WO2021017580A1 - Matériau en mousse de polystyrène léger à petit diamètre de pore et son procédé de préparation - Google Patents

Matériau en mousse de polystyrène léger à petit diamètre de pore et son procédé de préparation Download PDF

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WO2021017580A1
WO2021017580A1 PCT/CN2020/090998 CN2020090998W WO2021017580A1 WO 2021017580 A1 WO2021017580 A1 WO 2021017580A1 CN 2020090998 W CN2020090998 W CN 2020090998W WO 2021017580 A1 WO2021017580 A1 WO 2021017580A1
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polystyrene
polydimethylsiloxane
preparation
foaming
pressure
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PCT/CN2020/090998
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English (en)
Chinese (zh)
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赵玲
胡冬冬
强薇
刘涛
姚舜
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华东理工大学
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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
    • 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
    • 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
    • C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
    • C08J9/0014—Use of organic additives
    • C08J9/0023—Use of organic additives containing oxygen
    • 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
    • C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
    • C08J9/0061—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof characterized by the use of several polymeric components
    • 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
    • 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
    • C08J9/127—Mixtures of organic and inorganic blowing agents
    • 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
    • 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
    • C08J9/14—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 organic
    • C08J9/141—Hydrocarbons
    • 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
    • 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
    • C08J9/14—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 organic
    • C08J9/142—Compounds containing oxygen but no halogen atom
    • 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
    • C08J2203/00—Foams characterized by the expanding agent
    • C08J2203/06—CO2, N2 or noble gases
    • 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
    • C08J2203/00—Foams characterized by the expanding agent
    • C08J2203/08—Supercritical fluid
    • 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
    • C08J2203/00—Foams characterized by the expanding agent
    • C08J2203/12—Organic compounds only containing carbon, hydrogen and oxygen atoms, e.g. ketone or alcohol
    • 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
    • C08J2203/00—Foams characterized by the expanding agent
    • C08J2203/14—Saturated hydrocarbons, e.g. butane; Unspecified hydrocarbons
    • 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
    • C08J2203/00—Foams characterized by the expanding agent
    • C08J2203/18—Binary blends of expanding agents
    • C08J2203/182—Binary blends of expanding agents of physical blowing agents, e.g. acetone and butane
    • 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
    • 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
    • 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
    • C08J2483/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers
    • C08J2483/04—Polysiloxanes

Definitions

  • the invention relates to a polystyrene foam material and a preparation method thereof.
  • Polystyrene (PS) is an amorphous polymer with extremely high transparency, good electrical insulation, easy processing, and low cost. Because of these excellent characteristics, polystyrene foam products are widely used in food packaging, building insulation, product cushioning and shielding materials and other fields.
  • the main fluorine-containing physical blowing agents in the polystyrene foaming industry in my country such as hydrochlorofluorocarbons (HCFC), hydrofluorocarbons (HFC) and hydrocarbons (HC), are due to their solubility in polymers It is high and the foaming process spreads slowly, and the obtained polystyrene foamed product has a higher magnification.
  • pro-CO 2 additives such as fluorine-containing silicon-containing polymers, which can improve the interaction between the polymer matrix and CO 2 , thereby enhancing the cell density of the foamed material, but adding a nucleating agent separately Can not significantly increase the expansion ratio of the foaming material;
  • pro-CO 2 additives such as fluorine-containing silicon-containing polymers
  • the technical problem to be solved by the present invention is to overcome the prior art in the process of preparing polystyrene material by supercritical CO 2 foaming, the solubility of CO 2 in polystyrene is low, and the diffusion is fast, and the obtained polystyrene material has a pore size
  • the invention provides a polystyrene foam material and a preparation method thereof.
  • the preparation method has a simple process, does not produce bad smell and by-products, is good for the environment, and the additives are safe and environmentally friendly, and meet the development needs of related fields.
  • the polystyrene foam material has a large nucleation density, a small cell diameter, a large expansion ratio, and is environmentally friendly.
  • the invention provides a method for preparing a polystyrene foam material, which comprises the following steps: blending polystyrene and polydimethylsiloxane to obtain a polystyrene/polydimethylsiloxane blend ⁇ ;
  • the polystyrene / polydimethylsiloxane blend can be foamed under supercritical CO 2 conditions; wherein, the polydimethylsiloxane number molecular weight can be 2000g/mol ⁇ 17000g/mol.
  • the molecular weight of the polydimethylsiloxane is preferably 2000 g/mol to 6000 g/mol, more preferably 2000 g/mol.
  • the content of the polydimethylsiloxane in the polystyrene/polydimethylsiloxane blend may be 0.5 to 1.5% by weight, preferably 1% by weight.
  • the polystyrene material may be conventional in the field, and preferably is Yangzi BASF Petrochemical 158K general-purpose polystyrene.
  • the operation and conditions of the blending can be conventional in the art, and the blending is generally performed in a hack internal mixer conventional in the art.
  • the blending temperature is preferably 170-180°C, more preferably 170°C.
  • the blending time is preferably 15 to 20 minutes, more preferably 15 minutes.
  • the rotor speed in the blending is preferably 80-100 revolutions/min, more preferably 100 revolutions/min.
  • the polystyrene/polydimethylsiloxane blend may be a sheet.
  • the foaming under supercritical CO 2 conditions is carried out according to the following steps: placing the polystyrene/polydimethylsiloxane blend in an autoclave and filling CO 2 with replacement air three times; The autoclave is heated to the foaming temperature, and after holding for half an hour, it is filled with supercritical CO 2 to set the pressure to saturate the polystyrene/polydimethylsiloxane blend; then the pressure is relieved, A polystyrene foam material is obtained.
  • the heating can be a conventional program temperature controlled heating in the field, and the heating rate can be 8-12°C/min, preferably 10°C/min.
  • the foaming temperature may be 105-115°C, preferably 110°C.
  • the pressure of the supercritical CO 2 may be 14-15 MPa, preferably 15 MPa.
  • the saturation means that CO 2 reaches a dissolution equilibrium inside the matrix of the polystyrene/polydimethylsiloxane blend, and the saturation time can be 1 to 2 hours, preferably 2h.
  • the operation and conditions of the pressure relief can be conventional in the art, and the average rate of the pressure relief is preferably 500-600 MPa/s, more preferably 500 MPa/s.
  • the preparation method of the polystyrene foam material further comprises: adding to the polystyrene/polydimethylsiloxane blend before the foaming under supercritical CO 2 conditions Step of adding co-blowing agent.
  • the co-blowing agent may be absolute ethanol or n-pentane, wherein the purity of the n-pentane is >99.8%, preferably absolute ethanol.
  • the added amount of the co-blowing agent is 5-7 wt% of the supercritical CO 2 under the foaming temperature and pressure, preferably 5 wt%.
  • the present invention also provides a preparation method of polystyrene foam material, which comprises the following steps: after adding a co-blowing agent to polystyrene, foaming is done under supercritical CO 2 conditions.
  • the co-blowing agent may be absolute ethanol or n-pentane, wherein the purity of the n-pentane is >99.8%, preferably absolute ethanol.
  • the added amount of the co-blowing agent is 5-7 wt% of the supercritical CO 2 under the foaming temperature and pressure, preferably 5 wt%.
  • the foaming under supercritical CO 2 conditions is carried out as follows: the polystyrene and co-blowing agent are placed in an autoclave, filled with CO 2 to replace air three times; and the autoclave After heating to the foaming temperature and keeping it warm for half an hour, it is filled with supercritical CO 2 to set the pressure to saturate the polystyrene; then the pressure is released to obtain a polystyrene foam material.
  • the heating can be a conventional program temperature controlled heating in the field, and the heating rate can be 8-12°C/min, preferably 10°C/min.
  • the foaming temperature may be 105-115°C, preferably 110°C.
  • the pressure of the supercritical CO 2 may be 14-15 MPa, preferably 15 MPa.
  • the saturation means that CO 2 reaches a dissolution equilibrium inside the matrix of the polystyrene/polydimethylsiloxane blend, and the saturation time can be 1 to 2 hours, preferably 2h.
  • the operation and conditions of the pressure relief can be conventional in the art, and the average rate of the pressure relief is preferably 500-600 MPa/s, more preferably 500 MPa/s.
  • the invention also provides a polystyrene/polydimethylsiloxane blend, which is composed of the following components in mass fractions: 98.5-99.5wt% polystyrene and 0.5-1.5wt% polydimethylsiloxane Siloxane;
  • the polydimethylsiloxane has a number-weight molecular weight of 2000 g/mol to 17000 g/mol, preferably 2000 g/mol to 6000 g/mol, more preferably 2000 g/mol.
  • the invention also provides a polystyrene foam material prepared by the preparation method of the polystyrene foam material of the invention.
  • the cell diameter of the polystyrene foam material is less than 12 ⁇ m, preferably less than 9 ⁇ m; the cell expansion ratio is greater than 8 times, preferably greater than 11 times; the nucleation density is greater than 8.75 ⁇ 10 9 cells /cm 3 , preferably greater than 10.1 ⁇ 10 9 cells/cm 3 .
  • the reagents and raw materials used in the present invention are all commercially available.
  • the present invention adopts simple blending to prepare foaming samples, the process is simple, no bad smell and by-products are generated, it is good for the environment, and the additives are safe and environmentally friendly;
  • the obtained polystyrene foam material has the advantages of high foaming nucleation density, large foaming ratio, small cell diameter, etc. .
  • Figure 1 is a cross-sectional electron micrograph of the polystyrene foam product obtained in Example 1 of the present invention
  • Example 2 is a cross-sectional electron micrograph of a polystyrene foam product obtained in Example 2 of the present invention
  • Example 3 is a cross-sectional electron micrograph of the polystyrene foam product obtained in Example 3 of the present invention.
  • Example 4 is a cross-sectional electron microscope view of the polystyrene foam product obtained in Example 4 of the present invention.
  • Example 5 is a cross-sectional electron micrograph of a polystyrene foam product obtained in Example 5 of the present invention.
  • Example 6 is a cross-sectional electron micrograph of a polystyrene foam product obtained in Example 6 of the present invention.
  • Figure 7 is an electron micrograph of a cross-section of a polystyrene foam product obtained in Example 7 of the present invention.
  • Figure 9 is an electron micrograph of a cross-section of a polystyrene foam product obtained in Comparative Example 2 of the present invention.
  • Figure 11 is an electron micrograph of a cross-section of the polystyrene foamed product obtained in Comparative Example 4 of the present invention.
  • the polystyrene particles and polydimethylsiloxane are melt-blended through a Farm internal mixer, and after adding a co-blowing agent, they are foamed intermittently through an autoclave to obtain the desired foaming ratio and foam Polystyrene foam product with cell density and cell diameter.
  • the content of polydimethylsiloxane is 1wt%
  • the blending temperature is 170 °C
  • the blending time is 15 minutes
  • the torque speed is 100 revolutions/min
  • the blending obtains a polystyrene/polydimethylsiloxane blend.
  • the content of polydimethylsiloxane is 1wt%
  • the blending temperature is 170 °C
  • the blending time is 15 minutes
  • the torque speed is 100 revolutions/min
  • the blending obtains a polystyrene/polydimethylsiloxane blend.
  • the content of polydimethylsiloxane is 1wt%
  • the blending temperature is 170 °C
  • the blending time is 15 minutes
  • the torque speed is 100 revolutions/min
  • the blending obtains a polystyrene/polydimethylsiloxane blend.
  • the blend Place the blend in an autoclave, add the co-blowing agent n-pentane, add 5wt% of the mass of CO 2 at the experimental temperature and pressure, fill with CO 2 to replace air three times, and then program the autoclave for temperature control and heating.
  • the rate is 10°C/min, heated to a foaming temperature of 110°C, after holding for half an hour, filled with high-pressure CO 2 , the pressure is controlled to 15MPa, the blend is saturated for 2h, and then the pressure is quickly released.
  • the pressure release rate is 500MPa/ s, to obtain a microcellular foam material.
  • the content of polydimethylsiloxane is 1wt%
  • the blending temperature is 170 °C
  • the blending time is 15 minutes
  • the torque speed is 100 revolutions/min
  • the blending obtains a polystyrene/polydimethylsiloxane blend.
  • the blend was placed in an autoclave, filled with CO 2 to replace air three times, and then the autoclave was heated by programmed temperature control at a heating rate of 10°C/min, heated to a foaming temperature of 110°C, and after holding for half an hour, filled High-pressure CO 2 , the pressure is controlled to 15 MPa, the blend is saturated for 2 hours, and then the pressure is quickly relieved at a pressure relief rate of 500 MPa/s to obtain a microcellular foam material.
  • the content of polydimethylsiloxane is 1wt%
  • the blending temperature is 170 °C
  • the blending time is 15 minutes
  • the torque speed is 100 revolutions/min
  • the blending obtains a polystyrene/polydimethylsiloxane blend.
  • the blend was placed in an autoclave, filled with CO 2 to replace air three times, and then the autoclave was heated by programmed temperature control at a heating rate of 10°C/min, heated to a foaming temperature of 110°C, and after holding for half an hour, filled High-pressure CO 2 , the pressure is controlled to 15 MPa, the blend is saturated for 2 hours, and then the pressure is quickly relieved at a pressure relief rate of 500 MPa/s to obtain a microcellular foam material.
  • the addition amount is 5wt% of the CO 2 mass under the experimental temperature and pressure, fill with CO 2 to replace the air three times, and then program the autoclave to control the temperature Heating at a heating rate of 10°C/min, heating to a foaming temperature of 110°C, after holding for half an hour, fill with high-pressure CO 2 and control the pressure to 15MPa to saturate the blend for 2h, and then perform rapid pressure relief. It is 500MPa/s to obtain a microcellular foam material.
  • the polystyrene raw material and polyvinyl acetate (with a molecular weight of 17000g/mol) are put into a Hacker mixer and blended.
  • the content of polyvinyl acetate is 1wt%
  • the blending temperature is 180°C
  • the blending time is 10min
  • the torque speed is 100 revolutions/min, blending to obtain a polystyrene/polyvinyl acetate blend.
  • the blend was placed in an autoclave, filled with CO 2 to replace air three times, and then the autoclave was heated by programmed temperature control at a heating rate of 10°C/min, heated to a foaming temperature of 110°C, and after holding for half an hour, filled High-pressure CO 2 , the pressure is controlled to 15 MPa, the blend is saturated for 2 hours, and then the pressure is quickly relieved at a pressure relief rate of 500 MPa/s to obtain a microcellular foam material.
  • the polystyrene raw material placed in an autoclave, add the co-blowing agent acetone, the addition amount is 5wt% of the mass of CO 2 at the experimental temperature and pressure, fill with CO 2 to replace the air three times, and then program the autoclave to control temperature and heat.
  • the heating rate is 10°C/min, and the foaming temperature is 110°C. After holding for half an hour, it is filled with high-pressure CO 2 and the pressure is controlled to 15 MPa to saturate the blend for 2 hours, and then perform rapid pressure relief.
  • the pressure relief rate is 500 MPa /s to obtain a microcellular foam material.

Abstract

L'invention concerne un procédé de préparation d'un matériau en mousse de polystyrène comprenant les étapes suivantes consistant à : mélanger un polystyrène et un polydiméthylsiloxane pour obtenir un mélange polystyrène/polydiméthylsiloxane ; et faire mousser le mélange polystyrène/polydiméthylsiloxane dans des conditions de CO2 supercritique, le poids moléculaire moyen en nombre du polydiméthylsiloxane pouvant être compris entre 2 000 g/mol et 17 000 g/mol. Le procédé de préparation est simple à mettre en œuvre, ne produit pas d'odeurs désagréables ni de sous-produits, est écologique, utilise des additifs sans danger et respectueux de l'environnement, et répond aux exigences de développements dans des domaines apparentés. Le matériau en mousse de polystyrène présente une densité de nucléation élevée, un petit diamètre de cellules de mousse et un taux de moussage élevé, et est respectueux de l'environnement.
PCT/CN2020/090998 2019-08-01 2020-05-19 Matériau en mousse de polystyrène léger à petit diamètre de pore et son procédé de préparation WO2021017580A1 (fr)

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CN111138773A (zh) * 2019-08-01 2020-05-12 华东理工大学 一种具有小孔径的轻量聚苯乙烯发泡材料及其制备方法
CN111825877B (zh) * 2020-07-22 2023-03-14 华东理工大学 聚丙烯发泡材料及其制备方法
CN112210113B (zh) * 2020-10-21 2022-11-15 华东理工大学 聚丙烯发泡材料及其制备方法

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