CN114456511A - Expanded polyolefin bead and preparation method thereof - Google Patents
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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
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- 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
- 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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- C08J2201/00—Foams characterised by the foaming process
- C08J2201/02—Foams characterised by the foaming process characterised by mechanical pre- or post-treatments
- C08J2201/034—Post-expanding of foam beads or sheets
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- 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
- 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
- C08J2325/00—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 an aromatic carbocyclic ring; Derivatives of such polymers
- C08J2325/02—Homopolymers or copolymers of hydrocarbons
- C08J2325/04—Homopolymers or copolymers of styrene
- C08J2325/06—Polystyrene
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2351/00—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
- C08J2351/04—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 rubbers
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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
- C08J2423/04—Homopolymers or copolymers of ethene
- C08J2423/08—Copolymers of ethene
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- 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
- 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
- C08J2451/04—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 rubbers
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
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Abstract
The application belongs to the technical field of foaming materials, and particularly relates to a foaming polyolefin bead and a preparation method thereof, wherein the foaming polyolefin bead at least comprises the following components in percentage by mass: 20-35% of crystalline polymer, 8-20% of compatilizer and the balance of polystyrene. According to the preparation method of the expanded polyolefin beads, special material selection and proportioning are adopted, the polystyrene phase in the blend is uniformly dispersed in the crystalline polymer phase, and the cells are uniform; the obtained expanded beads have excellent rigidity and excellent resilience, and the beads are molded at a low sintering pressure (less than 0.12MPa), and the molded articles have little or no cracks or dents in appearance.
Description
Technical Field
The application belongs to the technical field of foaming materials, and particularly relates to a foamed polyolefin bead and a preparation method thereof.
Background
The foamed bead molded part is light and easy to adjust in shape, and is widely applied to the fields of automobile assembly parts, packaging and transporting buffer materials, light structural parts and the like. The most used bead foam products at present are expanded polystyrene EPS, followed by expanded polyethylene EPE and expanded polypropylene EPP. Under the same foaming ratio, EPS has more excellent rigidity and dimensional stability, but the fusion between beads is poorer, and a product is more fragile and cracked.
The chinese patent technology CN113502025A uses a co-extrusion process of cladding the core layer with the skin layer to obtain composite particles, and through a high-temperature and high-pressure kettle-type foaming process, foamed EPO beads are obtained, and the bead molded product does not indicate excellent toughness, and the surface quality further improves the space (no or few gaps and pits).
Therefore, there is a need for Expanded Polyolefin (EPO) beads based on polystyrene, and it is desired that molded articles thereof have excellent rigidity, high bead sintering strength, and excellent toughness.
Disclosure of Invention
In order to solve the problems, the application discloses expanded polyolefin beads and a preparation method thereof, and the process is simple and environment-friendly; special material selection and proportion are adopted, the polystyrene phase in the blend is uniformly dispersed in the crystalline polymer phase, and the cells are uniform; the obtained expanded beads have excellent rigidity and excellent resilience, the sintering pressure for bead molding is low (less than 0.12MPa), and the molded articles have little or no gaps and pits in appearance.
In a first aspect, the present application provides an expanded polyolefin bead, which employs the following technical solutions:
expanded polyolefin beads comprising at least the following components in mass percent: 20-35% of crystalline polymer, 8-20% of compatilizer and the balance of polystyrene.
Preferably, the polystyrene is GPPS or HIPS, the molecular weight is 20-35 ten thousand, the melt index is 3-10g/10min, and the flexural modulus is not lower than 1800 MPa.
Preferably, the crystalline polymer includes 50 to 85% of linear low density polyethylene and 15 to 50% of an ethylene-alpha olefin random copolymer or block copolymer;
the linear low-density polyethylene has a melt index of 3-10g/10min and a melting point of 100-110 ℃; the ethylene-alpha olefin random copolymer or block copolymer has a melt index of 2-10g/10min and a melting point of 95-125 ℃.
Preferably, the compatilizer at least comprises 30-50% of polystyrene with a peroxide bond in a side group, and the other compatilizer comprises one or more of maleic anhydride grafted EPDM, maleic anhydride grafted SEBS, maleic anhydride grafted POE, maleic anhydride grafted EVA, maleic anhydride grafted polyethylene and hydroxylated polyethylene.
Preferably, the expanded polyolefin beads further comprise 0.01 to 5% of an auxiliary.
Preferably, the above-mentioned auxiliaries comprise from 0.01 to 0.5% of a foam cell nucleating agent.
According to specific requirements, the auxiliary agent can also comprise other auxiliary agents, such as a coloring agent (0-4%), an antioxidant (0-0.5%), an antistatic agent (0-2%), a lubricant (0-1%), a plasticizer (0-5%) and the like.
Preferably, the foam cell nucleating agent is one or two of sodium chloride and potassium chloride, and the average grain diameter is 8-15 μm.
The sodium chloride and/or potassium chloride with special particle size has excellent water absorption and dispersibility, and is beneficial to the expansibility of the expanded beads and uniform cells.
In a second aspect, the present application provides a method for preparing expanded polyolefin beads, which adopts the following technical scheme:
a process for the preparation of expanded polyolefin beads, characterized in that: the method comprises the following steps:
(1) mixing polystyrene, a crystalline polymer, a compatilizer and an auxiliary agent, and then extruding, drawing, granulating to obtain blended particles;
(2) putting the blended particles, a dispersing medium, a dispersing agent and a dispersing auxiliary agent into a closed high-pressure resistant kettle according to a certain weight ratio, and continuously stirring; heating the materials in the kettle to 148 ℃ and 165 ℃, and filling CO2Keeping the pressure at 2.4-5.5MPa for 5-30 min; the dispersion was discharged into a low pressure zone to give expanded primary expanded polyolefin beads having a bulk density of 46-80 g/L.
(3) After the primary expanded polyolefin beads are maintained at normal temperature for 12-24 hours, sealing the primary expanded polyolefin beads into a pre-pressing tank, carrying pressure by using air, wherein the pressure carrying pressure is 0.2-0.5MPa, the pressure carrying time is 8-30 hours, and the primary expanded beads after carrying pressure are heated and expanded in a normal-pressure circulation foaming pipeline at 80-95 ℃ to form a secondary expanded bead finished product with lighter density; the bulk density is 12-45 g/L.
The bulk density of the secondary expanded beads is generally 12-45g/L, and when the bulk density is lower than 12g/L, the expanded beads are easy to break holes or lose use value; the bulk density of the primary expanded beads used for producing the secondary expanded beads is preferably 46 to 70g/L, and the primary beads are lighter in density and tend to break the closed cell structure, and the primary beads are higher in density and tend not to be secondarily expanded to a lighter density.
Preferably, the length of the blended micro-particles is 1.5-2.5mm, and the single weight is 1.5-3 mg; the dispersion medium is deionized water; the dispersant is silicate mineral powder, preferably kaolin, and the average particle size of the dispersant is 0.1-2 μm; the dispersing auxiliary agent is an anionic surfactant and at least comprises sodium dodecyl benzene sulfonate.
Preferably, the weight parts of the components are as follows: 100 parts of resin particles, 200 parts of dispersion medium 150-.
The application has the following beneficial effects:
(1) the expanded polyolefin bead adopts special material selection and proportion, the polystyrene phase in the blend is uniformly dispersed in the crystalline polymer phase, and the cells are uniform; the obtained expanded beads have excellent rigidity and excellent resilience, the sintering pressure for bead molding is low (less than 0.12MPa), and the molded articles have little or no gaps and pits in appearance.
(2) The ethylene-alpha olefin random copolymer or block copolymer added in the crystalline polymer is a crystalline elastomer, can endow the blended material with better toughness, and the combined compatilizer containing the polystyrene with peroxide bonds on the side group is favorable for the interface compatibility of the crystalline polymer and the polystyrene.
(3) The foam cell nucleating agent selects sodium chloride and/or potassium chloride with the average grain diameter of 8-15 mu m, and the sodium chloride and/or potassium chloride with special grain diameter has excellent water absorption and dispersibility, thereby being beneficial to the expansibility of the foaming bead and the uniformity of foam cells.
(4) The preparation method of the expanded polyolefin beads is simple and environment-friendly in process. The molded part prepared from the expanded beads has excellent rigidity and toughness, greatly improves the defect that an EPS (expandable polystyrene) using part is easy to be brittle, and well retains the using rigidity. The molded article has a density of 18 to 22g/L, a surface hardness of not less than 40Shore A, a tensile strength of not less than 250KPa, and an elongation at break of not less than 25%.
Drawings
The present application is further described below with reference to the drawings and examples.
FIG. 1 is an SEM photograph of a cross section of a secondary expanded bead of example 4 of the present application.
Detailed Description
The present application will now be described in further detail with reference to examples.
The foaming process comprises the following steps:
the components are mixed according to the following weight portions: 100 parts of resin particles, 200 parts of dispersion medium 150-.
(1) Putting the blended particles, a dispersing medium, a dispersing agent and a dispersing auxiliary agent into a closed high-pressure resistant kettle according to a certain weight ratio, and forming a dispersing system under the continuous stirring action;
(2) heating the dispersion in the kettle to a foaming temperature of 148-165 ℃ and introducing a certain amount of CO2The pressure reaches 2.4-5.5MPa, and the foaming time is kept for 5-30 min; release the dispersionPlacing in a low pressure zone to obtain expanded primary expanded polyolefin beads having a bulk density of 46-80 g/L;
(3) if foamed beads with lighter density are required, selecting primary foamed beads with the bulk density of 46-70g/L, after 12-24h of normal temperature maintenance, sealing the primary foamed beads into a pre-pressing tank, carrying pressure by using air, wherein the carrying pressure is 0.2-0.5MPa, and the carrying pressure time is 8-30h, and carrying the pressed primary foamed beads to be heated and expanded in a normal-pressure flowing foaming pipeline at the temperature of 80-95 ℃ to form a secondary foamed bead finished product with lighter density; the bulk density is 12-45 g/L.
The steam molding process with the expanded beads comprises the following steps: and filling the foamed particles subjected to pressure loading by the pre-pressing tank into a mold cavity through a vacuum pipeline, expanding the beads and fusing the skins mutually under the action of high-temperature steam, and cooling and shaping through flowing water on the surface of the mold to obtain the EPO molded part. The molded product needs to be further cured and shaped in a hot air curing chamber at 50-70 ℃ so as to obtain a usable EPO product.
The main experimental material properties are shown in table 1.
TABLE 1
The formulation of the crystalline polymer is shown in table 2, and each substance in table 2 is in mass percent.
TABLE 2
| Crystalline polymer | J1 | J2 | J3 | J4 | J5 |
| Linear low density polyethylene | 50 | 85 | 70 | 0 | 100 |
| Ethylene-alpha olefin random copolymer | 50 | 30 | 100 | 0 | |
| Ethylene-alpha olefin block copolymer | 15 |
The formulation of the compatibilizer is shown in table 3, and the materials in table 3 are in mass percent.
TABLE 3
| Compatilizer | X1 | X2 | X3 | X4 | X5 |
| Polystyrene with peroxide bond in side group | 30 | 50 | 40 | 0 | 100 |
| Maleic anhydride grafted EPDM | 30 | ||||
| Maleic anhydride grafted SEBS | 40 | 50 | 60 | 100 | 0 |
The formulations and parameters of the examples and comparative examples are shown in table 4, in which the substances are given in mass percent in table 4.
TABLE 4
The results of the performance test of the secondary expanded beads obtained in each example and comparative example are shown in Table 5.
TABLE 5
The lowest molding pressure: the minimum steam sintering pressure required for the broken-section cells of the expanded bead molding is greater than 95%.
Apparent mass of the product: "I" indicates that the surface of the product has more pits or gaps; "II" means a small number of pits or gaps on the surface of the article; "III" means that there are no, or few or very small pits or gaps in the surface of the article.
As is clear from Table 4, the secondary expanded beads of examples 1 to 4 were low in molding pressure, excellent in apparent mass of molded articles, and high in tensile strength and elongation at break. FIG. 1 is an SEM photograph of a cross section of the secondary expanded bead of example 4, and it can be seen that the secondary expanded bead prepared has a high cell uniformity.
The crystalline polymer component of comparative example 1, which is entirely elastomeric, theoretically facilitates an increase in material toughness (the greater the tensile strength and elongation at break values within a certain range, the better the toughness of the molded part), but the relative deterioration in sintered strength of the expanded beads also results in a decrease in elongation at break. The crystalline polymer component of comparative example 2 was entirely linear low density polyethylene, the toughness was relatively deteriorated, and the elongation at break was reduced. The compatibilizer of comparative example 3 lacks the effect of polystyrene having peroxide bonds in its pendant groups, and the compatibility of the crystalline polymer phase and the polystyrene phase becomes poor, resulting in a molded article that appears to have severe pits and gaps, and significantly reduced tensile strength and elongation at break. The compatibilizer of comparative example 4 lacks the effect of maleic anhydride grafted SEBS, and the compatibility of the crystalline polymer phase and the polystyrene phase becomes poor, resulting in a molded article having a severe appearance of pits and gaps, and a significant decrease in tensile strength and elongation at break.
The present embodiment is merely illustrative and not restrictive, and various changes and modifications may be made by persons skilled in the art without departing from the scope of the present invention as defined in the appended claims. The technical scope of the present application is not limited to the contents of the specification, and must be determined according to the scope of the claims.
Claims (10)
1. Expanded polyolefin beads characterized in that: the expanded polyolefin bead at least comprises the following components in percentage by mass: 20-35% of crystalline polymer, 8-20% of compatilizer and the balance of polystyrene.
2. The expanded polyolefin bead according to claim 1, wherein: the polystyrene is GPPS or HIPS, the molecular weight is 20-35 ten thousand, the melt index is 3-10g/10min, and the flexural modulus is not lower than 1800 MPa.
3. The expanded polyolefin bead according to claim 1, wherein: the crystalline polymer comprises 50-85% of linear low density polyethylene and 15-50% of ethylene-alpha olefin random copolymer or block copolymer;
the linear low-density polyethylene has a melt index of 3-10g/10min and a melting point of 100-110 ℃; the ethylene-alpha olefin random copolymer or block copolymer has a melt index of 2-10g/10min and a melting point of 95-125 ℃.
4. The expanded polyolefin bead according to claim 1, wherein: the compatilizer at least comprises 30-50% of polystyrene with a side group containing peroxide bonds, and the other compatilizer comprises one or more of maleic anhydride grafted EPDM, maleic anhydride grafted SEBS, maleic anhydride grafted POE, maleic anhydride grafted EVA, maleic anhydride grafted polyethylene and hydroxylated polyethylene.
5. The expanded polyolefin bead according to claim 1, wherein: the expanded polyolefin beads further comprise 0.01 to 5% of an auxiliary agent.
6. The expanded polyolefin bead according to claim 5, wherein: the auxiliary agent comprises 0.01-0.5% of foam cell nucleating agent.
7. The expanded polyolefin bead according to claim 6, wherein: the foam cell nucleating agent is one or two of sodium chloride and potassium chloride, and the average grain diameter is 8-15 mu m.
8. A process for the preparation of expanded polyolefin beads according to claim 5, characterized in that: the method comprises the following steps:
(1) mixing polystyrene, a crystalline polymer, a compatilizer and an auxiliary agent, and then extruding, drawing, granulating to obtain blended particles;
(2) putting the blended particles, a dispersing medium, a dispersing agent and a dispersing auxiliary agent into a closed high-pressure resistant kettle according to a certain weight ratio, and continuously stirring; heating the materials in the kettle to 148 ℃ and 165 ℃, and filling CO2Keeping the pressure at 2.4-5.5MPa for 5-30 min; releasing the dispersion into a low pressure zone to obtain expanded primary expanded polyolefin beads having a bulk density of 46-80 g/L;
(3) after the primary expanded polyolefin beads are maintained at normal temperature for 12-24 hours, sealing the primary expanded polyolefin beads into a pre-pressing tank, carrying pressure by using air, wherein the pressure carrying pressure is 0.2-0.5MPa, the pressure carrying time is 8-30 hours, and the primary expanded beads after carrying pressure are heated and expanded in a normal-pressure circulation foaming pipeline at 80-95 ℃ to form a secondary expanded bead finished product with lighter density; the bulk density is 12-45 g/L.
9. Process for the preparation of expanded polyolefin beads according to claim 8, characterized in that: the length of the blended particle is 1.5-2.5mm, and the single weight is 1.5-3 mg; the dispersion medium is deionized water; the dispersant is silicate mineral powder, preferably kaolin, and the average particle size of the dispersant is 0.1-2 μm; the dispersing auxiliary agent is an anionic surfactant and at least comprises sodium dodecyl benzene sulfonate.
10. Process for the preparation of expanded polyolefin beads according to claim 8, characterized in that: the weight parts of the components are as follows: 100 parts of resin particles, 200 parts of dispersion medium 150-.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115895083A (en) * | 2022-11-14 | 2023-04-04 | 江苏卡普丹建筑科技有限公司 | Foam core metal composite plate and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115895083A (en) * | 2022-11-14 | 2023-04-04 | 江苏卡普丹建筑科技有限公司 | Foam core metal composite plate and preparation method thereof |
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