CN111961245A - Preparation method of lightweight polypropylene foam material - Google Patents
Preparation method of lightweight polypropylene foam material Download PDFInfo
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- CN111961245A CN111961245A CN202010849558.2A CN202010849558A CN111961245A CN 111961245 A CN111961245 A CN 111961245A CN 202010849558 A CN202010849558 A CN 202010849558A CN 111961245 A CN111961245 A CN 111961245A
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- 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
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- 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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- C08K9/10—Encapsulated ingredients
Abstract
The invention relates to a preparation method of a lightweight polypropylene foam material, which comprises the following steps: preparing a composite foaming agent from sodium bicarbonate, citric acid and microcapsule xylitol; preparing polypropylene composite master batches from polypropylene resin, mica micro-sheets and an auxiliary agent; and mixing the composite foaming agent, the polypropylene composite master batch and dicumyl peroxide to obtain a finished product. The mica microchip is introduced in the preparation process of the polypropylene composite master batch; the material has a larger comparative area, so that more points for bubble nucleation are arranged on the interface of the polypropylene and the mica microchip, and the foaming is facilitated; meanwhile, the mica micro-sheets are arranged in the polypropylene base material in a layer-by-layer staggered and superposed manner, so that the mechanical property of the base material can be improved, the foaming effect is improved, and apparent flaws caused by gas overflow are reduced.
Description
Technical Field
The invention relates to the field of polypropylene materials, in particular to a preparation method of a lightweight polypropylene foam material.
Background
The polypropylene material is a material with high cost performance; therefore, the application of plastic parts to automobiles has been continuously expanded, and the plastic parts are widely applied to main plastic parts of automobiles such as bumpers, automobile instrument panels, door panels, center tunnels, pillars, and luggage cases.
The foamed polypropylene material features that polypropylene material is used as base material, and the middle layer of the material has dense closed micropores of ten-to-tens microns and dense skin structures on two sides. In recent years, foamed polypropylene materials have attracted more and more attention because of pursuit of lightweight, efficient, and low-cost production. However, the foaming effect of the current foamed polypropylene material needs to be improved.
Disclosure of Invention
The invention overcomes the defects of the prior art and provides the preparation method of the polypropylene foaming material with good foaming effect.
In order to achieve the purpose, the invention adopts the technical scheme that: the preparation method of the lightweight polypropylene foam material is characterized by comprising the following steps: the method comprises the following steps:
mixing and granulating sodium bicarbonate, citric acid and microcapsule xylitol; immersing the obtained particles into silicone oil, and carrying out ultrasonic treatment and stirring; then, carrying out post-treatment to obtain the composite foaming agent coated by the organic silicon;
weighing polypropylene resin, mica micro-sheets and an auxiliary agent; then mixing; melting and extruding the mixture to obtain polypropylene composite master batch;
weighing the propylene composite master batch, the composite foaming agent and dicumyl peroxide, and mixing to obtain a finished product.
Preferably, water is sprayed during the granulation.
As a more preferable scheme, 12-21 parts by mass of sodium bicarbonate, 28-42 parts by mass of citric acid and 4-8 parts by mass of microcapsule xylitol are mixed and added into a granulator, and then 15-30 parts by mass of water is sprayed into the granulator for granulation.
As a preferable scheme, the particles are immersed in silicone oil, and are subjected to ultrasonic treatment and stirred for 5-10 min; and then carrying out vacuum filtration and vacuum drying to obtain the composite foaming agent coated by the organic silicon.
As a preferred scheme, talcum powder, styrene thermoplastic elastomer, polypropylene resin, mica micro-sheets and an auxiliary agent are weighed and mixed.
More preferably, the auxiliary agent includes a compatibilizer, an antistatic agent, and an antioxidant.
As a more preferable scheme, 100 parts by mass of polypropylene resin, 10-20 parts by mass of mica micro-flake, 10-20 parts by mass of talcum powder, 2-12 parts by mass of styrene thermoplastic elastomer, 2-8 parts by mass of compatilizer, 0.5-2 parts by mass of antistatic agent and 0.5-1.5 parts by mass of antioxidant are weighed; and then dry-mixed for 1-3 h.
As a preferable scheme, the mixture is sent into a double-screw extruder to be melted, extruded, cooled and granulated to obtain the polypropylene composite master batch.
As a more preferable scheme, the temperature of each zone of the double-screw extruder is 185-230 ℃; the residence time of the mixture in the twin-screw extruder is 6-10 min.
As a more preferable scheme, the blank extruded by the double-screw extruder is cooled by circulating water at the temperature of 5-10 ℃.
The invention has the beneficial technical effects that: provides a preparation method of a polypropylene foaming material with good foaming effect. The mica microchip is introduced in the preparation process of the polypropylene composite master batch; the material has a larger comparative area, so that more points for bubble nucleation are arranged on the interface of the polypropylene and the mica microchip, and the foaming is facilitated; meanwhile, the mica micro-sheets are arranged in the polypropylene base material in a layer-by-layer staggered and superposed manner, so that the mechanical property of the base material can be improved, the foaming effect is improved, and apparent flaws caused by gas overflow are reduced.
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 preparation method of a lightweight polypropylene foam material comprises the following steps:
(1) mixing 15 parts by mass of sodium bicarbonate, 35 parts by mass of citric acid and 5 parts by mass of microcapsule xylitol, adding into a granulator, spraying 15 parts by mass of water into the granulator, and granulating; immersing the obtained particles into 100 parts by mass of silicone oil, and carrying out ultrasonic treatment and stirring for 5 min; and then carrying out vacuum filtration and vacuum drying to obtain the composite foaming agent coated by the organic silicon.
The step can better mix the phase-change material and the foaming agent together, and the compatibility of the composite foaming agent and the polypropylene material is better after coating.
(2) Weighing 100 parts by mass of polypropylene resin, 16 parts by mass of mica microchip, 15 parts by mass of talcum powder, 5 parts by mass of styrene thermoplastic elastomer, 5 parts by mass of compatilizer, 1 part by mass of antistatic agent and 1.5 parts by mass of antioxidant; after which it was dry blended for 1 h.
Wherein: the flow rate of the polypropylene resin under a 2.16kg load at a temperature of 230 ℃ is 30-40 g/min.
The mica micro-sheet is in a sheet structure in a microscopic state, the length of the sheet diameter is 80-100 mu m, and the thickness of the sheet layer is 2-3 mu m; the material has good compatibility with a polypropylene base material, can be well distributed in the polypropylene base material after being mixed, and has good associativity; the mica microchip has a larger comparative area, so that more points for bubble nucleation are arranged on the interface of the polypropylene and the mica microchip, and the foaming is facilitated; meanwhile, the mica micro-sheets form a layer-by-layer staggered and superposed arrangement state in the polypropylene base material, so that the mechanical property of the base material can be improved, the path for gas to migrate from the base material to the outside is increased, the migration difficulty is increased, and the overflow of foaming gas is reduced; thereby improving the foaming effect and reducing the apparent flaws caused by gas overflow.
The particle size of the talcum powder is coated by epoxy resin, and is 15-25 mu m; the styrene thermoplastic elastomer is SBS (styrene-butadiene-styrene block copolymer, total styrene content is 30-45 wt%), so as to improve the fluidity of the polypropylene composite material; the compatilizer is maleic anhydride grafted polypropylene (PP-g-MAH); the antistatic agent is a compound antistatic agent formed by compounding alkyl benzene sulfonate and siloxane; the antioxidant is hindered phenol antioxidant.
(3) And (3) feeding the mixture obtained in the step (2) into a double-screw extruder for melting, extruding, cooling and granulating to obtain the polypropylene composite master batch.
Wherein: the first zone temperature of the double-screw extruder is 180 ℃, the second zone temperature is 190 ℃, the third zone temperature is 195 ℃, the fourth zone temperature is 195 ℃, the fifth zone temperature is 200 ℃, the sixth zone temperature is 205 ℃, the seventh zone temperature is 210 ℃, the eighth zone temperature is 215 ℃, the ninth zone temperature is 215 ℃ and the tenth zone temperature is 220 ℃; the retention time of the mixed raw materials in a double-screw extruder is 10 min; the pressure was 12 MPa.
And cooling the extruded blank by circulating water at 5-10 ℃.
(4) Weighing the propylene composite master batch, the composite foaming agent and dicumyl peroxide according to the mass ratio: 100:3.5: 2, uniformly mixing to obtain a finished product.
Example 2
A preparation method of a lightweight polypropylene foam material comprises the following steps:
(1) mixing and adding 12 parts by mass of sodium bicarbonate, 28 parts by mass of citric acid and 8 parts by mass of microcapsule xylitol into a granulator, and then spraying 24 parts by mass of water into the granulator for granulation; immersing the obtained particles into 100 parts by mass of silicone oil, and carrying out ultrasonic treatment and stirring for 5 min; and then carrying out vacuum filtration and vacuum drying to obtain the composite foaming agent coated by the organic silicon.
(2) Weighing 100 parts by mass of polypropylene resin, 20 parts by mass of mica microchip, 10 parts by mass of talcum powder, 12 parts by mass of styrene thermoplastic elastomer, 8 parts by mass of compatilizer, 0.5 part by mass of antistatic agent and 1 part by mass of antioxidant; after which it was dry blended for 2 h.
(3) And (3) feeding the mixture obtained in the step (2) into a double-screw extruder for melting, extruding, cooling and granulating to obtain the polypropylene composite master batch.
Wherein: the first zone temperature of the double-screw extruder is 185 ℃, the second zone temperature is 195 ℃, the third zone temperature is 200 ℃, the fourth zone temperature is 200 ℃, the fifth zone temperature is 205 ℃, the sixth zone temperature is 210 ℃, the seventh zone temperature is 215 ℃, the eighth zone temperature is 220 ℃, the ninth zone temperature is 220 ℃ and the tenth zone temperature is 225 ℃; the retention time of the mixed raw materials in the double-screw extruder is 8 min; the pressure was 15 MPa.
The extruded billet was cooled with 5 ℃ circulating water.
(4) Weighing the propylene composite master batch, the composite foaming agent and dicumyl peroxide according to the mass ratio: 100:2: 2, uniformly mixing to obtain a finished product.
Example 3
A preparation method of a lightweight polypropylene foam material comprises the following steps:
(1) mixing and adding 21 parts by mass of sodium bicarbonate, 42 parts by mass of citric acid and 4 parts by mass of microcapsule xylitol into a granulator, and then spraying 30 parts by mass of water into the granulator for granulation; immersing the obtained particles into 100 parts by mass of silicone oil, and carrying out ultrasonic treatment and stirring for 10 min; and then carrying out vacuum filtration and vacuum drying to obtain the composite foaming agent coated by the organic silicon.
(2) Weighing 100 parts by mass of polypropylene resin, 10 parts by mass of mica microchip, 20 parts by mass of talcum powder, 2 parts by mass of styrene thermoplastic elastomer, 2 parts by mass of compatilizer, 2 parts by mass of antistatic agent and 0.5 part by mass of antioxidant; after which it was dry blended for 3 h.
(3) And (3) feeding the mixture obtained in the step (2) into a double-screw extruder for melting, extruding, cooling and granulating to obtain the polypropylene composite master batch.
Wherein: the first zone temperature of the double-screw extruder is 190 ℃, the second zone temperature is 195 ℃, the third zone temperature is 200 ℃, the fourth zone temperature is 205 ℃, the fifth zone temperature is 210 ℃, the sixth zone temperature is 215 ℃, the seventh zone temperature is 220 ℃, the eighth zone temperature is 225 ℃, the ninth zone temperature is 225 ℃ and the tenth zone temperature is 230 ℃; the retention time of the mixed raw materials in the double-screw extruder is 6 min; the pressure was 18 MPa.
And cooling the extruded blank by using circulating water at 10 ℃.
(4) Weighing the propylene composite master batch, the composite foaming agent and dicumyl peroxide according to the mass ratio: 100:4.5: 2, uniformly mixing to obtain a finished product.
Comparative example 1
This comparative example differs from example 1 in that: mica micro-sheets are not contained in the step (2).
The method specifically comprises the following steps:
a preparation method of a lightweight polypropylene foam material comprises the following steps:
(1) mixing 15 parts by mass of sodium bicarbonate, 35 parts by mass of citric acid and 5 parts by mass of microcapsule xylitol, adding into a granulator, spraying 15 parts by mass of water into the granulator, and granulating; immersing the obtained particles into 100 parts by mass of silicone oil, and carrying out ultrasonic treatment and stirring for 5 min; and then carrying out vacuum filtration and vacuum drying to obtain the composite foaming agent coated by the organic silicon.
(2) Weighing 100 parts by mass of polypropylene resin, 15 parts by mass of talcum powder, 5 parts by mass of styrene thermoplastic elastomer, 5 parts by mass of compatilizer, 1 part by mass of antistatic agent and 1.5 parts by mass of antioxidant; after which it was dry blended for 1 h.
(3) And (3) feeding the mixture obtained in the step (2) into a double-screw extruder for melting, extruding, cooling and granulating to obtain the polypropylene composite master batch.
Wherein: the first zone temperature of the double-screw extruder is 180 ℃, the second zone temperature is 190 ℃, the third zone temperature is 195 ℃, the fourth zone temperature is 195 ℃, the fifth zone temperature is 200 ℃, the sixth zone temperature is 205 ℃, the seventh zone temperature is 210 ℃, the eighth zone temperature is 215 ℃, the ninth zone temperature is 215 ℃ and the tenth zone temperature is 220 ℃; the retention time of the mixed raw materials in a double-screw extruder is 10 min; the pressure was 12 MPa.
And cooling the extruded blank by circulating water at 5-10 ℃.
(4) Weighing the propylene composite master batch, the composite foaming agent and dicumyl peroxide according to the mass ratio: 100:3.5: 2, uniformly mixing to obtain a finished product.
And (3) performance testing:
the polypropylene composites provided in examples 1-3 and comparative example 1 were injection molded on an injection molding machine to prepare samples 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.
And (3) testing the density: reference standard: ISO 1183; and (3) testing conditions are as follows: and (5) normal temperature.
The detection results are as follows:
example 1:
tensile strength: 20Mpa, flexural strength: 29Mpa, flexural modulus: 1650MPa, impact strength: (continuous), notched impact strength: 18 KJ · m-2Density: 0.85 g/cm-3Appearance: the surface of the part has no air mark and no pore flaw, and is microscopic: the middle of the part is observed by a scanning electron microscope to have uniform closed micropores of 3-10 microns.
Example 2:
tensile strength: 22Mpa, flexural strength: 28Mpa, flexural modulus: 1650MPa, impact strength: (continuous), notched impact strength: 19KJ · m-2Density:0.81g·cm-3appearance: the surface of the part has no air mark and no pore flaw, and is microscopic: the middle of the part is observed by a scanning electron microscope to have uniform closed micropores of 3-10 microns.
Example 3:
tensile strength: 18Mpa, flexural strength: 26Mpa, flexural modulus: 1550Mpa, impact strength: (continuous), notched impact strength: 16KJ · m-2Density: 0.90 g.cm-3Appearance: the surface of the part has no air mark and no pore flaw, and is microscopic: the middle of the part is observed by a scanning electron microscope to have uniform closed micropores of 3-10 microns.
Comparative example 1:
tensile strength: 17Mpa, flexural strength: 26Mpa, flexural modulus: 1550Mpa, impact strength: (continuous), notched impact strength: 14KJ · m-2Density: 1.02 g.cm-3Appearance: the surface of the part has no air mark but has hole flaws, and the microscopic: the distribution is poorer than that of the embodiment when the closed micropores between 20 and 40 microns are observed in the part through a scanning electron microscope.
According to the detection result, the following can be found:
(1) after the polypropylene materials obtained in the examples 1-3 are subjected to injection molding foaming, the obtained samples have closed micropores with the particle size of less than 10 micrometers and uniform distribution; the micropore particle size inside the sample of comparative example 1 is larger and slightly poor in distribution; the mica microchip has larger comparative area, so that more points for bubble nucleation are arranged on the interface of the polypropylene and the mica microchip, and the foaming is facilitated; meanwhile, the mica micro-sheets are arranged in the polypropylene base material in a layer-by-layer staggered and superposed manner, so that the path for gas to migrate from the base material to the outside is increased, the migration difficulty is increased, the overflow of foaming gas is reduced, and the foaming effect is improved.
(2) The mechanical properties of the injection-molded finished products of the polypropylene materials obtained in examples 1-3 are better than those of comparative example 1; the arrangement state of the mica micro-sheets formed in the polypropylene base material in a layer-by-layer staggered and superposed manner is shown, and the mechanical properties of the polypropylene composite material and the injection molding finished product thereof can be 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 preparation method of a lightweight polypropylene foam material is characterized by comprising the following steps: the method comprises the following steps:
mixing and granulating sodium bicarbonate, citric acid and microcapsule xylitol; immersing the obtained particles into silicone oil, and carrying out ultrasonic treatment and stirring; then, carrying out post-treatment to obtain the composite foaming agent coated by the organic silicon;
weighing polypropylene resin, mica micro-sheets and an auxiliary agent; then mixing; melting and extruding the mixture to obtain polypropylene composite master batch;
weighing the propylene composite master batch, the composite foaming agent and dicumyl peroxide, and mixing to obtain a finished product.
2. The method for preparing a lightweight polypropylene foam according to claim 1, wherein: and water is sprayed during granulation.
3. The method for preparing a lightweight polypropylene foam material according to claim 2, wherein: mixing and adding 12-21 parts by mass of sodium bicarbonate, 28-42 parts by mass of citric acid and 4-8 parts by mass of microcapsule xylitol into a granulator, and then spraying 15-30 parts by mass of water into the granulator for granulation.
4. The method for preparing a lightweight polypropylene foam according to claim 1, wherein: immersing the particles into silicone oil, performing ultrasonic treatment and stirring for 5-10 min; and then carrying out vacuum filtration and vacuum drying to obtain the composite foaming agent coated by the organic silicon.
5. The method for preparing a lightweight polypropylene foam according to claim 1, wherein: and mixing talcum powder, styrene thermoplastic elastomer, polypropylene resin, mica micro-sheets and assistant.
6. The method for producing a lightweight polypropylene foam material according to claim 5, wherein: the auxiliary agent comprises a compatilizer, an antistatic agent and an antioxidant.
7. The method for producing a lightweight polypropylene foam material according to claim 6, wherein: weighing 100 parts by mass of polypropylene resin, 10-20 parts by mass of mica microchip, 10-20 parts by mass of talcum powder, 2-12 parts by mass of styrene thermoplastic elastomer, 2-8 parts by mass of compatilizer, 0.5-2 parts by mass of antistatic agent and 0.5-1.5 parts by mass of antioxidant; and then dry-mixed for 1-3 h.
8. The method for preparing a lightweight polypropylene foam according to claim 1, wherein: and feeding the mixture into a double-screw extruder for melting, extruding, cooling and granulating to obtain the polypropylene composite master batch.
9. The method for producing a lightweight polypropylene foam material according to claim 8, wherein: the temperature of each area of the double-screw extruder is 185-230 ℃; the residence time of the mixture in the twin-screw extruder is 6-10 min.
10. The method for producing a lightweight polypropylene foam material according to claim 9, wherein: and the blank extruded by the double-screw extruder is cooled by circulating water at the temperature of 5-10 ℃.
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