CN107674406B - Supercritical CO2Bio-based porous carbon material for foam materials - Google Patents
Supercritical CO2Bio-based porous carbon material for foam materials Download PDFInfo
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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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- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/0014—Use of organic additives
- C08J9/0042—Use of organic additives containing silicon
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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
- C08J9/0066—Use of inorganic compounding ingredients
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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
- C08J2203/08—Supercritical fluid
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- C—CHEMISTRY; METALLURGY
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2205/00—Foams characterised by their properties
- C08J2205/04—Foams characterised by their properties characterised by the foam pores
- C08J2205/044—Micropores, i.e. average diameter being between 0,1 micrometer and 0,1 millimeter
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- C—CHEMISTRY; METALLURGY
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2375/00—Characterised by the use of polyureas or polyurethanes; Derivatives of such polymers
- C08J2375/04—Polyurethanes
Abstract
The invention discloses supercritical CO2The foaming material is a bio-based porous carbon material. The thermoplastic polyurethane/carbon composite material comprises, by weight, 50-100 parts of Thermoplastic Polyurethane (TPU), 1-10 parts of bio-based porous carbon, 0.1-2 parts of a coupling agent and 0.1-2 parts of an antioxidant. The bio-based porous carbon material takes natural bamboos or bamboo shoots as raw materials, the preparation process is simple, large-scale industrial production can be realized, and the bio-based porous carbon can be uniformly dispersed in a TPU matrix and shows good dispersion form and interface compatibility. SEM scanning is carried out on the section of the foaming fiber composite material, and the result shows that the introduction of porous carbon can greatly increase the expandability of fine fibers (200 mu m), and the foaming range is remarkably increased; with the increase of the fiber diameter, for the fiber with the diameter of 500 mu m, the introduction of the porous carbon effectively reduces the size of the foam cells and improves the density of the foam cells, and the prepared thermoplastic elastomer/bio-based porous carbon foaming material has high use value and application prospect.
Description
Technical Field
The invention relates to the technical field of engineering material application, in particular to a bio-based porous carbon material for a supercritical CO2 foaming material and application thereof in supercritical CO2Application of the foaming material.
Background
The polymer foaming material has been widely applied to the fields of automobiles, aviation, packaging, buildings and the like due to the advantages of light weight, low cost, good rebound resilience and good buffering performance. At present, the foaming methods are various, such as extrusion foaming, injection molding foaming, intermittent foaming and the like. The polymer foam material mainly reduces the bulk density of the material and reduces the cost on the premise of not damaging the properties of the polymer foam material. Compared with non-foamed plastic, the density of the foamed polymer material is 5-95% lower than that of unfoamed material, the impact strength is 5 times higher than that of unfoamed material, the specific stiffness (rigidity/mass ratio) is 3-5 times higher than that of unfoamed material, and good mechanical properties are still maintained. In addition, microcellular foams offer exceptional mechanical properties due to their smaller cell size and uniformity of cell size compared to similarly dense macroreticular foams, and can be a direct replacement for traditional polymeric materials as well as metals and inorganic materials in many engineering applications.
Typical polymer foaming systems consist of a polymer (or polymer monomer), a blowing agent, a nucleating agent and other necessary additives (flame retardants, surfactants, catalysts, etc.), generally blowing agents being divided into two types: physical blowing agents and chemical blowing agents. Chemical blowing agents are generally reactive substances that produce a gas by a chemical reaction or thermal decomposition; physical blowing agents are typically volatile chemicals (hydrocarbons/alcohols), inert gases (carbon dioxide, nitrogen, argon, water). Among them, carbon dioxide is the best choice for environmental protection, and the gas has good motion ability and strong diffusivity, so the method of supercritical carbon dioxide foaming is widely concerned by researchers.
The TPU is characterized by high hardness, high strength, good elasticity, low temperature resistance, good oil resistance, chemical resistance and environmental resistance, and can be widely applied to adhesives, polymer molding, automobiles, electronic devices, sports goods, toys and the like. The high flexibility of TPUs even at low temperatures, good wear behavior and low compression set, which lead to a wide range of applications of TPUs in the automotive, chemical and medical industries. Therefore, many scholars or companies at home and abroad have a great interest in the research on the TPU foaming material.
Disclosure of Invention
The invention aims to provide supercritical CO2The foaming material is made of a biological porous carbon material, the biological porous carbon material is made of natural bamboos or bamboo shoots, the preparation process is simple, large-scale industrial production can be realized, and the prepared foaming composite material has excellent mechanical properties and a cellular structure.
The supercritical CO2The bio-based porous carbon material for the foaming material is characterized by comprising 50-100 parts by weight of Thermoplastic Polyurethane (TPU), 0.1-10 parts by weight of bio-based porous carbon, 0.1-2 parts by weight of coupling agent and 0.1-2 parts by weight of antioxidant.
The supercritical CO2The bio-based porous carbon material for the foaming material is characterized by comprising, by weight, 60-90 parts of Thermoplastic Polyurethane (TPU), 2-9 parts of bio-based porous carbon, 0.3-1.8 parts of a coupling agent and 0.3-1.8 parts of an antioxidant.
The supercritical CO2The bio-based porous carbon material for the foaming material is characterized by comprising 70-80 parts by weight of Thermoplastic Polyurethane (TPU), 3-6 parts by weight of bio-based porous carbon, 0.5-1.5 parts by weight of coupling agent and 0.5-1.5 parts by weight of antioxidant.
The supercritical CO2The bio-based porous carbon material for the foaming material is characterized in that the molecular weight of Thermoplastic Polyurethane (TPU) is 1000-6000.
The supercritical CO2The biological-based porous carbon material for the foaming material is characterized in that the biological-based porous carbon is one or two of bamboo carbon and bamboo shoot carbon, and the specific surface area of the carbon material is 100-3000 m2The preparation of bio-based porous carbon is disclosed in the patent application at 201610340621.3.
The supercritical CO2The bio-based porous carbon material for the foaming material is characterized in that the coupling agent is vinyl trichlorosilane, vinyl triethoxysilane, gamma-One or two of chloropropyltrichlorosilane, gamma-chloropropyltriethoxysilane, gamma-aminopropyltriethoxysilane and gamma- (2, 3-epoxypropoxy) propyltrimethoxysilane.
The supercritical CO2The bio-based porous carbon material for the foaming material is characterized in that the antioxidant is one or two of antioxidant 1010, antioxidant 1076, antioxidant 215 and antioxidant 225.
The supercritical CO2Bio-based porous carbon material for foam material in supercritical CO2The application of the foaming material, in particular to the application of the porous bamboo carbon material of the invention as an adsorbent and heterogeneous nucleating agent of CO2, promotes the formation of cells, controls the quantity of the cells and can be directly used by foaming.
By adopting the technology, compared with the prior art, the invention has the following beneficial effects: the bio-based porous carbon raw material adopts natural bamboo or bamboo shoots, the processing technology is simple, and the specific surface area of the obtained porous carbon material is 600-3000 m2The filler can be uniformly dispersed in a Thermoplastic Polyurethane (TPU) matrix, and can show good dispersion form and interface compatibility, the storage modulus and the loss modulus of the composite material obtained by dynamic rheological analysis are increased along with the increase of the content of the bio-based carbon material, the effect of 3 parts is optimal, and the filler has the same rule on the mechanical property of the composite material; the storage modulus and loss modulus of the TPU composite material directly influence the processing and performance of the TPU composite material during processing and use. Therefore, in the detection and the description, the analysis result is added; bamboo charcoal is also an additive as a foaming agent, the content of the bamboo charcoal is increased, the storage modulus and the loss modulus of the bamboo charcoal are increased, the maximum value is reached at 3 parts, and the mechanical property (mainly tensile strength) is also the maximum at 3 parts.
Supercritical CO of the invention2Bio-based porous carbon material for foam material in supercritical CO2The research result of supercritical carbon dioxide foaming of the composite material shows that the introduction of the bio-based carbon material can greatly increase the expandability of TPU fine fibers (200 mu m), and the foaming range is remarkably increased; for TPU fibres with a diameter of 500 μm, of grapheneThe introduction of the graphene effectively reduces the cell size and increases the cell density, the cell size is reduced from 3.78 mu m to 1.97 mu m by introducing 5 wt% of the graphene, and the cell density is reduced from 4.93 × 109cells/cm3Increased to 2.42 × 1010cells/cm3Meanwhile, the influence of different temperatures, pressures and filler types on foaming is also researched, the composite material is between 80 ℃ and 125 ℃, the higher temperature is more beneficial to foaming, and the higher temperature enables the strength of the polymer to be reduced, so that the nucleation and growth of foam cells are facilitated; the foaming is facilitated by higher pressure between 8 MPa and 13.8 MPa, more carbon dioxide can be dissolved by high pressure, more nucleation points are provided, the viscosity of the polymer is reduced, and the growth of foam pores is facilitated.
Drawings
FIG. 1 is a scanning electron microscope image of a bio-based porous carbon material according to the present invention;
FIG. 2 is a transmission electron microscope image of the bio-based porous carbon material prepared in example 3 on a TPU material;
FIG. 3 is a comparison graph of the foaming ranges of TPU/G foams with different contents of bio-based porous carbon materials prepared in examples;
FIG. 4 is a graph showing the comparison of the cell sizes of TPU/G foams with different contents of bio-based porous carbon materials prepared in examples;
FIG. 5 is a statistical chart of the cell density of TPU/G foam materials with different contents of bio-based porous carbon materials prepared in examples.
Detailed Description
In order to better understand the present invention, the following examples are further provided to illustrate the present invention, but the present invention is not limited to the following examples.
Example 1:
supercritical CO2The bio-based porous carbon material for the foaming material comprises, by weight, 100 parts of Thermoplastic Polyurethane (TPU), 0.5 part of bio-based porous carbon, 0.2 part of coupling agent and 0.2 part of antioxidant.
The molecular weight of the thermoplastic polyurethane TPU is 2915.
The bio-based porous carbon is bamboo carbon, and the specific surface area of the carbon material is 2000m2/g。
The coupling agent is gamma- (2, 3-epoxypropoxy) propyl trimethoxy silane.
The antioxidant is 225.
Fully dissolving dried Thermoplastic Polyurethane (TPU) particles into DMF (dimethyl formamide), adding a bio-based carbon material G, performing ultrasonic treatment to obtain better dispersion to obtain uniform mixed liquor, pouring the mixed liquor into ice methanol to separate out a TPU/G composite material, and drying to prepare a bio-based porous carbon material (TPU/G composite material for short) for the supercritical CO2 foam material. Extruding the prepared composite material by an SJSZ-07A miniature double-screw extruder at the extrusion temperature of 195 ℃, 195 ℃, 200 ℃ and 200 ℃ to prepare the TPU/G composite material fiber with the diameter of 200 mu m. And (2) carrying out supercritical carbon dioxide microcellular foaming on the composite fiber by an intermittent foaming method, wherein the foaming temperature is 125 ℃, the saturation pressure is 13.8 MPa, the foaming time is 12h, the pressure relief time is 0.1S, stabilizing for 5S after pressure relief, and putting into ice water for cooling to obtain the TPU/G foamed composite material.
Example 2:
supercritical CO2The bio-based porous carbon material for the foaming material comprises, by weight, 100 parts of Thermoplastic Polyurethane (TPU), 1 part of bio-based porous carbon, 0.2 part of coupling agent and 0.2 part of antioxidant.
The molecular weight of the thermoplastic polyurethane TPU is 2915.
The bio-based porous carbon is bamboo carbon, and the specific surface area of the carbon material is 2000 m2/g。
The coupling agent is gamma- (2, 3-epoxypropoxy) propyl trimethoxy silane.
The antioxidant is 225.
Fully dissolving dried Thermoplastic Polyurethane (TPU) particles into DMF (dimethyl formamide), adding a bio-based carbon material G, performing ultrasonic treatment to obtain better dispersion, obtaining uniform mixed liquor, pouring the mixed liquor into ice methanol, separating out a TPU/G composite material, and drying to prepare the TPU/G composite material. Extruding the prepared composite material by an SJSZ-07A miniature double-screw extruder at the extrusion temperature of 195 ℃, 195 ℃, 200 ℃ and 200 ℃ to prepare the TPU/G composite material fiber with the diameter of 200 mu m. And (2) carrying out supercritical carbon dioxide microcellular foaming on the composite fiber by an intermittent foaming method, wherein the foaming temperature is 125 ℃, the saturation pressure is 13.8 MPa, the foaming time is 12h, the pressure relief time is 0.1S, stabilizing for 5S after pressure relief, and putting into ice water for cooling to obtain the TPU/G foamed composite material.
Example 3:
supercritical CO2The bio-based porous carbon material for the foaming material comprises, by weight, 100 parts of Thermoplastic Polyurethane (TPU), 3 parts of bio-based porous carbon, 0.2 part of coupling agent and 0.2 part of antioxidant.
The molecular weight of the thermoplastic polyurethane TPU is 2915.
The bio-based porous carbon is bamboo carbon, and the specific surface area of the carbon material is 2000 m2/g。
The coupling agent is gamma-aminopropyl triethoxysilane.
The antioxidant is 225.
Fully dissolving dried Thermoplastic Polyurethane (TPU) particles into DMF (dimethyl formamide), adding a bio-based carbon material G, performing ultrasonic treatment to obtain better dispersion, obtaining uniform mixed liquor, pouring the mixed liquor into ice methanol, separating out a TPU/G composite material, and drying to prepare the TPU/G composite material. Extruding the prepared composite material by an SJSZ-07A miniature double-screw extruder at the extrusion temperature of 195 ℃, 195 ℃, 200 ℃ and 200 ℃ to prepare the TPU/G composite material fiber with the diameter of 200 mu m. Supercritical carbon dioxide microcellular foaming is carried out on the composite fiber by an intermittent foaming method, the foaming temperature is 125 ℃, the saturation pressure is 13.8 MPa, the foaming time is 12 hours, the pressure relief time is 0.1S, after the pressure relief, the composite fiber is stabilized for 5S, the composite fiber is put into ice water to be cooled, and the TPU/G foamed composite material is obtained.
Example 4:
supercritical CO2The bio-based porous carbon material for the foaming material comprises, by weight, 100 parts of Thermoplastic Polyurethane (TPU), 5 parts of bio-based porous carbon, 0.2 part of coupling agent and 0.2 part of antioxidant.
The molecular weight of the thermoplastic polyurethane TPU is 2915.
The bio-based porous carbon is bamboo carbon, and the specific surface area of the carbon material is 2000 m2/g。
The coupling agent is gamma- (2, 3-epoxypropoxy) propyl trimethoxy silane.
The antioxidant is 225.
Fully dissolving dried Thermoplastic Polyurethane (TPU) particles into DMF (dimethyl formamide), adding a bio-based carbon material G, performing ultrasonic treatment to obtain better dispersion, obtaining uniform mixed liquor, pouring the mixed liquor into ice methanol, separating out a TPU/G composite material, and drying to prepare the TPU/G composite material. Extruding the prepared composite material by an SJSZ-07A miniature double-screw extruder at the extrusion temperature of 195 ℃, 195 ℃, 200 ℃ and 200 ℃ to prepare the TPU/G composite material fiber with the diameter of 200 mu m. And (2) carrying out supercritical carbon dioxide microcellular foaming on the composite fiber by an intermittent foaming method, wherein the foaming temperature is 125 ℃, the saturation pressure is 13.8 MPa, the foaming time is 12h, the pressure relief time is 0.1S, stabilizing for 5S after pressure relief, and putting into ice water for cooling to obtain the TPU/G foamed composite material.
In the embodiment, the coupling agent is one or two of vinyltrichlorosilane, vinyltriethoxysilane, gamma-chloropropyltrichlorosilane, gamma-chloropropyltriethoxysilane, gamma-aminopropyltriethoxysilane and gamma- (2, 3-glycidoxy) propyltrimethoxysilane instead of gamma- (2, 3-glycidoxy) propyltrimethoxysilane, and one or two of 1010, 1076, 215 and 225 as the antioxidant instead of the antioxidant 225, so that the same technical effect can be achieved.
The results of the measurements of the foamed material of the present example are shown in FIGS. 3, 4 and 5. It can be seen that, under the same magnification, as the content of the bio-based porous carbon increases, the foaming range gradually increases, and the increase of the content of the porous carbon also leads to the increase of the self expansion degree of the fiber, because after the porous carbon is added, the porous carbon has a barrier effect on the diffusion of carbon dioxide, the increase of the content of the porous carbon can prolong the diffusion time of carbon dioxide, which is more beneficial to the formation of cells, and the porous carbon also has a heterogeneous nucleation effect in a system, the energy barrier required to be overcome by nucleation is significantly reduced compared with homogeneous nucleation, the foaming effect can be significantly improved, and as the content of the porous carbon increases, the effect is more obvious, to sum up, the high barrier effect and the nucleation effect of the porous carbon both lead to the increase of the heterogeneous foaming range and the increase of the material expansion degree, but the addition amount is too much, which leads to the increase of, therefore, when the result of the bamboo carbon filling amount of the experiment is 3 parts, the comprehensive performance of the composite material is optimal.
The statistical figures 4 and 5 of the sizes and the densities of the pores of the TPU/G composite material with different porous carbon contents can be more intuitively seen, the size of the pores is reduced from 1.45 mu m to 1.24 mu m by adding 0.5 wt% of the porous carbon, and the density of the pores is reduced from 7.32 × 109cells/cm3Increased to 1.28 × 1010cells/cm3This is because the graphene is added to perform heterogeneous nucleation, the nanoparticles provide a large number of nucleation sites to nucleate the cells almost simultaneously, the effective gas for growing a single bubble becomes small, the cell size becomes small, the cell density increases, when the porous carbon content increases from 0.5 wt% to 5 wt%, the cell size increases from 1.24 μm to about 1.8 μm, and the cell density remains substantially unchanged, because the heterogeneous nucleation still exists with the increase of the porous carbon content, but because the fiber diameter of the composite material is small (200 μm), the diffusion speed of carbon dioxide is very fast, the porous carbon has a high barrier effect for the diffusion of carbon dioxide, and the higher the content is, the more significant the barrier effect is, so that the porous carbon can more easily enter the gas core, and the cells are increased. The results of comprehensive foaming and mechanical property data show that the TPU composite material added with 3 wt% of porous carbon has the best size and quantity results, and the TPU composite material has moderate energy storage and loss modulus and is suitable for industrial mass production.
Claims (7)
1. Supercritical CO2The bio-based porous carbon material for the foaming material is characterized by comprising 50-100 parts by weight of Thermoplastic Polyurethane (TPU), 0.1-10 parts by weight of bio-based porous carbon, 0.1-2 parts by weight of coupling agent and 0.1-2 parts by weight of antioxidant; the bio-based porous carbon is one or two of bamboo carbon and bamboo shoot carbon, and the specific surface area of the carbon material is 100-3000m2/g。
2. A supercritical CO according to claim 12The bio-based porous carbon material for the foaming material is characterized by comprising, by weight, 60-90 parts of Thermoplastic Polyurethane (TPU), 2-9 parts of bio-based porous carbon, 0.3-1.8 parts of a coupling agent and 0.3-1.8 parts of an antioxidant.
3. A supercritical CO according to claim 12The bio-based porous carbon material for the foaming material is characterized by comprising 70-80 parts by weight of Thermoplastic Polyurethane (TPU), 3-6 parts by weight of bio-based porous carbon, 0.5-1.5 parts by weight of coupling agent and 0.5-1.5 parts by weight of antioxidant.
4. A supercritical CO according to claim 12The bio-based porous carbon material for the foaming material is characterized in that the molecular weight of Thermoplastic Polyurethane (TPU) is 1000-6000.
5. A supercritical CO according to claim 12The biological porous carbon material for the foaming material is characterized in that the coupling agent is one or two of vinyl trichlorosilane, vinyl triethoxysilane, gamma-chloropropyl trichlorosilane, gamma-chloropropyl triethoxysilane, gamma-aminopropyl triethoxysilane and gamma- (2, 3-epoxypropoxy) propyl trimethoxysilane.
6. A supercritical CO according to claim 12The bio-based porous carbon material for the foaming material is characterized in that the antioxidant is one or two of antioxidant 1010, antioxidant 1076, antioxidant 215 and antioxidant 225.
7. Supercritical CO according to claim 12Bio-based porous carbon material for foam material in supercritical CO2Application in foaming materials.
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| CN110951035A (en) * | 2019-12-27 | 2020-04-03 | 福建安达福新材料科技有限公司 | Polyurethane foam material based on supercritical carbon dioxide and preparation method thereof |
| CN111205628A (en) * | 2020-02-27 | 2020-05-29 | 陕西科技大学 | Porous carbon modified waterborne polyurethane material and preparation method thereof |
| CN111393759A (en) * | 2020-04-02 | 2020-07-10 | 福建安达福新材料科技有限公司 | Polystyrene foam material based on supercritical fluid and preparation method thereof |
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