers on to polymers of hydrocarbons as defined in group C08F10/00 on to polymers of olefins having two or three carbon atoms
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- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/08—Polymer mixtures characterised by other features containing additives to improve the compatibility between two polymers
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- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/14—Polymer mixtures characterised by other features containing polymeric additives characterised by shape
- C08L2205/16—Fibres; Fibrils
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Abstract
The invention relates to a recycled polypropylene material for vehicles, which is prepared from recycled polypropylene resin, plant fibers, silicon oxide spiral nanotubes, a silane cross-linking agent and a cross-linking catalyst; wherein, the plant fiber is loaded with a peroxide initiator; the invention also relates to a preparation method of the polypropylene material. The polypropylene material and the injection molding finished product thereof have good mechanical properties; the molecular chain of the polypropylene resin is crosslinked under the action of benzoyl peroxide, allyl trimethoxy silane and dibutyltin octanoate to form a net structure, so that the mechanical property of an injection molding finished product is improved; meanwhile, because the grafting reaction is carried out near the plant fiber, the degree of the net-shaped structure of the polypropylene formed around the plant fiber is higher, so that the plant fiber can be better fused in the polypropylene base material, thereby better playing the role of the plant fiber and further improving the mechanical property of the injection molding finished product of the polypropylene material.
Description
Technical Field
The invention relates to the field of polypropylene materials, in particular to a recycled polypropylene material for vehicles and a preparation method thereof.
Background
With the continuous development of the automobile industry, the usage amount of polypropylene which is an important automobile plastic is also continuously increased; correspondingly, the problem of processing the waste and old automotive polypropylene materials is gradually highlighted; at present, a considerable part of automotive polypropylene is mainly treated by burning or landfill, so that resources are wasted, and adverse effects on the environment are also generated; therefore, the polypropylene material for the vehicle is recycled, so that the utilization rate of resources can be improved, and the environmental pollution can be reduced; however, the recycled polypropylene material generally has the problem of insufficient mechanical properties.
Disclosure of Invention
The invention overcomes the defects of the prior art and provides the recycled polypropylene material for the vehicle with good mechanical property and the preparation method thereof.
In order to achieve the purpose, the invention adopts the technical scheme that: provides a recycled polypropylene material for vehicles, which is characterized in that: the preparation raw materials comprise recycled polypropylene resin, plant fiber, silicon oxide spiral nano-tube, silane cross-linking agent and cross-linking catalyst; the plant fiber is loaded with a peroxide initiator.
Preferably, the silane cross-linking agent is allyl trimethoxy silane; the crosslinking catalyst is dibutyltin octoate; the peroxide initiator is benzoyl peroxide.
As a more preferred embodiment, the silica helical nanotubes are 1, 2-ethylene silica helical nanotubes.
More preferably, the paint also comprises a filler, a compatilizer and an antioxidant.
As a more preferable scheme, the preparation raw materials comprise 100 parts by mass of recycled polypropylene resin, 12-24 parts by mass of plant fiber loaded with benzoyl peroxide, 15-25 parts by mass of filler, 6-12 parts by mass of 1, 2-ethylene silicon oxide spiral nano-tube, 1-3 parts by mass of allyl trimethoxy silane, 0.2-1 part by mass of dibutyltin octanoate, 1-3 parts by mass of compatilizer and 0.5-1.5 parts by mass of antioxidant.
The invention also provides a method for preparing the recycled polypropylene material for the vehicle, which is characterized by comprising the following steps: the method comprises the following steps:
firstly, dissolving a peroxide initiator in a solvent, and then soaking plant fibers in the solvent; after the plant fiber is taken out, heating to remove the solvent; controlling the weight of the treated plant fiber to be increased by 4-10%;
weighing raw materials except for the crosslinking catalyst and mixing;
introducing the mixture into an extruder for melting and extruding; weighing a crosslinking catalyst and adding the crosslinking catalyst into the middle section of the extruder;
and cooling the extruded blank to obtain a finished product.
Preferably, the solvent is chloroform.
As a preferred scheme, the extruder is a double-screw extruder and comprises ten working areas; the crosslinking catalyst is added from six zones of the extruder.
As a more preferable scheme, the temperature of each work area of the extruder is not lower than 180 ℃, and the rotating speed of the twin screw is 250-300 rpm.
As a more preferable scheme, the blank is cooled by circulating water at the temperature of 5-25 ℃.
The invention has the beneficial technical effects that: provides a recycled polypropylene material with good mechanical property for vehicles and a preparation method thereof; the polypropylene material and the injection molding finished product thereof prepared by the invention have good mechanical properties; in the invention, polypropylene resin and allyltrimethoxysilane are firstly initiated by benzoyl peroxide loaded on plant fibers to generate a grafting reaction; then, under the action of a crosslinking catalyst dibutyltin octylate, molecular chains of polypropylene are crosslinked to form a net structure, so that the mechanical properties of the polypropylene composite material and the injection molding finished product thereof are improved; meanwhile, because the grafting reaction is carried out near the plant fiber, the degree of the net-shaped structure of the polypropylene formed around the plant fiber is higher, so that the plant fiber can be better fused in the polypropylene base material, thereby better playing the role of the plant fiber and further improving the mechanical property of the injection molding finished product of the polypropylene material.
Detailed Description
The invention is further described with reference to specific examples. The following examples are only for illustrating the technical solutions of the present invention more clearly, and the protection scope of the present invention is not limited thereby.
Example 1
A recycled and reused polypropylene material for vehicles is prepared from 100 parts by mass of recycled polypropylene resin, 16 parts by mass of benzoyl peroxide-loaded plant fiber, 20 parts by mass of filler, 8 parts by mass of 1, 2-ethylene silicon oxide spiral nano-tubes, 2 parts by mass of allyl trimethoxy silane, 1 part by mass of dibutyltin octanoate, 2 parts by mass of compatilizer and 1 part by mass of antioxidant.
Wherein: the plant fiber is porous carbon fiber, the diameter of the plant fiber is 5-8 mu m, and the length of the plant fiber is 15-20 mm; the surface of the plant fiber has a plurality of holes, and benzoyl peroxide serving as a peroxide initiator is loaded in the holes.
The filler is talcum powder with the surface coated by epoxy resin, the particle size of the talcum powder is 15-35 mu m, and the talcum powder and the polypropylene base material have better compatibility after being coated by the epoxy resin.
The 1, 2-ethylene silicon oxide spiral nanotube is a silicon oxide spiral nanotube which is a hollow tube with a spiral structure, the length of the tube is 3.0-8.0 mu m, the inner diameter of the tube is 50-200nm, and the tube wall has a porous structure; the silicon oxide spiral nano tube can be wound with a polypropylene base material to a certain extent, so that the mechanical properties of the polypropylene material and the injection molding product thereof can be improved. The silica helical nanotube can be prepared by a sol-gel replication method.
Allyl trimethoxy silane as silane cross-linking agent; dibutyl tin octoate is used as a crosslinking catalyst.
The compatilizer is maleic anhydride grafted polypropylene; the antioxidant is hindered phenol antioxidant.
The preparation method of the polypropylene material comprises the following steps:
(1) firstly, dissolving benzoyl peroxide in trichloromethane, and then soaking plant fibers in a solution to enable the solution to be attached to the plant fibers; then taking out, distilling the trichloromethane at 65 ℃, and collecting and recycling the trichloromethane; the weight of the treated plant fiber is controlled to be 6 percent, namely the amount of benzoyl peroxide attached to the surface of the plant fiber is 6 percent of the amount of the plant fiber.
(2) Weighing the recycled polypropylene resin, the plant fiber loaded with benzoyl peroxide, the filler, the 1, 2-ethylene silicon oxide spiral nanotube, the allyl trimethoxy silane, the compatilizer and the antioxidant according to the formula, and uniformly mixing.
(3) Introducing the mixture into a double-screw extruder for melting and extruding; the temperature at the time of melting was: 185 ℃ in the first zone, 205 ℃ in the second zone, 205 ℃ in the third zone, 215 ℃ in the fourth zone, 215 ℃ in the fifth zone, 215 ℃ in the sixth zone, 220 ℃ in the seventh zone, 225 ℃ in the eighth zone, 225 ℃ in the ninth zone and 225 ℃ in the tenth zone; the rotating speed of the double screws is 300 rpm; simultaneously, dibutyltin octoate is weighed according to the formula and added from six zones of an extruder.
In the melting process, polypropylene resin and allyltrimethoxysilane are firstly initiated to carry out grafting reaction under the initiation of benzoyl peroxide loaded on plant fibers; then, under the action of a crosslinking catalyst dibutyltin octylate, molecular chains of polypropylene are crosslinked to form a net structure, so that the mechanical properties of the polypropylene composite material and the injection molding finished product thereof are improved; because the grafting reaction is generated near the plant fiber, the degree of the net-shaped structure of the polypropylene formed around the plant fiber is higher, so that the plant fiber can be better fused in the polypropylene base material, thereby better playing the role of the plant fiber and further improving the mechanical property of the polypropylene material injection molding finished product.
(4) Cooling the extruded blank by circulating water at 5-25 ℃; and granulating to obtain the recycled automotive polypropylene material.
Example 2
A recycled and reused polypropylene material for vehicles is prepared from 100 parts by mass of recycled polypropylene resin, 12 parts by mass of benzoyl peroxide-loaded plant fiber, 25 parts by mass of filler, 6 parts by mass of 1, 2-ethylene silicon oxide spiral nano-tube, 1 part by mass of allyl trimethoxy silane, 0.2 part by mass of dibutyltin octanoate, 1 part by mass of compatilizer and 0.5 part by mass of antioxidant.
The preparation method of the polypropylene material comprises the following steps:
(1) firstly, dissolving benzoyl peroxide in trichloromethane, and then soaking plant fibers in a solution to enable the solution to be attached to the plant fibers; then taking out, distilling the trichloromethane at 65 ℃, and collecting and recycling the trichloromethane; the weight of the plant fiber is increased by 10 percent after the control treatment.
(2) Weighing the recycled polypropylene resin, the plant fiber loaded with benzoyl peroxide, the filler, the 1, 2-ethylene silicon oxide spiral nanotube, the allyl trimethoxy silane, the compatilizer and the antioxidant according to the formula, and uniformly mixing.
(3) Introducing the mixture into a double-screw extruder for melting and extruding; the temperature at the time of melting was: 190 ℃ in the first zone, 200 ℃ in the second zone, 205 ℃ in the third zone, 205 ℃ in the fourth zone, 210 ℃ in the fifth zone, 215 ℃ in the sixth zone, 220 ℃ in the seventh zone, 220 ℃ in the eighth zone, 225 ℃ in the ninth zone and 225 ℃ in the tenth zone; the rotating speed of the double screws is 250 rpm; simultaneously, dibutyltin octoate is weighed according to the formula and added from six zones of an extruder.
(4) Cooling the extruded blank by circulating water at 5-25 ℃; and granulating to obtain the recycled automotive polypropylene material.
Example 3
A recycled and reused polypropylene material for vehicles is prepared from 100 parts by mass of recycled polypropylene resin, 24 parts by mass of plant fiber loaded with benzoyl peroxide, 15 parts by mass of filler, 12 parts by mass of 1, 2-ethylene silicon oxide spiral nano-tubes, 3 parts by mass of allyl trimethoxy silane, 0.5 part by mass of dibutyltin octanoate, 3 parts by mass of compatilizer and 1.5 parts by mass of antioxidant.
The preparation method of the polypropylene material comprises the following steps:
(1) firstly, dissolving benzoyl peroxide in trichloromethane, and then soaking plant fibers in a solution to enable the solution to be attached to the plant fibers; then taking out, distilling the trichloromethane at 65 ℃, and collecting and recycling the trichloromethane; the weight of the plant fiber after the control treatment is increased by 4 percent.
(2) Weighing the recycled polypropylene resin, the plant fiber loaded with benzoyl peroxide, the filler, the 1, 2-ethylene silicon oxide spiral nanotube, the allyl trimethoxy silane, the compatilizer and the antioxidant according to the formula, and uniformly mixing.
(3) Introducing the mixture into a double-screw extruder for melting and extruding; the temperature at the time of melting was: 185 ℃ in the first zone, 205 ℃ in the second zone, 205 ℃ in the third zone, 215 ℃ in the fourth zone, 215 ℃ in the fifth zone, 215 ℃ in the sixth zone, 220 ℃ in the seventh zone, 225 ℃ in the eighth zone, 225 ℃ in the ninth zone and 225 ℃ in the tenth zone; the rotating speed of the double screws is 300 rpm; simultaneously, dibutyltin octoate is weighed according to the formula and added from six zones of an extruder.
(4) Cooling the extruded blank by circulating water at 5-25 ℃; and granulating to obtain the recycled automotive polypropylene material.
Comparative example 1
This comparative example differs from example 1 in that: the raw material composition does not contain benzoyl oxide, allyl trimethoxy silane and dibutyltin octoate; the preparation method does not comprise the step (1).
The concrete raw materials comprise: 100 parts by mass of recycled polypropylene resin, 15 parts by mass of plant fiber, 20 parts by mass of filler, 8 parts by mass of 1, 2-ethylene silicon oxide spiral nanotube, 2 parts by mass of compatilizer and 1 part by mass of antioxidant.
The preparation method comprises the following steps:
(1) the recycled polypropylene resin, the plant fiber, the filler, the 1, 2-ethylene silicon oxide spiral nano tube, the compatilizer and the antioxidant are weighed according to the formula and are uniformly mixed.
(2) Introducing the mixture into a double-screw extruder for melting and extruding; the temperature at the time of melting was: 185 ℃ in the first zone, 205 ℃ in the second zone, 205 ℃ in the third zone, 215 ℃ in the fourth zone, 215 ℃ in the fifth zone, 215 ℃ in the sixth zone, 220 ℃ in the seventh zone, 225 ℃ in the eighth zone, 225 ℃ in the ninth zone and 225 ℃ in the tenth zone; the twin screw speed was 300 rpm.
(3) Cooling the extruded blank by circulating water at 5-25 ℃; and granulating to obtain the recycled automotive polypropylene material.
Comparative example 2
This comparative example differs from example 1 in that: in the raw material composition, plant fibers and benzoyl oxide are mutually independent; the preparation method does not comprise the step (1).
The concrete raw materials comprise: 100 parts by mass of recycled polypropylene resin, 15 parts by mass of plant fiber, 1 part by mass of benzoyl oxide, 20 parts by mass of filler, 8 parts by mass of 1, 2-ethylene silicon oxide spiral nanotube, 2 parts by mass of allyl trimethoxy silane, 1 part by mass of dibutyltin octanoate, 2 parts by mass of compatilizer and 1 part by mass of antioxidant.
The preparation method comprises the following steps:
(1) the recycled polypropylene resin, the plant fiber, the benzoyl oxide, the filler, the 1, 2-ethylene silicon oxide spiral nano tube, the allyl trimethoxy silane, the compatilizer and the antioxidant are weighed according to the formula and are uniformly mixed.
(2) Introducing the mixture into a double-screw extruder for melting and extruding; the temperature at the time of melting was: 185 ℃ in the first zone, 205 ℃ in the second zone, 205 ℃ in the third zone, 215 ℃ in the fourth zone, 215 ℃ in the fifth zone, 215 ℃ in the sixth zone, 220 ℃ in the seventh zone, 225 ℃ in the eighth zone, 225 ℃ in the ninth zone and 225 ℃ in the tenth zone; the rotating speed of the double screws is 300 rpm; simultaneously, dibutyltin octoate is weighed according to the formula and added from six zones of an extruder.
(3) Cooling the extruded blank by circulating water at 5-25 ℃; and granulating to obtain the recycled automotive polypropylene material.
And (3) performance testing:
the polypropylene materials provided in examples 1-3 and comparative examples 1-2 were injection molded on an injection molding machine and tested for properties.
And (3) testing tensile strength: reference standard: ISO 527-2; and (3) testing conditions are as follows: the clamping distance is 50mm, and the speed is 50 mm/min.
And (3) testing the bending strength: reference standard: ISO 178; and (3) testing conditions are as follows: span 64mm, speed 14 mm/min.
Flexural modulus test: reference standard: ISO 178; and (3) testing conditions are as follows: span 64mm, speed 2 mm/min.
Unnotched impact strength test: reference standard: ISO 179; and (3) testing conditions are as follows: the span is 62 mm.
Notched impact strength test: reference standard: ISO 179; and (3) testing conditions are as follows: span 62mm, notch depth 1/3D.
The detection results are as follows:
example 1:
tensile strength: 62MPa, bending strength: 75Mpa, flexural modulus: 3500MPa, unnotched impact strength: 32 J.m-2Notched impact strength: 8KJ · m-2。
Example 2:
tensile strength: 60MPa, bending strength: 72MPa, flexural modulus: 3200MPa, unnotched impact strength: 31 J.m-2Notched impact strength: 8KJ · m-2。
Example 3:
tensile strength: 63Mpa, bending strength: 78MPa, flexural modulus: 3500MPa, unnotched impact strength: 30 J.m-2Notched impact strength: 7KJ · m-2。
Comparative example 1:
tensile strength: 48MPa, bending strength: 62MPa, flexural modulus: 2800MPa, unnotched impact strength: 25 J.m-2Notched impact strength: 5KJ · m-2。
Comparative example 2:
tensile strength: 58MPa, bending strength: 72MPa, flexural modulus: 3300MPa, unnotched impact strength: 30 J.m-2Notched impact strength: 7KJ · m-2。
According to the detection result, the following can be found:
(1) the mechanical properties of the polypropylene material obtained in comparative example 1 were inferior to those of the samples provided in examples 1 to 3. The molecular chain of the polypropylene resin is crosslinked under the action of benzoyl peroxide, allyl trimethoxy silane and dibutyltin octanoate to form a net structure, so that the mechanical property of the injection molding finished product is improved.
(2) The mechanical property of the sample injection molded by the polypropylene material obtained in the comparative example 2 is poorer than that of the sample injection molded in the example 1, because the benzoyl peroxide is attached to the surface of the plant fiber in the example 1, the grafting reaction of the polypropylene resin and the allyltrimethoxysilane occurs near the plant fiber, so that the network structure of the polypropylene is formed around the plant fiber to a higher degree, the plant fiber can be better fused in the polypropylene base material, the function of the plant fiber is better exerted, and the mechanical property of the injection molded product is improved.
In light of the foregoing description of the preferred embodiment of the present invention, it is to be understood that various changes and modifications may be made by one skilled in the art without departing from the spirit and scope of the invention. The technical scope of the present invention is not limited to the content of the specification, and must be determined according to the scope of the claims.
Claims (10)
1. A recycled polypropylene material for vehicles is characterized in that: the preparation raw materials comprise recycled polypropylene resin, plant fiber, silicon oxide spiral nano-tube, silane cross-linking agent and cross-linking catalyst; the plant fiber is loaded with a peroxide initiator.
2. The recycled vehicular polypropylene material of claim 1, wherein: the silane cross-linking agent is allyl trimethoxy silane; the crosslinking catalyst is dibutyltin octoate; the peroxide initiator is benzoyl peroxide.
3. The recycled vehicular polypropylene material of claim 2, wherein: the silicon oxide spiral nanotube is a 1, 2-ethylene silicon oxide spiral nanotube.
4. The recycled vehicular polypropylene material of claim 3, wherein: also comprises filler, compatilizer and antioxidant.
5. The recycled vehicular polypropylene material of claim 4, wherein: the preparation raw materials comprise 100 parts by mass of recycled polypropylene resin, 12-24 parts by mass of plant fiber loaded with benzoyl peroxide, 15-25 parts by mass of filler, 6-12 parts by mass of 1, 2-ethylene silicon oxide spiral nanotube, 1-3 parts by mass of allyl trimethoxy silane, 0.2-1 part by mass of dibutyltin octanoate, 1-3 parts by mass of compatilizer and 0.5-1.5 parts by mass of antioxidant.
6. A method for preparing the recycled vehicular polypropylene material as claimed in any one of claims 1 to 5, wherein: the method comprises the following steps:
firstly, dissolving a peroxide initiator in a solvent, and then soaking plant fibers in the solvent; after the plant fiber is taken out, heating to remove the solvent; controlling the weight of the treated plant fiber to be increased by 4-10%;
weighing raw materials except for the crosslinking catalyst and mixing;
introducing the mixture into an extruder for melting and extruding; weighing a crosslinking catalyst and adding the crosslinking catalyst into the middle section of the extruder;
and cooling the extruded blank to obtain a finished product.
7. The method for producing a recycled vehicular polypropylene material according to claim 6, wherein: the solvent is chloroform.
8. The method for producing a recycled vehicular polypropylene material according to claim 6, wherein: the extruder is a double-screw extruder and comprises ten work areas; the crosslinking catalyst is added from six zones of the extruder.
9. The method for producing a recycled vehicular polypropylene material according to claim 8, wherein: the temperature of each work area of the extruder is not lower than 180 ℃, and the rotating speed of the twin screw is 250-300 rpm.
10. The method for producing a recycled vehicular polypropylene material according to claim 9, wherein: the blank is cooled by circulating water at 5-25 ℃.
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