CN110128741B - Polyolefin foam material and preparation method thereof - Google Patents

Polyolefin foam material and preparation method thereof Download PDF

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CN110128741B
CN110128741B CN201810134382.5A CN201810134382A CN110128741B CN 110128741 B CN110128741 B CN 110128741B CN 201810134382 A CN201810134382 A CN 201810134382A CN 110128741 B CN110128741 B CN 110128741B
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stage screw
polyolefin foam
parts
weight
temperature
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CN110128741A (en
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庞永艳
郑文革
黄朋科
刘伟
吴明辉
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Ningbo Institute of Material Technology and Engineering of CAS
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Ningbo Institute of Material Technology and Engineering of CAS
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Abstract

The invention relates to a polyolefin foam material and a preparation method thereofThe preparation method comprises the following steps: (a) weighing 60-90 parts by weight of polyolefin, 10-40 parts by weight of intumescent flame retardant and 0-5 parts by weight of synergist, mixing, adding into an extruder, and performing melt extrusion to obtain a premix; (b) adding the premix into a single-screw extruder, and extruding and foaming to obtain a polyolefin foam material; the single-screw extruder comprises an upper-stage screw and a lower-stage screw which are connected in series, the temperature of the upper-stage screw is 130-230 ℃, the temperature of the lower-stage screw is 80-180 ℃, the temperature of an extrusion die is 80-180 ℃, and supercritical carbon dioxide is injected at 1/5-1/3 of the upper-stage screw. The resulting polyolefin foam had a cell density of 104cell/cm3～1014cell/cm3The expansion ratio is 1.25 to 30. The preparation method improves the dispersion effect of the flame retardant, and the obtained polyolefin foam material has the advantages of uniform cell structure, high foaming rate, controllable orientation degree, excellent flame retardant property and excellent mechanical property.

Description

Polyolefin foam material and preparation method thereof
Technical Field
The invention relates to the technical field of preparation of high polymer materials, in particular to a polyolefin foam material and a preparation method thereof.
Background
Polyolefin foam materials are composed only of carbon and hydrogen elements, are extremely combustible, and are more combustible than unfoamed polyolefin materials, so that flame retardant treatment of the foamed polyolefin materials is particularly important.
Compared with flame-retardant foaming materials such as polyurethane, polystyrene, melamine and the like, the flame-retardant treatment of the polyolefin foaming material is relatively late to start, and the defects of low foaming ratio, poor flame retardant dispersion effect, uneven cellular structure of the foaming material, poor mechanical property, low production phase ratio and the like exist, the technical difficulty is high, and related core technologies are rarely reported at home and abroad at present.
Disclosure of Invention
Therefore, it is necessary to provide a polyolefin foam material and a preparation method thereof, wherein the preparation method is simple to operate and high in production efficiency, and the prepared polyolefin foam material is uniform in cell structure, high in foaming rate, good in flame retardant effect and excellent in mechanical property.
A preparation method of a polyolefin foam material comprises the following steps:
(a) weighing 60-90 parts by weight of polyolefin, 10-40 parts by weight of intumescent flame retardant and 0-5 parts by weight of synergist, mixing, adding into an extruder, and performing melt extrusion to obtain a premix;
(b) adding the premix into a single-screw extruder, and extruding and foaming to obtain a polyolefin foam material; the single-screw extruder comprises an upper-stage screw and a lower-stage screw which are connected in series, the temperature of the upper-stage screw is 130-230 ℃, the temperature of the lower-stage screw is 80-180 ℃, the temperature of an extrusion die is 80-180 ℃, and supercritical carbon dioxide is injected into 1/5-1/3 parts of the upper-stage screw.
The preparation method of the polyolefin foam material has the following advantages:
firstly, the preparation method integrates processing and foaming, can continuously and efficiently prepare the foaming material and meet the increasing requirements of the polyolefin foaming material. And the single-screw extruder comprises an upper-stage screw and a lower-stage screw which are connected in series, the upper-stage screw mainly plays a role in plasticizing and melting the polymer and primarily mixing the polymer melt and the supercritical carbon dioxide, and the lower-stage screw mainly plays a role in fully mixing the polymer melt and the supercritical carbon dioxide and facilitating the foaming of the polymer in an extrusion die through temperature control. And thirdly, the supercritical carbon dioxide is used as a foaming agent, so that the foaming agent is green and environment-friendly, has low price, and has strong plasticizing capacity and diffusion capacity. The plasticizing and mass transfer effects of the supercritical carbon dioxide can improve the dispersion of the intumescent flame retardant, and further improve the cellular structure of the foaming material. Therefore, the preparation method effectively solves the problems that the intumescent flame retardant is easy to agglomerate and is difficult to process when the addition amount is large, improves the dispersion effect of the intumescent flame retardant, and improves the flame retardant efficiency of the intumescent flame retardant.
The invention also provides aThe polyolefin foam material prepared by the preparation method has the cell density of 104cell/cm3～1014cell/cm3The expansion ratio is 1.25 to 30.
The polyolefin foam material prepared by the preparation method has controllable density, uniform cell structure and high foaming multiplying power, and finally can obtain excellent flame retardant property and mechanical property.
Drawings
FIG. 1 is a scanning electron micrograph of a cell structure of a polyolefin foam prepared in example 1 of the present invention;
FIG. 2 is a photograph showing mechanical properties of the polyolefin foam prepared in example 1 of the present invention.
Detailed Description
The polyolefin foam material and the preparation method thereof provided by the present invention will be further explained below.
The invention provides a preparation method of a polyolefin foam material, which comprises the following steps:
(a) weighing 60-90 parts by weight of polyolefin, 10-40 parts by weight of intumescent flame retardant and 0-5 parts by weight of synergist, mixing, adding into an extruder, and performing melt extrusion to obtain a premix;
(b) adding the premix into a single-screw extruder, and extruding and foaming to obtain a polyolefin foam material; the single-screw extruder comprises an upper-stage screw and a lower-stage screw which are connected in series, the temperature of the upper-stage screw is 130-230 ℃, the temperature of the lower-stage screw is 80-180 ℃, the temperature of an extrusion die is 80-180 ℃, and supercritical carbon dioxide is injected into 1/5-1/3 parts of the upper-stage screw.
In the step (a), the polyolefin is at least one of polyethylene, polypropylene, ethylene-propylene rubber and ethylene-octene copolymer. The intumescent flame retardant comprises the following components in percentage by mass (2-4): (0-1): (0-1) mixing an acid source, a carbon source and a gas source, wherein the mass ratio is preferably (2-4): (0.01-1): (0.01-1), and more preferably 3:1: 1. The acid source is at least one of ammonium polyphosphate, melamine polyphosphate, cyanuric acid, ammonium dihydrogen phosphate, tricresyl phosphate, alkyl phosphate, phosphonate, hypophosphite and phosphinate, and preferably one or two of ammonium polyphosphate and melamine polyphosphate. The carbon source is at least one of pentaerythritol, dipentaerythritol, tripentaerythritol, phenolic resin, cyclodextrin, starch and sorbitol, and preferably one or two of starch and pentaerythritol. The gas source is at least one of urea, urea-formaldehyde resin, dicyandiamide and melamine, and the melamine is preferred. The synergist is at least one of antimony trioxide, calcium carbonate, magnesium carbonate, silicon dioxide, montmorillonite, trehalite and kaolin. The total mass of the intumescent flame retardant and the synergist accounts for 10-40% of the total mass of the premix.
In the step (a), the extruder is a single-screw extruder or a double-screw extruder, and the temperature of the single-screw extruder or the double-screw extruder is 120-230 ℃. Preferably, the polyolefin, the intumescent flame retardant and the synergist are uniformly mixed by a high-speed mixer, and then added into a single-screw extruder or a double-screw extruder for melt extrusion to obtain a premix.
The dosage of the supercritical carbon dioxide in the step (b) is 0.5-15% of the total mass of the premix. The injection pressure of the supercritical carbon dioxide is 7 MPa-25 MPa.
The pressure of the single-screw extruder in the step (b) is 7MPa to 30 MPa.
The temperature of the lower-stage screw in the step (b) is lower than that of the upper-stage screw, the difference is T, and T is more than or equal to 15 ℃ and less than or equal to 80 ℃.
Because the melt strength is too high to be beneficial to the growth of the foam holes, and the melt strength is too low to be beneficial to the fixation of the foam holes, the single-screw extruder adopted by the invention comprises an upper-stage screw and a lower-stage screw which are connected in series. The upper-stage screw mainly plays a role in plasticizing and melting a polymer and primarily mixing a polymer melt and supercritical carbon dioxide, and the lower-stage screw mainly plays a role in fully mixing the polymer melt and the supercritical carbon dioxide and facilitating foaming of the polymer in an extrusion die through temperature control. The temperature of the lower-stage screw is lower than that of the upper-stage screw, the difference is T, T is more than or equal to 15 ℃ and less than or equal to 80 ℃, so that the supercritical carbon dioxide can be dissolved in the polymer melt to form a uniform system, and a uniform cell structure is formed; meanwhile, the strength of the polymer melt is ensured to be more suitable for foaming, and a better cell structure and a larger expansion ratio are formed. In order to obtain the polyolefin foaming material with more uniform foam cells, preferably, supercritical carbon dioxide is injected at 1/4 of the upper-stage screw, the dosage of the supercritical carbon dioxide is 1-10% of the total mass of the premix, the injection pressure of the supercritical carbon dioxide is 10 MPa-20 MPa, the temperature of the upper-stage screw is 140-200 ℃, the temperature of the lower-stage screw is 100-175 ℃, the difference between the temperature of the lower-stage screw and the temperature of the upper-stage screw is T, T is more than or equal to 20 ℃ and less than or equal to 60 ℃, and the pressure of the single-screw extruder is 8 MPa-18 MPa.
And (c) after the polyolefin foam material is obtained by extrusion foaming in the step (b), a collection step (c) is further included, wherein the polyolefin foam material is collected by traction of a traction device in the step (c), the traction ratio of the traction device is 0-80, and the drawing speed is 0.1-3.0 m/s. The traction device is equipment with a traction function, and comprises but is not limited to casting equipment, calendaring equipment, a granulator and spinning equipment. By adjusting the stretching speed of the traction device, the orientation of the polymer molecular chain can be adjusted, so that the orientation degree of the polyolefin foam material can be adjusted, and the mechanical property of the polyolefin foam material can be improved.
Considering that the strength of the polyolefin foam material is low when the draft ratio is 0, the draft ratio is preferably 1 to 30.
The preparation method of the polyolefin foam material integrates processing and foaming, can continuously and efficiently prepare the foam material, has the advantages of environmental protection, low energy consumption, high production efficiency and the like, and meets the increasing requirements of the polyolefin foam material.
In the processing process of the preparation method, the single-screw extruder comprises an upper-stage screw and a lower-stage screw which are connected in series, the upper-stage screw mainly plays roles in plasticizing and melting the polymer and primarily mixing the polymer melt and the supercritical carbon dioxide, and the lower-stage screw mainly plays roles in fully mixing the polymer melt and the supercritical carbon dioxide and facilitating the foaming of the polymer in an extrusion die through temperature control.
The preparation method adopts supercritical carbon dioxide as a foaming agent, and the foaming agent is green and environment-friendly, has low price, and has strong plasticizing capacity and diffusion capacity. The plasticizing and mass transfer effects of the supercritical carbon dioxide can improve the dispersion of the flame retardant, and further improve the cellular structure of the foaming material.
Therefore, the preparation method effectively solves the problems that the intumescent flame retardant is easy to agglomerate and is difficult to process when the addition amount is large, improves the dispersion effect of the flame retardant, and improves the flame retardant efficiency of the flame retardant.
The invention also provides a polyolefin foam material obtained by the preparation method, and the foam cell density of the polyolefin foam material is 104cell/cm3～1014cell/cm3The expansion ratio is 1.25 to 30.
The polyolefin foam material obtained by the preparation method comprises at least two of polyolefin, intumescent flame retardant and synergist, and the intumescent flame retardant and the synergist are uniformly dispersed in the polyolefin foam material. The obtained polyolefin foam material has controllable density, uniform cell structure, high foaming multiplying power and controllable orientation degree, and can finally obtain excellent flame retardant property and mechanical property. Therefore, the polyolefin foam material can be widely applied to the fields of automobiles, packaging, electronic products, building materials and the like.
Hereinafter, the polyolefin and the preparation method thereof will be further described by the following specific examples.
Example 1:
weighing 85 parts by weight of polypropylene, 12 parts by weight of ammonium polyphosphate, 4 parts by weight of pentaerythritol and 1 part by weight of magnesium carbonate.
The raw materials are mixed by a high-speed mixer and then added into a double-screw extruder, and the mixture is melted and extruded at the temperature of 195 ℃ to obtain a premix.
The premix is added to a single screw extruder comprising an upper stage screw and a lower stage screw in series. Wherein the temperature of the upper-stage screw of the single-screw extruder is 195 ℃, the temperature of the lower-stage screw is 160 ℃, and the temperature of the extrusion die is 158 ℃. At 1/4 of the upper stage screw, 3 parts by weight of supercritical carbon dioxide was injected, and the injection pressure was set to 20 MPa. And (3) maintaining the pressure in the single-screw extruder at 12MPa, extruding and foaming, and stretching by adopting a calendering device to obtain the polypropylene foam material, wherein the stretching speed of the calendering device is 0.8m/s, and the draw ratio is 2.1.
Example 2:
weighing 71 parts by weight of polypropylene, 23 parts by weight of ammonium polyphosphate and 6 parts by weight of pentaerythritol.
The raw materials are mixed by a high-speed mixer and then added into a single-screw extruder, and the mixture is melted and extruded at 200 ℃ to obtain a premix.
The premix is added to a single screw extruder comprising an upper stage screw and a lower stage screw in series. Wherein the temperature of the upper-stage screw of the single-screw extruder is set to be 190 ℃, the temperature of the lower-stage screw is set to be 175 ℃, and the temperature of the extrusion die is 168 ℃. At 1/4 of the upper stage screw, 6 parts by weight of supercritical carbon dioxide was injected, and the injection pressure was set to 15 MPa. And (3) maintaining the pressure in the single-screw extruder at 7.5MPa, extruding and foaming, and stretching by adopting a granulator to obtain the polypropylene foaming master batch, wherein the stretching speed of the granulator is 2.1m/s, and the drafting ratio is 8.
Example 3:
weighing 70 parts by weight of polyethylene, 18 parts by weight of ammonium polyphosphate, 6 parts by weight of pentaerythritol and 5 parts by weight of calcium carbonate.
The raw materials are mixed by a high-speed mixer and then added into a double-screw extruder, and the mixture is melted and extruded at the temperature of 170 ℃ to obtain a premix.
The premix is added to a single screw extruder comprising an upper stage screw and a lower stage screw in series. Wherein the temperature of the upper-stage screw of the single-screw extruder is set to be 190 ℃, the temperature of the lower-stage screw is set to be 145 ℃, and the temperature of the extrusion die is 144 ℃. At 1/4 of the upper stage screw, 5 parts by weight of supercritical carbon dioxide was injected under a pressure of 17 MPa. And (3) maintaining the pressure in the single-screw extruder at 10MPa, extruding and foaming, and stretching by adopting a casting device to obtain the polyethylene foam material, wherein the stretching speed of the casting device is 2.5m/s, and the drafting ratio is 30.
Example 4:
70 parts by weight of ethylene propylene rubber and 30 parts by weight of tricresyl phosphate are weighed.
The raw materials are mixed by a high-speed mixer and then added into a single-screw extruder, and the mixture is melted and extruded at 160 ℃ to obtain a premix.
The premix is added to a single screw extruder comprising an upper stage screw and a lower stage screw in series. Wherein the temperature of the upper-stage screw of the single-screw extruder is set as 140 ℃, the temperature of the lower-stage screw is set as 100 ℃, and the temperature of the extrusion die is set as 90 ℃. At 1/4 of the upper stage screw, 7 parts by weight of supercritical carbon dioxide was injected under a pressure of 17 MPa. And (3) maintaining the pressure in the single-screw extruder at 8MPa, extruding and foaming, and stretching by adopting a calendering device to obtain the ethylene propylene rubber foaming material, wherein the stretching speed of the calendering device is 1.8m/s, and the draft ratio is 20.
Example 5:
60 parts by weight of polypropylene, 5 parts by weight of polyethylene, 25 parts by weight of melamine phosphate, 5 parts by weight of dipentaerythritol and 5 parts by weight of silicon dioxide are weighed.
The raw materials are mixed by a high-speed mixer and then added into a double-screw extruder, and the mixture is melted and extruded at the temperature of 195 ℃ to obtain a premix.
The premix is added to a single screw extruder comprising an upper stage screw and a lower stage screw in series. Wherein the temperature of the upper-stage screw of the single-screw extruder is 195 ℃, the temperature of the lower-stage screw is 150 ℃, and the temperature of the extrusion die is 150 ℃. At 1/4 of the upper stage screw, 4 parts by weight of supercritical carbon dioxide was injected, and the injection pressure was set to 15 MPa. The pressure in the single screw extruder is maintained at 18MPa, the polypropylene/polyethylene composite foaming material is extruded and foamed, and the polypropylene/polyethylene composite foaming material is obtained by adopting a spinning device for stretching, wherein the stretching speed of the spinning device is 3.0m/s, and the drawing ratio is 80.
Example 6:
80 parts by weight of polypropylene, 16 parts by weight of melamine phosphate and 4 parts by weight of dipentaerythritol are weighed out.
The raw materials are mixed by a high-speed mixer and then added into a single-screw extruder, and the mixture is melted and extruded at 180 ℃ to obtain a premix.
The premix is added to a single screw extruder comprising an upper stage screw and a lower stage screw in series. Wherein the temperature of the upper-stage screw of the single-screw extruder is set to be 200 ℃, the temperature of the lower-stage screw is set to be 180 ℃, and the temperature of the extrusion die is 178 ℃.2 parts by weight of supercritical carbon dioxide was injected into 1/4 of the upper-stage screw at an injection pressure of 15 MPa. And (3) maintaining the pressure in the single-screw extruder at 20MPa, extruding and foaming, and stretching by adopting a spinning device to obtain the polypropylene foam material, wherein the stretching speed of the spinning device is 0.5m/s, and the draw ratio is 1.2.
Example 7:
weighing 67 parts by weight of polypropylene, 10 parts by weight of polyethylene, 12 parts by weight of ammonium polyphosphate, 3 parts by weight of dipentaerythritol, 3 parts by weight of urea and 5 parts by weight of silicon dioxide.
The raw materials are mixed by a high-speed mixer and then added into a double-screw extruder, and the mixture is melted and extruded at the temperature of 195 ℃ to obtain a premix.
The premix is added to a single screw extruder comprising an upper stage screw and a lower stage screw in series. Wherein the temperature of the upper-stage screw of the single-screw extruder is 195 ℃, the temperature of the lower-stage screw is 160 ℃, and the temperature of the extrusion die is 154 ℃. At 1/4 of the upper stage screw, 9 parts by weight of supercritical carbon dioxide was injected under an injection pressure of 18 MPa. And (3) maintaining the pressure in the single-screw extruder at 30MPa, extruding and foaming, and stretching by adopting a spinning device to obtain the polypropylene/polyethylene composite foamed material, wherein the stretching speed of the spinning device is 1.9m/s, and the drafting ratio is 15.
Example 8:
70 parts by weight of polypropylene and 30 parts by weight of ammonium polyphosphate are weighed.
The raw materials are mixed by a high-speed mixer and then added into a single-screw extruder, and the mixture is melted and extruded at 210 ℃ to obtain a premix.
The premix is added to a single screw extruder comprising an upper stage screw and a lower stage screw in series. Wherein the temperature of the upper-stage screw of the single-screw extruder is set to be 220 ℃, the temperature of the lower-stage screw is set to be 160 ℃, and the temperature of the extrusion die is 160 ℃.8 parts by weight of supercritical carbon dioxide was injected into 1/4 of the upper-stage screw at an injection pressure of 11 MPa. And (3) maintaining the pressure in the single-screw extruder at 13MPa, extruding and foaming, and stretching by adopting a casting device to obtain the polypropylene foam material, wherein the stretching speed of the casting device is 0.8m/s, and the draft ratio is 10.
Example 9:
weighing 85 parts by weight of ethylene propylene rubber, 10 parts by weight of ammonium polyphosphate, 4 parts by weight of phenolic resin and 1 part by weight of montmorillonite.
The raw materials are mixed by a high-speed mixer and then added into a double-screw extruder, and the mixture is melted and extruded at the temperature of 195 ℃ to obtain a premix.
The premix is added to a single screw extruder comprising an upper stage screw and a lower stage screw in series. Wherein the temperature of the upper-stage screw of the single-screw extruder is set to be 130 ℃, the temperature of the lower-stage screw is set to be 80 ℃, and the temperature of the extrusion die is 80 ℃. At 1/4 on the upper stage screw, 15 parts by weight of supercritical carbon dioxide was injected under a pressure of 25 MPa. And (3) maintaining the pressure in the single-screw extruder at 12MPa, extruding and foaming, and stretching by adopting a casting device to obtain the ethylene propylene rubber foaming material, wherein the stretching speed of the casting device is 1.8m/s, and the draft ratio is 35.
Example 10:
weighing 82 parts by weight of polypropylene, 8 parts by weight of ammonium polyphosphate, 4 parts by weight of pentaerythritol, 4 parts by weight of melamine and 2 parts by weight of antimony trioxide.
The raw materials are mixed by a high-speed mixer and then added into a double-screw extruder, and the mixture is melted and extruded at the temperature of 195 ℃ to obtain a premix.
The premix is added to a single screw extruder comprising an upper stage screw and a lower stage screw in series. Wherein the temperature of the upper-stage screw of the single-screw extruder is 195 ℃, the temperature of the lower-stage screw is 180 ℃, and the temperature of the extrusion die is 180 ℃. At 1/4 of the upper stage screw, 0.5 part by weight of supercritical carbon dioxide was injected at an injection pressure of 7 MPa. And (3) maintaining the pressure in the single-screw extruder at 7MPa, extruding and foaming, and stretching by adopting a casting device to obtain the polypropylene foam material, wherein the stretching speed of the casting device is 0.5m/s, and the draft ratio is 1.
Example 11:
weighing 90 parts by weight of polypropylene, 6 parts by weight of ammonium polyphosphate, 2 parts by weight of phenolic resin and 2 parts by weight of melamine.
The raw materials are mixed by a high-speed mixer and then added into a double-screw extruder, and the mixture is melted and extruded at 120 ℃ to obtain the premix.
The premix is added to a single screw extruder comprising an upper stage screw and a lower stage screw in series. Wherein the temperature of the upper-stage screw of the single-screw extruder is 195 ℃, the temperature of the lower-stage screw is 154 ℃, and the temperature of the extrusion die is 150 ℃. At 1/5 of the upper stage screw, 1 part by weight of supercritical carbon dioxide was injected under a pressure of 10 MPa. And (3) maintaining the pressure in the single-screw extruder at 10MPa, extruding and foaming, and stretching by adopting a casting device to obtain the polypropylene foam material, wherein the stretching speed of the casting device is 2.1m/s, and the draft ratio is 25.
Example 12:
60 parts by weight of polypropylene, 25 parts by weight of ammonium polyphosphate, 7.5 parts by weight of starch and 7.5 parts by weight of urea are weighed.
The raw materials are mixed by a high-speed mixer and then added into a double-screw extruder, and the mixture is melted and extruded at 230 ℃ to obtain the premix.
The premix is added to a single screw extruder comprising an upper stage screw and a lower stage screw in series. Wherein the temperature of the upper-stage screw of the single-screw extruder is 230 ℃, the temperature of the lower-stage screw is 150 ℃, and the temperature of the extrusion die is 155 ℃. At 1/3 on the upper stage screw, 15 parts by weight of supercritical carbon dioxide was injected under an injection pressure of 18 MPa. And (3) maintaining the pressure in the single-screw extruder at 7MPa, extruding and foaming, and stretching by adopting a casting device to obtain the polypropylene foam material, wherein the stretching speed of the casting device is 0.1m/s, and the draft ratio is 1.
Example 13:
weighing 85 parts by weight of polypropylene, 10 parts by weight of ammonium polyphosphate, 4 parts by weight of pentaerythritol and 1 part by weight of magnesium carbonate.
The raw materials are mixed by a high-speed mixer and then added into a double-screw extruder, and the mixture is melted and extruded at the temperature of 195 ℃ to obtain a premix.
The premix is added to a single screw extruder comprising an upper stage screw and a lower stage screw in series. Wherein the temperature of the upper-stage screw of the single-screw extruder is 195 ℃, the temperature of the lower-stage screw is 160 ℃, and the temperature of the extrusion die is 160 ℃. At 1/4 of the upper stage screw, 3 parts by weight of supercritical carbon dioxide was injected, and the injection pressure was set to 20 MPa. The pressure in the single-screw extruder is maintained at 12MPa, and the polypropylene foaming material is obtained by extrusion foaming.
Comparative example 1:
95 parts by weight of polypropylene and 5 parts by weight of calcium carbonate are weighed.
The raw materials are mixed by a high-speed mixer and then added into a double-screw extruder, and the mixture is melted and extruded at 200 ℃ to obtain the premix.
The premix is added to a single screw extruder comprising an upper stage screw and a lower stage screw in series. Wherein the temperature of the upper stage screw of the single screw extruder is set to 200 ℃ and the temperature of the lower stage screw is set to 170 ℃. At 1/4 of the upper stage screw, 4 parts by weight of supercritical carbon dioxide was injected, and the injection pressure was set to 15 MPa. The pressure in the single-screw extruder is maintained at 10MPa, and the polypropylene foaming material is obtained by extrusion foaming.
Comparative example 2:
100 parts by weight of polypropylene are weighed.
The raw materials are mixed by a high-speed mixer and then added into a double-screw extruder, and the mixture is melted and extruded at 200 ℃ to obtain the premix.
The premix is added to a single screw extruder comprising an upper stage screw and a lower stage screw in series. Wherein the temperature of the upper stage screw of the single screw extruder is set to 200 ℃ and the temperature of the lower stage screw is set to 170 ℃. At 1/4 of the upper stage screw, 4 parts by weight of supercritical carbon dioxide was injected, and the injection pressure was set to 15 MPa. And (3) maintaining the pressure in the single-screw extruder at 10MPa, extruding, foaming and stretching by adopting a casting device to obtain the polypropylene foam material, wherein the stretching speed of the casting device is 3.6m/s, and the draft ratio is 5.
The polyolefin foams obtained in examples 1 to 13, comparative example 1 and comparative example 2 were characterized in flame retardancy and mechanical properties, and the results are shown in Table 1. Wherein, the flame retardant property characterization adopts a VOUCH 5801A oxygen index tester and a VOUCH 5410 foam horizontal combustion tester.
TABLE 1
Figure BDA0001575831970000111
Figure BDA0001575831970000121
As can be seen from Table 1, the polyolefin foams which are not flame-retardant and modified in comparative examples 1 and 2 belong to flammable samples, and the polyolefin foams which are not obtained by the traction device in comparative examples 1 and 13 have poor mechanical properties.
The flame-retardant polyolefin foam materials obtained in the above examples 1 to 12 have controllable density, uniform cell structure, high foaming ratio, higher oxygen index, foam level combustion grade and specific tensile strength, and excellent flame retardant property and mechanical property.
The polypropylene foam material obtained in example 1 was subjected to microstructure and mechanical property characterization, wherein a ZEISS scanning electron microscope was used for microstructure characterization, an INSTRON universal tester was used for mechanical property characterization, and the results are shown in FIGS. 1 and 2. As can be seen from fig. 1, the polypropylene foam has a uniform cell structure. As can be seen from FIG. 2, the density was only 0.07g/cm3The polypropylene foaming material can lift objects which are thousands of times heavier than the polypropylene foaming material, and shows that the polypropylene foaming material has excellent mechanical properties.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.

Claims (9)

1. The preparation method of the polyolefin foam material is characterized by comprising the following steps:
(a) weighing 60-90 parts by weight of polyolefin, 10-40 parts by weight of intumescent flame retardant and 0-5 parts by weight of synergist, mixing, adding into an extruder, and performing melt extrusion to obtain a premix;
(b) adding the premix into a single-screw extruder, and extruding and foaming to obtain a polyolefin foam material; the single-screw extruder comprises an upper-stage screw and a lower-stage screw which are connected in series, the temperature of the upper-stage screw is 130-230 ℃, the temperature of the lower-stage screw is 80-180 ℃, the temperature of the lower-stage screw is lower than that of the upper-stage screw, the difference is T, T is more than or equal to 15 ℃ and less than or equal to 80 ℃, the temperature of an extrusion die is 80-180 ℃, and supercritical carbon dioxide is injected into 1/5-1/3 parts of the upper-stage screw.
2. The method for preparing polyolefin foam according to claim 1, wherein the polyolefin in step (a) is at least one of polyethylene, polypropylene, ethylene-propylene rubber, and ethylene-octene copolymer.
3. The method for preparing polyolefin foam material according to claim 1, wherein the intumescent flame retardant in step (a) is prepared by mixing an acid source, a carbon source and a gas source in a mass ratio of (2-4): (0-1).
4. The method for preparing polyolefin foam material according to claim 1, wherein the synergist in step (a) is at least one of antimony trioxide, calcium carbonate, magnesium carbonate, silica, montmorillonite, trehalite and kaolin.
5. The process for preparing polyolefin foam according to claim 1, wherein the total mass of the intumescent flame retardant and the synergist in step (a) is 10-40% of the mass of the premix.
6. The method for preparing polyolefin foam according to claim 1, wherein the amount of the supercritical carbon dioxide used in the step (b) is 0.5 to 15% by mass of the premix.
7. The method for preparing polyolefin foam according to claim 1, wherein the injection pressure of the supercritical carbon dioxide in the step (b) is 7MPa to 25 MPa.
8. The method for preparing polyolefin foam according to claim 1, further comprising a step (c) after the step (b) of extrusion foaming to obtain polyolefin foam: and (3) drawing and collecting the polyolefin foaming material by using a drawing device, wherein the drawing ratio of the drawing device is 0-80, and the drawing speed is 0.1-3.0 m/s.
9. The polyolefin foam material prepared by the preparation method of any one of claims 1 to 8, wherein the cell density of the polyolefin foam material is 104cell/cm3～1014cell/cm3The expansion ratio is 1.25 to 30.
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