CN113896992B - Foamed polypropylene beads and molded articles thereof - Google Patents
Foamed polypropylene beads and molded articles thereof Download PDFInfo
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- CN113896992B CN113896992B CN202111287190.6A CN202111287190A CN113896992B CN 113896992 B CN113896992 B CN 113896992B CN 202111287190 A CN202111287190 A CN 202111287190A CN 113896992 B CN113896992 B CN 113896992B
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/16—Making expandable particles
- C08J9/18—Making expandable particles by impregnating polymer particles with the blowing agent
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- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/04—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
- C08J9/12—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a physical blowing agent
- C08J9/122—Hydrogen, oxygen, CO2, nitrogen or noble gases
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- C08J2203/00—Foams characterized by the expanding agent
- C08J2203/06—CO2, N2 or noble gases
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2323/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- 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
- C08J2323/14—Copolymers of propene
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- C08J2423/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2423/02—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
- C08J2423/10—Homopolymers or copolymers of propene
- C08J2423/14—Copolymers of propene
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2427/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers
- C08J2427/02—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment
- C08J2427/12—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
- C08J2427/16—Homopolymers or copolymers of vinylidene fluoride
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2427/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers
- C08J2427/02—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment
- C08J2427/12—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
- C08J2427/18—Homopolymers or copolymers of tetrafluoroethylene
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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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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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- 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
- C08K7/00—Use of ingredients characterised by shape
- C08K7/02—Fibres or whiskers
- C08K7/04—Fibres or whiskers inorganic
- C08K7/14—Glass
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Abstract
The invention belongs to the technical field of foaming polypropylene, and in particular relates to a foaming polypropylene bead and a molded part thereof, wherein the foaming polypropylene bead is prepared by a high-temperature high-pressure kettle foaming method through composite particles, the composite particles comprise a core layer and a skin layer, and the core layer comprises the following components in percentage by mass: 3-10% of maleic anhydride modified polypropylene wax, 0.1-3% of plasticizer, 6-20% of reinforcing fiber, 0-0.1% of cell nucleating agent and the balance of polypropylene A; the cortex comprises the following components in percentage by mass: 3-10% of maleic anhydride modified polypropylene wax, 0.02-0.5% of fluorine-containing compound, 6-30% of reinforcing fiber and the balance of polypropylene B; the melting point of the polypropylene A is 145-152 ℃, and the melting point of the polypropylene B is 120-135 ℃. The molded article prepared from the expanded polypropylene beads has strong warping resistance and excellent dimensional stability, and the surface hardness of the molded article with the density of 28-32g/L is not lower than 55Shore A.
Description
Technical Field
The invention belongs to the technical field of foaming polypropylene, and particularly relates to foaming polypropylene beads and molded parts thereof.
Background
The expanded polypropylene beads (EPP) produced by the kettle-type foaming method have the advantages of high expansion ratio, excellent rebound resilience and suitability for steam molding, so that the EPP molded parts retain the characteristics of light weight, firm sintering, excellent mechanical property and excellent energy absorption, and are widely used in the fields of automobile part structural materials, precise packaging materials and the like.
Along with the continuous expansion of EPP application markets, in some application scenes with larger environmental temperature change spans, the EPP structural member or the buffering protection part is required to have small buckling deformation. In particular, when the EPP products with high foaming ratio on the market at present suddenly change along with the ambient temperature, the EPP products are difficult to maintain dimensional stability or small buckling deformation, and have defects on the use effect.
In view of the above, there is a need for developing a foamed polypropylene bead having small warp deformation and excellent dimensional stability and a molded article thereof.
Disclosure of Invention
In order to solve the problems, the invention discloses a foaming polypropylene bead and a molded part thereof, wherein the foaming polypropylene bead uses composite particles of low-melting-point PP coated with high-melting-point PP, which is beneficial to the low molding pressure of the foaming bead, the plasticizer is beneficial to improving the molding expansibility of the foaming bead, the foaming core layer has enough molding expansibility under the lower molding pressure, the molded part has excellent surface, meanwhile, the core layer is added with reinforcing fibers, the EPP bead and the anti-buckling deformation capability of the molded part thereof are beneficial to improving, and the skin layer is also added with reinforcing fibers, so that the hardness of the surface of the foaming bead can be enhanced, and the EPP molded part has a promoting effect on the anti-buckling deformation of the EPP molded part.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
the expanded polypropylene beads are prepared by a high-temperature high-pressure kettle type foaming method through composite particles, wherein the composite particles comprise a core layer and a skin layer, and the core layer comprises the following components in percentage by mass: 3-10% of maleic anhydride modified polypropylene wax, 0.1-3% of plasticizer, 6-20% of reinforcing fiber, 0-0.1% of cell nucleating agent and the balance of polypropylene A; the cortex comprises the following components in percentage by mass: 3-10% of maleic anhydride modified polypropylene wax, 0.02-0.5% of fluorine-containing compound, 6-30% of reinforcing fiber and the balance of polypropylene B; the melting point of the polypropylene A is 145-152 ℃, and the melting point of the polypropylene B is 120-135 ℃.
Preferably, the polypropylene A is random copolymer polypropylene, preferably polypropylene butyl copolymer polypropylene, and has a melt index of 6-9g/10min; the polypropylene B is propylene-ethylene-butylene ternary random copolymer, and the melt index is 7-12g/10min.
Preferably, the reinforcing fiber is one or more of glass fiber, carbon fiber and aramid fiber, and the diameter of the reinforcing fiber is 0.2-30 μm, and the length-diameter ratio is 7-20.
Preferably, the fluorine-containing compound is a powder of a fluorine-containing rubber and/or a fluorine-containing resin, and the powder has an average particle diameter of 1 to 20 μm;
the plasticizer is one or more of liquid paraffin, dioctyl phthalate, dibutyl phthalate, ma Laisong glyceride sea acid and glyceryl monostearate;
the average molecular weight of the maleic anhydride modified polypropylene wax is 5000-10000.
Preferably, the cell nucleating agent is one or more of silicon dioxide, zinc borate, talcum powder, barium sulfate and calcium carbonate, and the particle size of the cell nucleating agent is 3-6 mu m.
Preferably, the cell nucleating agent is silica.
Preferably, the cortex accounts for 3-20% of the total mass of the composite particles; the length of the composite particles is 1.2-2.5mm, and the single weight is 0.5-1.8mg.
Preferably, the preparation method of the composite particles comprises the following steps:
(1) The reinforced fiber is treated by a silane coupling agent, dried, mixed with polypropylene A, maleic anhydride modified polypropylene wax, a plasticizer and a foam cell nucleating agent according to a certain proportion, and extruded and granulated by a double screw to prepare a core layer master batch;
(2) The reinforced fiber is treated by a silane coupling agent, dried, mixed with maleic anhydride modified polypropylene wax, fluorine compound powder and polypropylene B according to a certain proportion, and extruded and granulated by a double screw to prepare a skin master batch;
(3) And respectively adding the core layer master batch and the skin layer master batch into a core layer extruder and a skin layer extruder of a double single screw co-extrusion unit, plasticizing, and granulating through a co-extrusion die to obtain the composite particles with the skin layers coating the core layer.
Preferably, the preparation method of the foaming polypropylene beads comprises the following steps: adding the composite particles, dispersant and water into an autoclave, sealing, and adding CO 2 Continuously stirring, raising the temperature of the reaction kettle to a foaming temperature, regulating the pressure in the kettle to a foaming pressure, maintaining the pressure at the foaming temperature and the pressure for 5-30min, discharging the materials into a normal-pressure foaming pipeline for foaming under the conditions of the foaming temperature and the pressure, wherein the atmosphere temperature in the foaming pipeline is 90-110 ℃, the time of the materials in the foaming pipeline is 4-15s, and finally obtaining the foaming beads with the bulk density of 15-120g/L, wherein the endothermic enthalpy value of a melting peak of the foaming beads in a primary DSC melting curve is 14-23J/g (hereinafter referred to as the endothermic enthalpy value of a high-temperature melting peak).
The foamed polypropylene bead molded part is obtained by adopting the foamed polypropylene beads through steam sintering molding, and comprises the following specific steps: the expanded beads are molded by steam molding after being air-borne.
The invention has the following beneficial effects:
(1) The composite particles of the low-melting-point PP coated with the high-melting-point PP are used for the expanded polypropylene beads, the low molding pressure of the expanded polypropylene beads is facilitated, the plasticizer is favorable for improving the molding expansibility of the expanded polypropylene beads, the expanded core layer has enough molding expansibility under the lower molding pressure, the molded product has excellent surface, meanwhile, the reinforcing fiber is added into the core layer, the EPP beads and the molded product of the EPP beads are improved in buckling deformation resistance, the reinforcing fiber is added into the skin layer, the hardness of the surface of the expanded polypropylene beads can be enhanced, the EPP molded product is promoted, the molded product prepared by the expanded polypropylene beads has strong buckling deformation resistance and excellent dimensional stability, and the surface hardness of the molded product with the density of 28-32g/L is not lower than 55Shore A.
(2) The addition amount of the plasticizer is controlled to be 0.1-3%, when the content of the plasticizer is lower than 0.1%, the molding promoting effect is not obvious, and when the content of the plasticizer is higher than 3%, the EPP warping resistance is weakened; the addition amount of the reinforcing fibers in the core layer is 6-20%, the fiber content in the core layer is lower than 6%, the reinforcing effect is not obvious, and the foamability of the core layer is affected when the fiber content is higher than 20%, namely the closed cell structure is not facilitated.
(3) The core layer of the foaming bead obtained by foaming the composite particles is of a closed cell structure, the skin layer is not foamed or is very little foamed, the skin layer ratio of the composite particles is 3-20%, and the foaming bead and a formed part are better in buckling deformation resistance on the premise of guaranteeing stable promotion of sintering of the surface of the bead.
Detailed Description
The present invention will now be described in further detail with reference to examples.
Polypropylene A is polypropylene propylene-ethylene-butylene copolymer, polypropylene B is propylene-ethylene-butylene terpolymer, and the molecular weight of the maleic anhydride modified polypropylene wax is 8000.
The main experimental material properties are shown in table 1.
TABLE 1
The formulations and parameters of the composite particles S1 to S7 and the composite particles D1 to D6 are shown in Table 2.
TABLE 2
The preparation method of the composite particles comprises the following steps:
(1) The reinforced fiber is treated by a silane coupling agent, dried, mixed with polypropylene A, maleic anhydride modified polypropylene wax, a plasticizer and a foam cell nucleating agent according to a certain proportion, and extruded and granulated by a double screw to prepare a core layer master batch;
(2) The reinforced fiber is treated by a silane coupling agent, dried, mixed with maleic anhydride modified polypropylene wax, fluorine compound powder and polypropylene B according to a certain proportion, and extruded and granulated by a double screw to prepare a skin master batch;
(3) And respectively adding the core layer master batch and the skin layer master batch into a core layer extruder and a skin layer extruder of a double single screw co-extrusion unit, plasticizing, and granulating through a co-extrusion die to obtain the composite particles with the skin layers coating the core layer.
The preparation method of the foaming beads by adopting the composite particles S1-S4 and the composite particles D1-D7 comprises the following steps: adding the composite particles, dispersant and water into an autoclave, sealing, and adding CO 2 Continuously stirring, raising the temperature of the reaction kettle to a foaming temperature, regulating the pressure in the kettle to a foaming pressure, maintaining the pressure for 5-30min under the conditions of the foaming temperature and the pressure, discharging the materials into a normal-pressure foaming pipeline for foaming, wherein the atmosphere temperature in the foaming pipeline is 90-110 ℃, the time of the materials in the foaming pipeline is 4-15s, and finally obtaining the foaming beads with the bulk density of 15-120g/L, and the endothermic enthalpy value of a melting peak higher than the inherent melting point in a primary DSC melting curve of the foaming beads is 14-23J/g.
The prepared foaming beads are subjected to air bearing pressure and then are molded by vapor to obtain molded parts.
The various parameters and molding properties during the preparation of examples 1-4 and comparative examples 1-6 are shown in Table 3.
TABLE 3 Table 3
Wherein, the minimum molding pressure: the foamed bead molding has broken cells at a minimum vapor sintering pressure required for 95% or more.
Apparent mass of the product: "i" means more pits or crevices on the surface of the article; "ii" means a small number of pits or gaps in the surface of the article; "iii" means that the surface of the article has no or very few or very small pits or gaps.
High-low temperature alternating damp-heat experiment: cutting the molded part into sample blocks with the length of 200mm, the width of 200mm and the thickness of 30mm, wherein the test conditions are as follows: storing at 90 ℃ for 3 hours; storing for 1h at normal temperature; storing at-40 ℃ for 3 hours; storing for 1h at normal temperature; storing at 50deg.C and 95% RH for 15 hr, and storing at normal temperature for 1 hr; the above 6 processing steps were 1 cycle, and the sample was run for 3 cycles. And measuring the length, width and thickness of the sample block after the high-low temperature alternating damp heat treatment, wherein the deformation is preferably less than 1%. Each sample was tested simultaneously for 6 sets of coupons, and the data of the largest deformation in the coupons (deformation of the length, width, and thickness dimensions of the 6 sets of coupons) was recorded in the table. The smaller the deformation value of the high-low temperature alternating damp-heat experiment is, the stronger the warping resistance of the sample under the influence of temperature is.
Comparative examples 1-4 in Table 3 the foaming conditions were adjusted in order to obtain a bulk density similar to that of example 4, since the composite particle formulation was different from example 4.
The molded samples of examples 1-4 all had excellent warp resistance and surface hardness. Comparative example 1, the composite microparticle core layer was not added with fiber reinforcement, and the molded part was large in deformation in high-low temperature alternating wet heat experiments; comparative example 2, in which fiber reinforcement was absent in the composite microparticle skin, the surface hardness of the molded article was reduced, and the deformation in the high-low temperature alternating wet heat test was large; comparative example 3, the foam core layer has lower reinforcing fiber content and weaker reinforcing effect, and the molded part has larger deformation in a high-low temperature alternating wet heat experiment; comparative example 4, the foam core layer has too high content of reinforced fiber, influences the foaming capacity of the core layer, is unfavorable for a closed cell structure, and has large deformation in a high-low temperature alternating damp-heat experiment of a molded part; comparative example 5, the foam core layer reinforced fiber has smaller length-diameter ratio, weak fiber reinforcement effect and larger deformation of the molded part in a high-low temperature alternating wet heat experiment; in comparative example 6, the length-diameter ratio of the reinforced fiber of the foaming core layer is too large, the foaming capacity of the core layer is affected, the closed cell structure is not facilitated, and the deformation of a molded part in a high-low temperature alternating damp-heat experiment is large.
With the above-described preferred embodiments according to the present invention as an illustration, the above-described descriptions can be used by persons skilled in the relevant art to make various changes and modifications without departing from the scope of the technical idea of the present invention. The technical scope of the present invention is not limited to the description, but must be determined according to the scope of claims.
Claims (6)
1. A foamed polypropylene bead characterized by: the foaming polypropylene beads are prepared by a high-temperature high-pressure kettle foaming method through composite particles, the composite particles comprise a core layer and a skin layer, and the core layer comprises the following components in percentage by mass: 3-10% of maleic anhydride modified polypropylene wax, 0.1-3% of plasticizer, 6-20% of reinforcing fiber, 0-0.1% of cell nucleating agent and the balance of polypropylene A; the cortex comprises the following components in percentage by mass: 3-10% of maleic anhydride modified polypropylene wax, 0.02-0.5% of fluorine-containing compound, 6-30% of reinforcing fiber and the balance of polypropylene B; the melting point of the polypropylene A is 145-152 ℃, and the melting point of the polypropylene B is 120-135 ℃; the reinforcing fiber is one or more of glass fiber, carbon fiber and aramid fiber, the diameter of the reinforcing fiber is 0.2-30 mu m, and the length-diameter ratio is 7-20;
the cortex accounts for 3-20% of the total mass of the composite particles; the length of the composite particles is 1.2-2.5mm, and the single weight is 0.5-1.8mg;
the preparation method of the composite particles comprises the following steps: (1) The reinforced fiber is treated by a silane coupling agent, dried, mixed with polypropylene A, maleic anhydride modified polypropylene wax, a plasticizer and a foam cell nucleating agent according to a certain proportion, and extruded and granulated by a double screw to prepare a core layer master batch; (2) The reinforced fiber is treated by a silane coupling agent, dried, mixed with maleic anhydride modified polypropylene wax, fluorine compound powder and polypropylene B according to a certain proportion, and extruded and granulated by a double screw to prepare a skin master batch; (3) Respectively adding the core layer master batch and the skin layer master batch into a core layer extruder and a skin layer extruder of a double single screw co-extruder unit, plasticizing, and simultaneously carrying out filament discharge granulation through a co-extrusion die to obtain composite particles of the skin layer coated core layer;
the preparation method of the foaming polypropylene beads comprises the following steps: adding the composite particles, dispersant and water into an autoclave, sealing, and adding CO 2 Continuously stirring, increasing the temperature of the reaction kettle to the foaming temperature, regulating the pressure in the kettle to the foaming pressure, maintaining the pressure at the foaming temperature and the pressure for 5-30min, discharging the materials into a normal-pressure foaming pipeline for foaming under the pressure release, wherein the atmosphere temperature in the foaming pipeline is 90-110 ℃, and the materials are in the state of beingThe time of the foaming pipeline is 4-15s, and finally the foaming beads with the bulk density of 15-120g/L are obtained, and the endothermic enthalpy value of a melting peak higher than the inherent melting point in the primary DSC melting curve of the foaming beads is 14-23J/g.
2. The expanded polypropylene bead according to claim 1, wherein: the polypropylene A is polypropylene copolymer polypropylene with a melt index of 6-9g/10min; the polypropylene B is propylene-ethylene-butylene ternary random copolymer, and the melt index is 7-12g/10min.
3. The expanded polypropylene bead according to claim 1, wherein: the fluorine-containing compound is fluorine-containing rubber and/or fluorine-containing resin powder, and the average particle size of the powder is 1-20 mu m; the plasticizer is one or more of liquid paraffin, dioctyl phthalate, dibutyl phthalate, ma Laisong glyceride sea acid and glyceryl monostearate; the average molecular weight of the maleic anhydride modified polypropylene wax is 5000-10000.
4. The expanded polypropylene bead according to claim 1, wherein: the cell nucleating agent is one or more of silicon dioxide, zinc borate, talcum powder, barium sulfate and calcium carbonate, and the particle size of the cell nucleating agent is 3-6 mu m.
5. The expanded polypropylene bead according to claim 1, wherein: the cell nucleating agent is silicon dioxide.
6. A foamed polypropylene bead molded article characterized by: the expanded polypropylene beads according to any one of claims 1 to 5, which are obtained by steam sintering molding, comprising the following steps: the expanded beads are molded by steam molding after being air-borne.
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