CN110760095A - Preparation process of polycarbonate foamed sheet and product thereof - Google Patents
Preparation process of polycarbonate foamed sheet and product thereof Download PDFInfo
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- CN110760095A CN110760095A CN201810825735.6A CN201810825735A CN110760095A CN 110760095 A CN110760095 A CN 110760095A CN 201810825735 A CN201810825735 A CN 201810825735A CN 110760095 A CN110760095 A CN 110760095A
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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
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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
- C08J2203/00—Foams characterized by the expanding agent
- C08J2203/06—CO2, N2 or noble gases
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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
- C08J2369/00—Characterised by the use of polycarbonates; Derivatives of polycarbonates
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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
- C08J2433/00—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 only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
- C08J2433/04—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 only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers esters
- C08J2433/06—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 only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers esters of esters containing only carbon, hydrogen, and oxygen, the oxygen atom being present only as part of the carboxyl radical
- C08J2433/10—Homopolymers or copolymers of methacrylic acid esters
- C08J2433/12—Homopolymers or copolymers of methyl methacrylate
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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
- C08J2467/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
- C08J2467/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
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Abstract
The invention discloses a preparation process of a polycarbonate foamed sheet, which comprises the following steps: placing the sheet containing the polycarbonate in high-pressure fluid until the sheet is saturated, and taking out the sheet after pressure relief to obtain a saturated sheet; the pressure of the high-pressure fluid is 1.0-6.0 MPa; placing the prepared saturated sheet in a heat medium, and foaming to obtain the polycarbonate foamed sheet; the temperature of the heat medium is 145-210 ℃; the foaming time is 5-60 s. The preparation process is mild in reaction condition, environment-friendly and short in foaming time, and the prepared polycarbonate foamed sheet is light in weight, has a smooth surface, has the cell size of 10-50 microns and is uniform in cell size distribution.
Description
Technical Field
The invention relates to the technical field of plastic foaming materials, in particular to a preparation process of a polycarbonate foaming sheet and a product thereof.
Background
The polycarbonate resin (PC) is thermoplastic engineering plastic with excellent comprehensive performance, has good impact resistance and dimensional stability, low water absorption, no odor, no toxicity, weak acid and alkali resistance, excellent dielectric property and good mechanical property at common use temperature. PC resins have become a popular engineering plastic with a rapidly increasing rate of use in recent years due to their excellent balance of properties.
The polymer foam material has the characteristics of light weight, sound insulation, heat insulation and the like, so that the use cost can be reduced, the toughness can be improved, the fatigue life can be prolonged and the like after the PC is prepared into the foam material. The PC foam material has the advantages of high impact toughness, strong energy absorption and shock resistance, long fatigue life, good sound and heat insulation and the like, and can be used as light structural materials for aerospace and the like, automobile industrial parts, sound insulation materials and the like. The PC foamed sheet can be made into a product through a simple thermal forming process, and the manufacturing technology has the advantages of short production period and convenience in operation, and meets the requirements of actual industrial production.
At present, the preparation of PC foamed sheets mainly comprises a chemical foaming method and a physical foaming method, wherein the physical foaming method is widely applied due to the simple and environment-friendly preparation process, small size of foam pores of a foamed product and uniform distribution of the foam pores. The simplest and most common method in the physical foaming method is a kettle pressure batch method, which can be divided into two methods: the first method is a step-by-step heating method: after the polymer is saturated and absorbed with a low temperature supercritical fluid in an autoclave, foaming is carried out by releasing the pressure and then rapidly raising the temperature of the sample. The second method is a rapid depressurization method: supercritical fluid to polymer in high pressure kettleAfter saturation, rapid pressure relief is carried out, and micropores are directly formed. The cell morphology can be controlled by controlling the rate of pressure relief, the time of incubation after pressure relief, and the saturation pressure and temperature. Among them, carbon dioxide (CO)2) The fluid is a clean, cheap and environment-friendly physical foaming agent, and is widely used for preparing PC foamed sheets by a physical foaming method.
For example, Yang Yong (CO)2Microcellular foamed polycarbonate/polystyrene, poplar courage, zheng leather, zhang shang bin, wang wen, luohui, plastic, No. 1, volume 39, 2010) are prepared into microcellular foamed materials of polycarbonate/polystyrene blends at relatively low pressure by a rapid temperature rise method. The specific experimental process is as follows: pure PC, pure PS and a blended sample of PC80/PS20 were placed in an autoclave at 25 ℃ with 48MPa of CO2And (3) quickly relieving pressure after saturation for 36h, putting the saturated sample into a glycerol bath with a set temperature for foaming for 40s, and finally putting the sample into an ice water bath for cooling and shaping to obtain a foamed sample. The foaming process is a rapid depressurization method, the adopted saturation pressure is up to 48MPa, the requirement on production equipment is high, and potential safety hazards exist.
Also, as disclosed in chinese patent publication No. CN 107674233a, a method for preparing a polycarbonate microcellular foam material includes the steps of 1: soaking in a supercritical fluid at 100-140 ℃ and 1-15 MPa for 10-600 min; step 2: and (3) putting the soaked polycarbonate material in the step (1) into a pressure container, filling a supercritical fluid to 15-30 MPa, and then controlling the pressure relief rate to be 50-500 MPa/s to prepare the polycarbonate microporous foaming material. The foaming process is also a rapid depressurization method, requires higher pressure and has high requirements on equipment.
Disclosure of Invention
The invention aims at the technical problems and discloses a preparation process of a polycarbonate foamed sheet, which has the advantages of mild reaction conditions, environmental friendliness and short foaming time, and the prepared polycarbonate foamed sheet is light in weight, has a smooth surface, has the cell size of 10-50 mu m and is uniform in cell size distribution.
The specific technical scheme is as follows:
a preparation process of a polycarbonate foamed sheet comprises the following steps:
(1) placing the sheet containing the polycarbonate in high-pressure fluid until the sheet is saturated, and taking out the sheet after pressure relief to obtain a saturated sheet;
the pressure of the high-pressure fluid is 1.0-6.0 MPa;
(2) placing the saturated sheet prepared in the step (1) in a heat medium, and foaming to obtain the polycarbonate foamed sheet;
the temperature of the heat medium is 145-210 ℃;
the foaming time is 5-60 s.
The invention adopts a heating foaming method for preparing the polycarbonate foaming sheet for the first time, the process greatly reduces the pressure of high-pressure fluid, the saturation time is short, the obtained saturated sheet has excellent stability, can be placed for a period of time in an atmospheric environment, and has feasibility of realizing industrial production.
In the step (1), after the polycarbonate is saturated under the pressure of 1.0-6.0 MPa, the gas solubility of the matrix can change, and the solubility is about 40-120 (gCO)2/kgPC) due to CO2The plasticizing effect of (2) can improve the movement capacity of the PC molecular chains, so that the foaming temperature in the step (2) is set to be 145-210 ℃ and the foaming time is set to be 5-60 s based on the solubility of the saturated sheet and the movement capacity of the PC molecular chains in the material. The foamed sheet having a uniform cell distribution can be produced under the above foaming conditions, and when the foaming conditions are out of the above set ranges, it may cause difficulty in foaming or unevenness in cell size distribution.
In step (1), the polycarbonate-containing sheet is selected from pure polycarbonate, such as a commercial PC web;
or a blend of polycarbonate and at least one of siloxane, styrene, polyethylene, polymethyl methacrylate, thermoplastic polyurethane, polylactic acid, polybutylene terephthalate, acrylonitrile-butadiene-styrene, and polyamide.
Preferably, the content of the polycarbonate in the blend is 55-99 wt%.
Further preferably, the polycarbonate-containing sheet is selected from a PC/PMMA blend sheet or a PC/PET blend sheet. PMMA is an amorphous polymer, can be used as a cell nucleation point after a PC matrix is added, improves the foaming performance of PC, and is favorable for forming a larger cell structure with uniform distribution because the matrix strength is lower than that of PC; the crystallization rate of PET is slow, and the formed crystals can be used as a foam cell nucleating agent to increase the density of foam cells.
Besides the blend prepared by blending PC and other polymers is used as a raw material sheet, the filler can be added for modification, and the method is suitable for industrial application and has a high market value.
Preferably, the filler is selected from at least one of nano silica, montmorillonite, graphene and talcum powder;
the filler is added in an amount of 0.005 to 5.0 wt% based on the total mass of the polycarbonate-containing sheet.
Preferably, the thickness of the polycarbonate-containing sheet is 0.01 to 3.0 mm. According to the thickness of the raw material sheet, the saturation time of the sheet is required to be prolonged along with the increase of the thickness, and the storage time in the atmosphere after saturation can be prolonged along with the increase of the thickness of the sheet.
Preferably, in step (1), the high-pressure fluid is selected from a pure gas or a mixture of a gas and an organic solvent;
the gas is selected from carbon dioxide or nitrogen;
the organic solvent is selected from at least one of butane, pentane and ethanol.
The organic solvent accounts for 0.01-2.0% of the total volume of the high-pressure fluid.
It has been found through experimentation that the required saturation time can be significantly reduced when a mixture of gas and organic solvent is used as the high pressure fluid.
Further preferably, the organic solvent is selected from butane, and accounts for 0.02-0.1% of the total volume of the high-pressure fluid.
Preferably, in the step (2), the heat medium is selected from air heated to a set temperature and simethicone. That is, foaming can be performed in a high temperature oil bath or a forced air oven.
Preferably, the pressure of the high-pressure fluid is 2.0-3.0 MPa, the temperature of the heat medium is 150-190 ℃, and the foaming time is 15-50 s.
When foaming is carried out in a high-temperature oil bath, the preferable foaming temperature is 150-180 ℃, and the foaming time is 15-25 s;
when foaming is carried out in a blast oven, the preferable foaming temperature is 160-190 ℃, and the foaming time is 25-50 s;
the invention also discloses a polycarbonate foamed sheet prepared by the process, the size of the foam pores is 10-50 mu m, the size distribution of the foam pores is uniform, the surface of the foamed sheet is smooth, and the density is 0.3-0.8 g/cm3。
Compared with the prior art, the invention has the following beneficial effects:
(1) the invention provides a method for preparing a PC foamed sheet by a physical foaming method, the pressure of the required high-pressure fluid is only 1.0-6.0 MPa, the requirement on equipment is low, and the potential safety hazard is greatly reduced; the method also greatly shortens the saturation time, the saturation time is only 0.5-4 h under the optimized condition, and the production period is greatly shortened.
(2) The saturated sheet prepared by the step (1) has excellent stability, can be placed in an atmospheric environment for a period of time, and provides possibility for realizing industrial production.
(3) The foaming mode in the step (2) of the invention is various, and the foaming can be carried out by adopting high-temperature oil or a blast oven, and can be selected according to the actual production requirement.
(4) The PC foamed sheet prepared by the invention has the advantages of small density, small cell size and uniform cell size distribution.
Drawings
FIG. 1 is a sectional cell morphology of a PC foamed sheet prepared in example 1;
FIG. 2 is a sectional cell morphology of the PC foamed sheet prepared in example 5.
Detailed Description
The following examples are further illustrative of the present invention and should not be construed as limiting the scope of the invention. If the invention is modified in some insubstantial ways in light of the above disclosure, it would be within the scope of the invention.
Example 1
Placing 0.5mm thick PC sheet in autoclave, introducing high pressure CO at 3MPa2And (3) flowing the liquid, wherein the saturation temperature is 25 ℃, and the saturation time is 1h, so that a saturated PC sheet is obtained. After the PC sheet was left to stand in an atmospheric environment for 5 seconds, the PC sheet was placed in a forced air oven at 170 ℃ to foam for 35 seconds, to obtain a PC micro-foamed sheet.
The prepared PC micro-foamed sheet has a smooth appearance structure, and the quenching section of a PC micro-foamed sheet sample is analyzed by a scanning electron microscope, as shown in figure 1, the PC micro-foamed sheet has the cell size of 10-30 mu m, the cell size is uniformly distributed, and the density is 0.55g/cm3。
Example 2
In the embodiment, except that the thickness of the PC sheet is 3mm, the saturated PC sheet is placed in the atmospheric environment for 2 hours and then foamed, and the other conditions are the same as those of the embodiment 1, the size of the foam pores of the prepared PC micro-foamed sheet is 10-30 mu m, the size distribution of the foam pores is uniform, and the density of the PC micro-foamed sheet is 0.80g/cm3。
Example 3
In the embodiment, except that the saturation pressure is changed to 2.0MPa, the other conditions are the same as those of the embodiment 1, the size of the foam pores of the prepared PC micro-foaming sheet is 20-40 mu m, the size distribution of the foam pores is uniform, and the density of the PC micro-foaming sheet is 0.65g/cm3。
Example 4
In the present example, except that the saturation pressure was changed to 6.0MPa, the conditions were the same as in example 1, and the obtained PC micro-foamed sheet had a cell size of 10 to 50 μm, a non-uniform cell distribution, and a density of 0.50g/cm3。
Example 5
In this example, the PC micro-foamed sheet prepared in example 1 was smooth and flat, except that the foaming was carried out in an oil bath of high temperature dimethylsilicone oil under the foaming temperature of 150 ℃ for 20 seconds, and the quenching section of the PC micro-foamed sheet sample was analyzed by scanning electron microscopy as shown in FIG. 2The method shows that the size of the foam pores of the PC micro-foamed sheet is 10-30 mu m, the distribution of the foam pores is uniform, and the density of the PC micro-foamed sheet is 0.50g/cm3。
Example 6
In the present example, the conditions were the same as those in example 1 except that the thickness of the PC sheet was changed to 0.1mm, and the prepared PC micro-foamed sheet had a cell size of 10 to 30 μm, a uniform cell distribution and a density of 0.35g/cm3。
Example 7
In this example, the PC micro-foamed sheet prepared under the same conditions as in example 1 except that the saturated fluid of the PC sheet is a high-pressure fluid of a mixture of carbon dioxide and butane (the volume content of butane in the high-pressure fluid is 0.05%) and is saturated for 0.5h, has a cell size of 10-30 μm and uniform cell distribution, and has a density of 0.50g/cm3。
Example 8
Uniformly mixing PC particles and nano silicon dioxide by a high-speed mixer, adding the mixture into a double-screw extruder, extruding and conveying a sample melt to a die orifice of the extruder by double screws, and extruding the PC nano composite melt to prepare a sheet with the thickness of 0.5mm by drafting. In this example, the amount of nanosilica added was 0.1 wt% except that the sheet was a PC/nanosilica composite. The other conditions are the same as those of the example 1, the size of the foam pores of the prepared PC micro-foaming sheet is 5-20 mu m, the distribution of the foam pores is uniform, and the density of the prepared PC micro-foaming sheet is 0.45g/cm3。
Example 9
Uniformly mixing the PC particles and the PMMA particles through a high-speed mixer, adding the mixture into a double-screw extruder, extruding and conveying a sample melt to a die orifice of the extruder through double screws, and extruding the PC/PMMA composite melt to prepare a sheet with the thickness of 0.5mm through drafting. In this example, PMMA was added in an amount of 10.0 wt% except that the sheet was a PC/PMMA composite sheet. The other conditions are the same as example 1, the size of the prepared PC micro-foaming sheet is 20-35 mu m, the distribution of the foam holes is uniform, and the density is 0.40g/cm3。
Example 10
In this example, PET was added in an amount of 10.0 wt% except that the sheet was a PC/PET composite sheet. Other conditions were the same as in example 8The obtained PC micro-foaming sheet has the cell size of 5-25 mu m, uniform cell distribution and density of 0.45g/cm3。
Example 11
In this example, the amount of PMMA added is 10.0 wt% and the amount of nanosilicon dioxide added is 0.1 wt%, except that the sheet is a PC/PMMA/nanosilicon dioxide composite sheet. The other conditions are the same as those of the example 8, the size of the foam pores of the prepared PC/PMMA/nano micro-foamed sheet is 5-25 mu m, the foam pores are uniformly distributed, and the density of the prepared PC/PMMA/nano micro-foamed sheet is 0.35g/cm3。
Comparative example 1
The PC foamed sheet in this comparative example was prepared in the same manner as in example 1 except that the temperature of the forced air oven was 100 ℃, the foaming time was 10 seconds, and the density of the PC micro-foamed sheet was 1.12g/cm3。
Comparative example 2
In this comparative example, the number of cells formed was small and the density of the PC micro-foamed sheet was 1.08g/cm under the same conditions as in example 1 except that the saturation pressure was changed to 0.5MPa3。
Claims (10)
1. A preparation process of a polycarbonate foamed sheet is characterized by comprising the following steps:
(1) placing the sheet containing the polycarbonate in high-pressure fluid until the sheet is saturated, and taking out the sheet after pressure relief to obtain a saturated sheet;
the pressure of the high-pressure fluid is 1.0-6.0 MPa;
(2) placing the saturated sheet prepared in the step (1) in a heat medium, and foaming to obtain the polycarbonate foamed sheet;
the temperature of the heat medium is 145-210 ℃;
the foaming time is 5-60 s.
2. The process for preparing a polycarbonate foamed sheet according to claim 1, wherein in the step (1), the polycarbonate-containing sheet is selected from the group consisting of pure polycarbonate;
or a blend of polycarbonate and at least one of siloxane, styrene, polyethylene, polymethyl methacrylate, thermoplastic polyurethane, polylactic acid, polybutylene terephthalate, acrylonitrile-butadiene-styrene, and polyamide.
3. The process for preparing a polycarbonate foamed sheet according to claim 2, wherein the blend contains the polycarbonate in an amount of 55 to 99 wt%.
4. The process for preparing a polycarbonate foamed sheet according to claim 1, wherein in the step (1), the polycarbonate-containing sheet further comprises a filler;
the filler is selected from at least one of nano silicon dioxide, montmorillonite, graphene and talcum powder;
the filler is added in an amount of 0.005 to 5.0 wt% based on the total mass of the polycarbonate-containing sheet.
5. The process for preparing a polycarbonate foamed sheet according to claim 1, wherein in the step (1), the thickness of the polycarbonate-containing sheet is 0.01 to 3.0 mm.
6. The process for preparing a polycarbonate foamed sheet according to claim 1, wherein in the step (1), the high-pressure fluid is selected from a pure gas or a mixture of a gas and an organic solvent;
the gas is selected from carbon dioxide or nitrogen;
the organic solvent is selected from at least one of butane, pentane and ethanol.
7. The process for preparing a polycarbonate foamed sheet according to claim 6, wherein in the step (1), the organic solvent accounts for 0.01 to 2.0% of the total volume of the high-pressure fluid.
8. The process for preparing a polycarbonate foamed sheet according to claim 1, wherein in the step (2), the heat medium is selected from air or dimethylsilicone oil heated to a set temperature.
9. The process for preparing a polycarbonate foamed sheet according to any one of claims 1 to 8, wherein the pressure of the high-pressure fluid is 2.0 to 3.0MPa, the temperature of the heat medium is 150 to 190 ℃, and the foaming time is 15 to 50 s.
10. A polycarbonate foamed sheet prepared according to the process of any one of claims 1 to 9.
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| JP2003253032A (en) * | 2002-02-28 | 2003-09-10 | Idemitsu Petrochem Co Ltd | Foamable thermoplastic resin composition and foam thereof |
| CN101223460A (en) * | 2005-07-14 | 2008-07-16 | 帝人化成株式会社 | Foamed resin sheet and liquid crystal display |
| CN102241830A (en) * | 2011-04-28 | 2011-11-16 | 中国科学院宁波材料技术与工程研究所 | Preparation method of biodegradable polymer foamed sheet product |
| CN102702561A (en) * | 2012-05-25 | 2012-10-03 | 中国科学院宁波材料技术与工程研究所 | Preparation method of low-density thermoplastic polyimide micro-foamed material |
| US20160137806A1 (en) * | 2013-06-28 | 2016-05-19 | University Of Washington Through Its Center For Commercialization | Solid-state thermoplastic nanofoams |
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- 2018-07-25 CN CN201810825735.6A patent/CN110760095A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2003253032A (en) * | 2002-02-28 | 2003-09-10 | Idemitsu Petrochem Co Ltd | Foamable thermoplastic resin composition and foam thereof |
| CN101223460A (en) * | 2005-07-14 | 2008-07-16 | 帝人化成株式会社 | Foamed resin sheet and liquid crystal display |
| CN102241830A (en) * | 2011-04-28 | 2011-11-16 | 中国科学院宁波材料技术与工程研究所 | Preparation method of biodegradable polymer foamed sheet product |
| CN102702561A (en) * | 2012-05-25 | 2012-10-03 | 中国科学院宁波材料技术与工程研究所 | Preparation method of low-density thermoplastic polyimide micro-foamed material |
| US20160137806A1 (en) * | 2013-06-28 | 2016-05-19 | University Of Washington Through Its Center For Commercialization | Solid-state thermoplastic nanofoams |
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