CN114456511B - Foaming polyolefin beads 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
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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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- C08J2203/00—Foams characterized by the expanding agent
- C08J2203/06—CO2, N2 or noble gases
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- 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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- 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
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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 foaming polyolefin beads, special material selection and proportion are adopted, a polystyrene phase in the blend is uniformly dispersed in a crystalline polymer phase, and cells are uniform; the resulting expanded beads have excellent rigidity and excellent resilience, the bead molding sintering pressure is low (less than 0.12 MPa), and the molded article has little or no appearance of gaps and pits.
Description
Technical Field
The application belongs to the technical field of foaming materials, and particularly relates to a foaming polyolefin bead and a preparation method thereof.
Background
The foam bead molded part is light in weight and easy to adjust in shape, and is widely applied to the fields of automobile assembly parts, packaging and transportation buffer materials, light structural parts and the like. The bead foam products with the largest usage amount at present are expanded polystyrene EPS, and then expanded polyethylene EPE and expanded polypropylene EPP. Under the same foaming ratio, EPS has more excellent rigidity and dimensional stability, but fusion bonding among beads is worse, and a finished piece is more fragile and cracked.
Chinese patent CN113502025a uses a coextrusion process of a sheath-coated core layer to obtain composite particles, and a high-temperature and high-pressure kettle-type foaming process is performed to obtain expanded EPO beads, and the molded product of the beads does not show excellent toughness, and further improves the surface quality (no or few gaps or pits).
Therefore, there is a need to develop a polystyrene-based Expanded Polyolefin (EPO) bead, which is expected to have excellent rigidity of molded articles, while having high bead sintering strength and excellent toughness of molded articles.
Disclosure of Invention
In order to solve the problems, the application discloses a foaming polyolefin bead and a preparation method thereof, and the process is simple and environment-friendly; adopting 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 resulting expanded beads have excellent rigidity and excellent resilience, the bead molding sintering pressure is low (less than 0.12 MPa), and the molded article has little or no appearance of gaps and pits.
In a first aspect, the present application provides a foamed polyolefin bead, employing the following technical scheme:
a foamed polyolefin bead 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 1800MPa.
Preferably, the crystalline polymer comprises 50-85% of linear low density polyethylene and 15-50% of ethylene-alpha olefin random copolymer or block copolymer;
the melt index of the linear low density polyethylene is 3-10g/10min, and the melting point is 100-110 ℃; the melt index of the ethylene-alpha olefin random copolymer or the block copolymer is 2-10g/10min, and the melting point is 95-125 ℃.
Preferably, the compatilizer at least comprises polystyrene with a peroxide bond at 30-50% of side groups, 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 agent.
Preferably, the above-mentioned auxiliary agents include 0.01 to 0.5% of a cell nucleating agent.
According to specific requirements, other auxiliary agents such as coloring agents (0-4%), antioxidants (0-0.5%), antistatic agents (0-2%), lubricants (0-1%), plasticizers (0-5%) and the like can be further included in the auxiliary agents.
Preferably, the cell nucleating agent is one or two of sodium chloride and potassium chloride, and the average particle diameter is 8-15 μm.
Sodium chloride and/or potassium chloride with special particle size has excellent water absorption and dispersibility, and is favorable for the expansibility and the uniformity of cells of the foaming beads.
In a second aspect, the present application provides a method for preparing expanded polyolefin beads, which adopts the following technical scheme:
a process for preparing expanded polyolefin beads characterized by: the method comprises the following steps:
(1) Mixing polystyrene, a crystalline polymer, a compatilizer and an auxiliary agent, extruding, wiredrawing and granulating to obtain blended particles;
(2) Will blend into micro-sizedThe particles, the dispersing medium, the dispersing agent and the dispersing auxiliary agent are put into a closed high-pressure resistant kettle according to a certain weight proportion, and the mixture is stirred continuously; heating the material in the kettle to 148-165 ℃ and filling CO 2 The pressure reaches 2.4-5.5MPa, and the pressure is kept for 5-30min; the dispersion is released into the low pressure zone to give expanded primary expanded polyolefin beads having a bulk density of from 46 to 80g/L.
(3) Sealing the primary foaming polyolefin beads into a pre-pressing tank after 12-24h of normal temperature health maintenance, carrying out pressure loading by air for 8-30h under the pressure of 0.2-0.5MPa, and heating and expanding the primary foaming beads after the pressure loading in a normal pressure circulation foaming pipeline at 80-95 ℃ to form a secondary foaming bead finished product with lighter density; bulk density is 12-45g/L.
The bulk density of the secondary foaming beads is generally 12-45g/L, and when the bulk density is lower than 12g/L, the foaming beads are extremely easy to break holes or lose use value; the bulk density of the primary expanded beads used to produce the secondary expanded beads is preferably 46 to 70g/L, with the primary beads having a lighter density being more likely to break the closed cell structure and the primary beads having a higher density being less likely to be secondarily expanded to a lighter density.
Preferably, the length of the blended particles is 1.5-2.5mm, and the single weight is 1.5-3mg; the dispersion medium is deionized water; the dispersing agent is silicate mineral powder, preferably kaolin, and has an average particle size of 0.1-2 mu m; the dispersing aid is an anionic surfactant and at least comprises sodium dodecyl benzene sulfonate.
Preferably, the components are as follows in parts by weight: 100 parts of resin particles, 150-200 parts of dispersing medium, 0.1-0.5 part of dispersing agent and 0.01-0.3 part of dispersing auxiliary agent.
The application has the following beneficial effects:
(1) The foaming polyolefin beads adopt 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 resulting expanded beads have excellent rigidity and excellent resilience, the bead molding sintering pressure is low (less than 0.12 MPa), and the molded article has little or no appearance of gaps and pits.
(2) The ethylene-alpha olefin random copolymer or block copolymer added in the crystalline polymer is a crystalline elastomer, can endow the blending material with better toughness, and the combined compatilizer containing the polystyrene with the peroxide bond at the side group is beneficial to the interfacial compatibility of the crystalline polymer and the polystyrene.
(3) The foam cell nucleating agent is sodium chloride and/or potassium chloride with the average particle size of 8-15 mu m, and the sodium chloride and/or potassium chloride with the special particle size has excellent water absorption and dispersibility, and is favorable for the expansibility of the foaming beads and the uniformity of the foam cells.
(4) The preparation method of the foaming polyolefin beads has the advantages of simple and environment-friendly process. The molded part prepared from the foaming beads has excellent rigidity and toughness, so that the fragile defect of EPS used parts is greatly improved, and the use rigidity is well reserved. The molding has a density of 18-22g/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 proportioned according to the following weight portions: 100 parts of resin particles, 150-200 parts of dispersing medium, 0.1-0.5 part of dispersing agent and 0.01-0.3 part of dispersing auxiliary agent.
(1) Adding 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 proportion, and forming a dispersing system under the continuous stirring action;
(2) Heating the dispersion system in the kettle to 148-165 deg.C foaming temperature, and charging certain amount of CO 2 The pressure is enabled to reach 2.4-5.5MPa, and the foaming time is kept for 5-30min; releasing the dispersion into a low pressure zone to obtain expanded primary expanded polyolefin beads having a bulk density of from 46 to 80g/L;
(3) If the foaming beads with lighter density are required to be obtained, the primary foaming beads with the bulk density of 46-70g/L are selected, after the normal temperature curing for 12-24 hours, the foaming beads are sealed into a prepressing tank, air is used for carrying pressure, the carrying pressure is 0.2-0.5MPa, the carrying pressure time is 8-30 hours, and the primary foaming beads after carrying pressure are heated and expanded in a normal pressure circulation foaming pipeline at 80-95 ℃ to form a secondary foaming bead finished product with lighter density; bulk density is 12-45g/L.
The steam molding process of the foaming beads comprises the following steps: filling the foamed particles subjected to the pre-pressing tank loading into a die cavity through a vacuum pipeline, expanding the beads and sintering the surfaces of the foamed particles under the action of high-temperature steam, and cooling and shaping the foamed particles through flowing water on the surface of the die to obtain the EPO molded part. The molded product needs further curing and shaping in a hot air curing chamber at 50-70 ℃ to obtain the 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 the mass percentages of the materials in Table 2 are shown.
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 copolymers | 15 |
The formulations of the compatilizers are shown in table 3, and the mass percentages of the substances in table 3 are shown.
TABLE 3 Table 3
| Compatibilizing agent | X1 | X2 | X3 | X4 | X5 |
| Polystyrene with peroxide bond on 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 each example and comparative example are shown in Table 4, and the materials in Table 4 are calculated as mass percentages.
TABLE 4 Table 4
The results of the performance test of the secondarily expanded beads obtained in each of the examples and comparative examples are shown in Table 5.
TABLE 5
Minimum forming 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 gaps 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.
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 had higher tensile strength and elongation at break. Fig. 1 is an SEM photograph of a cross section of the secondary expanded beads of example 4, and it can be seen that the prepared secondary expanded beads have high cell uniformity.
The crystalline polymer component of comparative example 1 was entirely an elastomer, which was theoretically advantageous for increasing the toughness of the material (the larger the tensile strength and elongation at break values were in a certain range, the better the toughness of the molded article), but the sintering strength of the expanded beads was relatively poor, and also resulted in a decrease in elongation at break. The crystalline polymer component of comparative example 2 was entirely linear low density polyethylene, relatively poor in toughness and reduced in elongation at break. The compatibilizing agent of comparative example 3 lacks the effect of polystyrene having peroxide bonds in the side groups, and the compatibility of the crystalline polymer phase and the polystyrene phase becomes poor, resulting in serious pits and gaps appearing in the appearance of molded articles, 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 severe pits and gaps appearing in the appearance of molded articles, and the tensile strength and elongation at break are significantly reduced.
The present embodiment is merely illustrative of the present application, and the present application is not limited thereto, and a worker can make various changes and modifications without departing from the scope of the technical idea of the present application. 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 claims.
Claims (7)
1. A foamed polyolefin bead characterized by: the foaming polyolefin beads at least comprise the following components in percentage by mass: 20-35% of crystalline polymer, 8-20% of compatilizer and the balance of polystyrene;
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 1800MPa;
the crystalline polymer comprises 50-85% of linear low density polyethylene and 15-50% of ethylene-alpha olefin random copolymer or block copolymer;
the melt index of the linear low density polyethylene is 3-10g/10min, and the melting point is 100-110 ℃; the melt index of the ethylene-alpha olefin random copolymer or the block copolymer is 2-10g/10min, and the melting point is 95-125 ℃;
the compatilizer comprises polystyrene with 30-50% of side groups containing peroxide bonds, and also 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.
2. The expanded polyolefin beads according to claim 1, wherein: the expanded polyolefin beads further comprise 0.01-5% of an auxiliary agent.
3. The expanded polyolefin beads according to claim 2, wherein: the auxiliary agent comprises 0.01-0.5% of a cell nucleating agent.
4. The expanded polyolefin beads of claim 3, 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.
5. A process for the preparation of expanded polyolefin beads according to claim 2, characterized in that: the method comprises the following steps:
(1) Mixing polystyrene, a crystalline polymer, a compatilizer and an auxiliary agent, extruding, wiredrawing and granulating to obtain blended particles;
(2) Adding the blended particles, a dispersing medium, a dispersing agent and a dispersing aid into a closed high-pressure resistant kettle according to a certain weight proportion, and continuously stirring; heating the material in the kettle to 148-165 ℃ and filling CO 2 The pressure reaches 2.4-5.5MPa, and the pressure is kept for 5-30min; releasing the dispersion into a low pressure zone to obtain expanded primary expanded polyolefin beads having a bulk density of from 46 to 80g/L;
(3) Sealing the primary foaming polyolefin beads into a pre-pressing tank after 12-24h of normal temperature health maintenance, carrying out pressure loading by air for 8-30h under the pressure of 0.2-0.5MPa, and carrying out thermal expansion on the carried primary foaming beads in a normal pressure circulation foaming pipeline at 80-95 ℃ to form a secondary foaming bead finished product with lighter density; bulk density is 12-45g/L.
6. The method of producing expanded polyolefin beads according to claim 5, wherein: the length of the blending particles is 1.5-2.5mm, and the single weight is 1.5-3mg; the dispersion medium is deionized water; the dispersing agent is silicate mineral powder, and the average particle size of the dispersing agent is 0.1-2 mu m; the dispersing aid is an anionic surfactant and at least comprises sodium dodecyl benzene sulfonate.
7. The method of producing expanded polyolefin beads according to claim 5, wherein: the weight portions of the components are as follows: 100 parts of resin particles, 150-200 parts of dispersing medium, 0.1-0.5 part of dispersing agent and 0.01-0.3 part of dispersing auxiliary agent.
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| US20110269858A1 (en) * | 2008-12-30 | 2011-11-03 | Basf Se | Elastic molded foam based on polyolefin/styrene polymer mixtures |
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