CN112876824A - Degradable PBST/PPC composite foaming material and preparation method thereof - Google Patents
Degradable PBST/PPC composite foaming material and preparation method thereof Download PDFInfo
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- C08J9/104—Hydrazines; Hydrazides; Semicarbazides; Semicarbazones; Hydrazones; Derivatives thereof
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Abstract
The invention relates to the technical field of foaming materials, in particular to a degradable PBST/PPC composite foaming material and a preparation method thereof. The composite foaming material is prepared from the following raw materials in parts by weight: 100 parts of a polymer; 0.5-3 parts of a chain extender; 0.5-3 parts of an end-capping agent; 0.5-5 parts of a nucleating agent; 0.5-2 parts of a foaming agent; 0.1-3 parts of a plasticizer; the polymer comprises polybutylene terephthalate succinate and polypropylene carbonate. According to the invention, a chain extender is adopted to carry out chain extension on a specific polymer, an end capping agent is adopted to carry out end capping, and other raw materials are matched for synergistic effect, after extrusion processing, a main chain in an obtained material system contains functional fragments, an interpenetrating network structure is formed, chain entanglement is generated, the melt strength of the system is increased, the melt index of the system is improved, and the finally obtained composite foam material has the advantages of excellent tensile property, high melt index of the system and excellent foaming property.
Description
Technical Field
The invention relates to the technical field of foaming materials, in particular to a degradable PBST/PPC composite foaming material and a preparation method thereof.
Background
The foaming composite material is a composite material which takes plastic as a basic component and contains a large amount of gas structures. The doctor of Changchun's republic of Han Changyu jade expounds the distinction between common foamed plastic and microporous foamed plastic in his doctor's thesis, the strength of foamed composite material in China is low, and the variety and quality of foamed composite material need to be greatly improved. The microcellular foam material can improve the mechanical property of the plastic foam body, simultaneously, the mechanical property of the matrix can not be reduced under the condition of reducing the density of the material, and the microcellular foam material can also improve the impact strength, the toughness and the fatigue life, and has the functions of heat insulation, sound insulation, shock absorption and the like, thereby expanding the application range of the microcellular foam material. In recent years, with the consideration of cost performance, environmental pollution, recycling and other factors, the micro-foaming composite material becomes a novel material with great development potential.
The current foam materials are mainly made of polyethylene, polystyrene, etc. The waste of these materials is difficult to decompose, which brings certain negative effects to the environment, especially because of the large volume, the pollution to the environment is not negligible. Solving the problem of white pollution is a problem which is generally concerned by people. The biodegradable plastic has the characteristics of exerting the excellent performance of the plastic when in use, causing no pollution to the environment when being discarded after use and being rapidly decomposed by various organisms (enzymes). Therefore, the method for treating both symptoms and root causes is the method for vigorously developing and popularizing the environment biodegradable high polymer material, and also conforms to the trend of greening the high polymer material at present.
The doctor Han dichroa, Changchun strain, develops the foam material of polylactic acid, polycaprolactone and a blending system thereof, and theoretically researches the quantitative relation between the melt viscosity of the resin and the processing of the foam material. The research on the structure and the performance of poly epsilon-caprolactone (PCL) foam plastic and polybutylene succinate (PBS) foam plastic is developed by Lihao doctor in sequence. Both studies are high foaming composites.
Chenqiao and guoslong provided a biodegradable aliphatic polycarbonate foam material and a preparation method thereof in a patent of published invention CN108192311A, and a biodegradable PBAT foam material and a preparation method thereof in a patent CN108264736A, wherein the Chenqiao and guoslong adopt a three-step method to prepare three hot melts in the two patents, and then the three hot melts are finally mixed and extruded to obtain a molecular structure such as a DNA sequence structure, thereby realizing continuous stability and controllability of operation time, temperature window and foam material physical properties. The group of research in Mengzhou of Zhongshan university reported that PPC/CaCO was prepared using AC as blowing agent and ZnO as co-blowing agent3In J Polym Res, PPC foam composite materials are prepared by using N, N' -Dinitrosopentamethylenetetramine (DPT) as a foaming agent and urea as a co-foaming agent. The king red topic group of the research institute of chemistry for application of Changchun takes ADR-4368 as a chain extender, and adopts a supercritical method to prepare the foaming composite material of a PBAT/PPC blending system.
However, the methods for preparing the foamed materials provided by the above patents are difficult to develop industrially, and most of the high molecular foamed materials are petroleum-based products, which are one of the major sources of environmental hazards after consumption, especially for packaging. The main factors causing harm are that the foam plastic is light in weight and large in volume, and is difficult to recycle after use. The animal feed is discarded in the environment and can not be digested by the environment, the animal feed by mistake can cause damage and even death, and the canal is blocked. Therefore, in order to solve the above environmental problems, we have developed a biodegradable foamed composite material in an attempt to replace currently used foams such as polystyrene foam, polyethylene foam and polyurethane foam, and alleviate the environmental pollution pressure.
Disclosure of Invention
In view of the above, the technical problem to be solved by the present invention is to provide a degradable PBST/PPC composite foam material and a preparation method thereof, wherein the composite foam material has excellent physical properties.
The invention provides a degradable PBST/PPC composite foaming material which is prepared from the following raw materials in parts by weight:
the polymer comprises polybutylene terephthalate succinate and polypropylene carbonate.
Preferably, the mass ratio of the polybutylene terephthalate to the polypropylene carbonate is 50-90: 50-10.
Preferably, the foaming agent comprises one or more of azodicarbonamide, sodium bicarbonate and 4, 4' -oxybis-benzenesulfonylhydrazide.
Preferably, the chain extender comprises dicumyl peroxide;
the capping agent comprises maleic anhydride;
the nucleating agent comprises talcum powder;
the plasticizer comprises epoxidized soybean oil.
Preferably, the thickness of the degradable PBST/PPC composite foaming material is 0.9-1 mm;
the density of the degradable PBST/PPC composite foaming material is 0.8-1 g/cm3。
Preferably, the melt index of the composite foaming material is 3-5 g/10min (190 ℃, 2.16 kg).
The invention also provides a preparation method of the degradable PBST/PPC composite foaming material, which comprises the following steps:
mixing a polymer, a chain extender, a terminating agent, a nucleating agent, a foaming agent and a plasticizer, and extruding and molding to obtain the degradable PBST/PPC composite foaming material.
Preferably, the mixing is carried out at room temperature;
the mixing time is 10-20 min.
Preferably, the extrusion is carried out in an extruder formed by connecting a double-screw extrusion structure and a single-screw extrusion structure in series;
the length-diameter ratio of the twin-screw is 36: 1;
the first zone temperature of the double-screw extrusion structure is 150-155 ℃, the second zone temperature is 170-175 ℃, the third zone temperature is 180-185 ℃, and the fourth zone temperature is 190-195 ℃;
the length-diameter ratio of the single screw is 30: 1;
the temperature of the single-screw extrusion structure in the first area is 195-200 ℃, the temperature of the second area is 190-195 ℃, the temperature of the third area is 175-180 ℃, and the temperature of the fourth area is 170-175 ℃;
the temperature of the head of the extruder is 160-165 ℃.
The invention provides a degradable PBST/PPC composite foaming material which is prepared from the following raw materials in parts by weight: 100 parts of a polymer; 0.5-3 parts of a chain extender; 0.5-3 parts of an end-capping agent; 0.5-5 parts of a nucleating agent; 0.5-2 parts of a foaming agent; 0.1-3 parts of a plasticizer; the polymer comprises polybutylene terephthalate succinate and polypropylene carbonate. According to the invention, a chain extender is adopted to carry out chain extension on a specific polymer, an end capping agent is adopted to carry out end capping, and other raw materials are matched for synergistic effect, after extrusion processing, a main chain in an obtained material system contains functional fragments, a mutually-penetrated network structure is formed, chain entanglement is generated, the melt strength of the system is increased, the melt index of the system is improved, and the finally obtained degradable PBST/PPC composite foaming material has the advantages of excellent tensile property, high melt index of the system and excellent foaming property. Meanwhile, the processing process conditions such as processing time, processing temperature and the like of the degradable PBST/PPC composite foaming material system are optimized, the physical property of the degradable PBST/PPC composite foaming material system is improved, and the continuous and controllable manufacturing of the degradable PBST/PPC composite foaming material by one-step method is realized.
Drawings
FIG. 1 is an SEM image of a degradable PBST/PPC composite foamed material of example 1 of the invention;
FIG. 2 is the degradable PBST/PPC composite foam of example 1 under controlled composting conditionsCO of feed2A graph of the amount of released versus time;
FIG. 3 is a graph of biodegradation rate of the degradable PBST/PPC composite foam of example 1 under controlled composting conditions versus time.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments of the present invention, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention provides a degradable PBST/PPC composite foaming material which is prepared from the following raw materials in parts by weight:
the polymers include polybutylene terephthalate succinate (PBST) and polypropylene carbonate (PPC).
The degradable PBST/PPC composite foaming material provided by the invention is prepared from polymer. In certain embodiments of the present invention, the weight fraction of the polymer is 100 parts.
The polymers include polybutylene terephthalate succinate (PBST) and polypropylene carbonate (PPC).
In certain embodiments of the invention, the PBST is available from China petrochemical group, Inc. certification division, model number TS 159.
In certain embodiments of the invention, the PPC has a weight average molecular weight of 3.0 x 105g/mol. In certain embodiments of the present invention, the PPC is prepared by copolymerization of carbon dioxide and propylene oxide over a catalyst. Specifically, the compound can be prepared according to the method disclosed in Chinese patent CN 101402726B.
In certain embodiments of the present invention, the mass ratio of polybutylene terephthalate to polypropylene carbonate is 50 to 90: 50-10. In certain embodiments, the mass ratio of polybutylene terephthalate to polypropylene carbonate is 90: 10. 80: 20. 70: 30. 60: 40 or 50: 50.
the raw materials for preparing the degradable PBST/PPC composite foaming material also comprise a chain extender. In certain embodiments of the present invention, the weight part of the chain extender is 0.5 to 3 parts. In certain embodiments of the present invention, the chain extender comprises dicumyl peroxide (DCP) and/or bis- (2-tert-butylperoxyisopropyl) benzene (BIBP).
The raw materials for preparing the degradable PBST/PPC composite foaming material also comprise an end-capping reagent. In certain embodiments of the present invention, the capping agent is present in an amount of 0.5 to 3 parts by weight. In certain embodiments of the present invention, the capping agent comprises Maleic Anhydride (MA).
The raw materials for preparing the degradable PBST/PPC composite foaming material also comprise a nucleating agent. In certain embodiments of the present invention, the nucleating agent is 0.5 to 5 parts by weight. In certain embodiments of the present invention, the nucleating agent comprises talc. In certain embodiments, the nucleating agent is talc SK-98.
The degradable PBST/PPC composite foaming material provided by the invention also comprises a foaming agent as a raw material for preparation. In certain embodiments of the present invention, the blowing agent is present in an amount of 0.5 to 2 parts by weight. In certain embodiments of the present invention, the blowing agent comprises Azodicarbonamide (AC), sodium bicarbonate (NaHCO)3) And 4, 4' -oxybis-benzenesulfonyl hydrazide (OBSH).
The degradable PBST/PPC composite foaming material provided by the invention also comprises a plasticizer as a raw material for preparation. In certain embodiments of the present invention, the plasticizer is present in an amount of 0.1 to 3 parts by weight. In certain embodiments of the present invention, the plasticizer comprises Epoxidized Soybean Oil (ESO).
In certain embodiments of the invention, the thickness of the degradable PBST/PPC composite foaming material is 0.9-1 mm.
The degradable PBST/PPC composite foaming material provided by the invention has uniform cell distribution and uniform cell size. In certain embodiments of the invention, the degradable PBST/PPC composite foaming material has a pore size ranging from 0.09 to 0.11 μm.
In certain embodiments of the invention, the degradable PBST/PPC composite foaming material has a density of 0.8-1 g/cm3. In certain embodiments, the degradable PBST/PPC composite foam has a density of 0.81g/cm3、0.83g/cm3、0.86g/cm3、0.91g/cm3Or 0.90g/cm3. The degradable PBST/PPC composite foaming material provided by the invention is a micro-foaming composite material, and realizes the low density of the degradable foaming composite material, thereby reducing the weight of the degradable foaming composite material. Meanwhile, the degradable PBST/PPC composite foaming material provided by the invention is biodegradable.
In certain embodiments of the invention, the degradable PBST/PPC composite foam material has a melt index of 3-5 g/10min (190 ℃, 2.16 kg).
The invention also provides a method for preparing the degradable PBST/PPC composite foaming material by adopting a one-step method, which comprises the following steps:
mixing a polymer, a chain extender, a terminating agent, a nucleating agent, a foaming agent and a plasticizer, and extruding and molding to obtain the degradable PBST/PPC composite foaming material.
In certain embodiments of the invention, the mixing is performed at room temperature. In some embodiments of the present invention, the mixing time is 10-20 min.
In certain embodiments of the present invention, the extrusion is performed in an extruder having a twin screw extrusion configuration and a single screw extrusion configuration in series.
In certain embodiments of the invention, the twin screws have a length to diameter ratio of 36: 1.
in certain embodiments of the present invention, the twin screws are rotated at a speed of 210 to 230 rpm.
In some embodiments of the present invention, the first zone temperature of the twin-screw extrusion structure is 150 to 155 ℃, the second zone temperature is 170 to 175 ℃, the third zone temperature is 180 to 185 ℃, and the fourth zone temperature is 190 to 195 ℃.
In certain embodiments of the invention, the single screw has a length to diameter ratio of 30: 1.
in some embodiments of the present invention, the rotation speed of the single screw is 60-70 rpm.
In some embodiments of the present invention, the temperature of the first zone of the single screw extrusion structure is 195-200 ℃, the temperature of the second zone is 190-195 ℃, the temperature of the third zone is 175-180 ℃, and the temperature of the fourth zone is 170-175 ℃.
In some embodiments of the invention, the extruder head temperature is 160 to 165 ℃.
The source of the above-mentioned raw materials is not particularly limited in the present invention, and may be generally commercially available.
According to the invention, a specific polymer is subjected to chain extension by adopting a chain extender to carry out chain extension on PBST resin, an end-capping agent MA is adopted to carry out end capping on PPC, and meanwhile, the chain-capping agent MA is matched with the synergistic effect of other raw materials, and after extrusion processing, a main chain in an obtained material system contains functional segments to form a mutually-penetrated network structure, so that chain entanglement is generated, the melt strength of the system is increased, the melt index of the system is improved, and the finally obtained degradable PBST/PPC composite foaming material has the advantages of excellent tensile property, high melt index of the system and excellent foaming property. Meanwhile, the processing process conditions such as processing time, processing temperature and the like of the degradable PBST/PPC composite foaming material system are optimized, the physical property of the degradable PBST/PPC composite foaming material system is improved, and the continuous and controllable manufacturing of the degradable PBST/PPC composite foaming material by one-step method is realized.
In order to further illustrate the present invention, the following examples are provided to describe the degradable PBST/PPC composite foamed material and the preparation method thereof in detail, but should not be construed as limiting the scope of the present invention.
The starting materials used in the following examples are all generally commercially available.
Example 1
Stirring and mixing 90 parts by weight of PBST, 10 parts by weight of PPC, 3 parts by weight of DCP, 2 parts by weight of MA, 2 parts by weight of AC, 1 part by weight of talcum powder SK-98 and 3 parts by weight of ESO in a high-speed stirrer for 10min at room temperature to obtain a mixed material, then adding the mixed material into an extruder formed by connecting a double-screw extrusion structure and a single-screw extrusion structure in series, and carrying out extrusion molding to obtain a degradable PBST/PPC composite foaming material (the thickness of the degradable PBST/PPC composite foaming material is controlled to be 0.9-1 mm);
the first zone temperature of the twin-screw extrusion structure is 152 ℃, the second zone temperature is 170 ℃, the third zone temperature is 185 ℃, and the fourth zone temperature is 192 ℃;
the length-diameter ratio of the twin screw is 36: 1, the rotating speed of the twin-screw is 220 rpm;
the temperature of a first area of the single-screw extrusion structure is 197 ℃, the temperature of a second area is 193 ℃, the temperature of a third area is 175 ℃, and the temperature of a fourth area is 170 ℃;
the length-diameter ratio of the single screw is 30: 1, the rotating speed of the single screw is 65 rpm;
the head temperature of the extruder was 162 ℃.
FIG. 1 is an SEM image of a degradable PBST/PPC composite foamed material of example 1 of the invention. As can be seen from FIG. 1, the degradable PBST/PPC composite foaming material has uniform cell distribution, and the cell size is 0.09-0.11 μm, which is relatively uniform.
According to GB/T19277-2003, the CO of the PBST/PPC composite foaming material degradable in the example 1 under the controlled composting condition is obtained by performing experimental operation by adopting a method for measuring the release of carbon dioxide according to the measurement of the final aerobic biological decomposition and disintegration capability of the PBST/PPC foaming composite under the controlled composting condition2Is plotted against time, as shown in figure 2; and the biodegradation rate of the degradable PBST/PPC composite foam of example 1 under controlled composting conditions versus time as shown in figure 3.
FIG. 2 is CO of the degradable PBST/PPC composite foam of example 1 under controlled composting conditions2Graph of the amount of released versus time. FIG. 3 is a graph of biodegradation rate of the degradable PBST/PPC composite foam of example 1 under controlled composting conditions versus time. As can be seen from FIGS. 2 and 3, PPC was tested at 10About 0d, CO2The release amount and the biological decomposition rate tend to be stable, the maximum release amount is 103g, and the maximum biological decomposition rate is about 62 percent.
Example 2
Stirring and mixing 80 parts by weight of PBST, 20 parts by weight of PPC, 3 parts by weight of DCP, 2 parts by weight of MA, 2 parts by weight of AC, 1 part by weight of talcum powder SK-98 and 3 parts by weight of ESO in a high-speed stirrer for 10min to obtain a mixed material, then adding the mixed material into an extruder formed by connecting a double-screw extrusion structure and a single-screw extrusion structure in series, and carrying out extrusion molding to obtain a degradable PBST/PPC composite foaming material (the thickness of the degradable PBST/PPC composite foaming material is controlled to be 0.9-1 mm);
the extruder operating parameters were the same as in example 1.
Example 3
Stirring and mixing 70 parts by weight of PBST, 30 parts by weight of PPC, 3 parts by weight of DCP, 2 parts by weight of MA, 2 parts by weight of AC, 1 part by weight of talcum powder SK-98 and 3 parts by weight of ESO in a high-speed stirrer for 10min to obtain a mixed material, then adding the mixed material into an extruder formed by connecting a double-screw extrusion structure and a single-screw extrusion structure in series, and carrying out extrusion molding to obtain a degradable PBST/PPC composite foaming material (the thickness of the degradable PBST/PPC composite foaming material is controlled to be 0.9-1 mm);
the extruder operating parameters were the same as in example 1.
Example 4
Stirring and mixing 60 parts by weight of PBST, 40 parts by weight of PPC, 3 parts by weight of DCP, 2 parts by weight of MA, 2 parts by weight of AC, 1 part by weight of talcum powder SK-98 and 3 parts by weight of ESO in a high-speed stirrer for 10min to obtain a mixed material, then adding the mixed material into an extruder formed by connecting a double-screw extrusion structure and a single-screw extrusion structure in series, and carrying out extrusion molding to obtain a degradable PBST/PPC composite foaming material (the thickness of the degradable PBST/PPC composite foaming material is controlled to be 0.9-1 mm);
the extruder operating parameters were the same as in example 1.
Example 5
Stirring and mixing 50 parts by weight of PBST, 50 parts by weight of PPC, 3 parts by weight of DCP, 2 parts by weight of MA, 2 parts by weight of AC, 1 part by weight of talcum powder SK-98 and 3 parts by weight of ESO in a high-speed stirrer for 10min to obtain a mixed material, then adding the mixed material into an extruder formed by connecting a double-screw extrusion structure and a single-screw extrusion structure in series, and carrying out extrusion molding to obtain a degradable PBST/PPC composite foaming material (the thickness of the degradable PBST/PPC composite foaming material is controlled to be 0.9-1 mm);
the extruder operating parameters were the same as in example 1.
Example 6
Stirring and mixing 70 parts by weight of PBST, 30 parts by weight of PPC, 3 parts by weight of DCP, 2 parts by weight of MA, 2 parts by weight of OBSH, 1 part by weight of talcum powder SK-98 and 3 parts by weight of ESO in a high-speed stirrer for 10min to obtain a mixed material, then adding the mixed material into an extruder formed by connecting a double-screw extrusion structure and a single-screw extrusion structure in series, and carrying out extrusion molding to obtain a degradable PBST/PPC composite foaming material (the thickness of the degradable PBST/PPC composite foaming material is controlled to be 0.9-1 mm);
the extruder operating parameters were the same as in example 1.
Example 7
Stirring and mixing 70 parts by weight of PBST, 30 parts by weight of PPC, 3 parts by weight of DCP, 2 parts by weight of MA, 2 parts by weight of sodium bicarbonate, 1 part by weight of talcum powder SK-98 and 3 parts by weight of ESO in a high-speed stirrer for 10min to obtain a mixed material, then adding the mixed material into an extruder formed by connecting a double-screw extrusion structure and a single-screw extrusion structure in series, and carrying out extrusion molding to obtain a degradable PBST/PPC composite foaming material (the thickness of the degradable PBST/PPC composite foaming material is controlled to be 0.9-1 mm);
the extruder operating parameters were the same as in example 1.
The mechanical property detection of the degradable PBST/PPC composite foaming material prepared in the embodiment 1-7 is carried out, and the detection result is shown in Table 1:
table 1 results of mechanical property measurements of composite foamed materials prepared in examples 1 to 7
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (9)
2. The degradable PBST/PPC composite foam material according to claim 1, wherein the mass ratio of polybutylene terephthalate to polypropylene carbonate is 50-90: 50-10.
3. The degradable PBST/PPC composite foaming material according to claim 1, wherein the foaming agent comprises one or more of azodicarbonamide, sodium bicarbonate and 4, 4' -oxybis-benzenesulfonylhydrazide.
4. The degradable PBST/PPC composite foam according to claim 1, wherein the chain extender comprises dicumyl peroxide;
the capping agent comprises maleic anhydride;
the nucleating agent comprises talcum powder;
the plasticizer comprises epoxidized soybean oil.
5. The degradable PBST/PPC composite foam material according to claim 1, wherein the degradable PBST/PPC composite foam material has a thickness of 0.9-1 mm;
the density of the degradable PBST/PPC composite foaming material is 0.8-1 g/cm3。
6. The degradable PBST/PPC composite foam according to claim 1, wherein the composite foam has a melt index of 3-5 g/10min (190 ℃, 2.16 kg).
7. The method of preparing the degradable PBST/PPC composite foamed material of claim 1, comprising the steps of:
mixing a polymer, a chain extender, a terminating agent, a nucleating agent, a foaming agent and a plasticizer, and extruding and molding to obtain the degradable PBST/PPC composite foaming material.
8. The method of claim 7, wherein the mixing is performed at room temperature;
the mixing time is 10-20 min.
9. The production method according to claim 7, wherein the extrusion is performed in an extruder in which a twin-screw extrusion structure and a single-screw extrusion structure are connected in series;
the length-diameter ratio of the twin-screw is 36: 1;
the first zone temperature of the double-screw extrusion structure is 150-155 ℃, the second zone temperature is 170-175 ℃, the third zone temperature is 180-185 ℃, and the fourth zone temperature is 190-195 ℃;
the length-diameter ratio of the single screw is 30: 1;
the temperature of the single-screw extrusion structure in the first area is 195-200 ℃, the temperature of the second area is 190-195 ℃, the temperature of the third area is 175-180 ℃, and the temperature of the fourth area is 170-175 ℃;
the temperature of the head of the extruder is 160-165 ℃.
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