CN111218022A - Preparation method and product of negative Poisson ratio bio-based rigid foam material - Google Patents
Preparation method and product of negative Poisson ratio bio-based rigid foam material 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
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08J2367/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
- C08J2367/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2367/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
- C08J2367/04—Polyesters derived from hydroxy carboxylic acids, e.g. lactones
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Abstract
The invention relates to a preparation method of a negative Poisson ratio bio-based rigid foam material and a product, belonging to the technical field of materials. According to the method, firstly, a bio-based rigid foam material is prepared by a supercritical fluid foaming technology, and then the bio-based rigid foam material is used as a raw material to prepare the negative Poisson's ratio bio-based rigid foam material by a heating-three-dimensional axial compression method. The method is simple and easy to operate, has low requirements on equipment, is low in cost and is suitable for expanded production. The foam material prepared by the method is light in weight and degradable, has excellent mechanical properties such as compression, shock resistance and the like, and has good application prospects in the fields of aerospace, automobiles, ships, encapsulation and the like.
Description
Technical Field
The invention belongs to the technical field of materials, and particularly relates to a preparation method and a product of a negative poisson's ratio bio-based rigid foam material.
Background
The foam material is integrally distributed with countless micropores which are mutually communicated or not communicated, so that the apparent density is obviously reduced, and the foam material has the advantages of high specific strength, light weight, good insulating, sound insulating and heat insulating properties and the like, and is widely applied to the fields of packaging and transportation, biomedical, aerospace, automobile parts and the like. In recent years, with the improvement of the requirements of related fields and industries on material lightweight and functionalization, researchers at home and abroad pay more attention to the preparation of novel polymer porous materials and the modification of polymer porous materials, and a large number of literature reports are made on the novel polymer porous materials, so that the polymer porous materials are rapidly developed. However, with the increasing prominence of energy and environmental problems and the increasing requirements for the related properties of polymer foams, the preparation of polymer porous materials by a non-pollution and environment-friendly processing and forming technology and the modification and enhancement of the properties of polymer foams are the trends of future development.
At present, the bio-based polymer materials which are most widely studied on bio-based foam materials are polylactic acid (PLA), polybutylene succinate (PBS), Polyhydroxyalkanoate (PHA), and the like, but because molecular chains of these bio-based polymer materials are linear, and main interactions between molecules are dominated by van der waals force, most of the foam materials using the bio-based polymer materials as a matrix are rigid foam materials, but the problems of high brittleness, poor compression performance and shock resistance, and other mechanical properties generally exist. In order to solve the problems, researchers at home and abroad perform physical blending modification, chemical grafting or copolymerization modification, ionic polymer copolymerization modification and the like on the bio-based material according to the theories of macromolecular chain physical crosslinking, chemical crosslinking and the like, and become the main research direction for solving the problem of poor mechanical properties of the bio-based rigid foam material at present.
Such as the Journal of Applied Polymer Science,2014,131(18), in which organic montmorillonite (OMMT) is used to improve the foaming properties of PLA/PBS blends. Mechanical testing was performed to compare the change in properties of the PLA/PBS foam before and after OMMT enhancement. The compression characteristics of PLA/PBS foam are discussed. X-ray diffraction (XRD) and scanning electron microscopy were performed to study the interaction between OMMT and PLA/PBS foam and the effect of OMMT on the cell structure. Polymers,2019,11(11):1852, by compounding Carbon Black (CB) with polybutylene succinate (PBS) to make PBS/CB complexes by supercritical CO2(ScCO2) Fluid foaming successfully produced a foam having a density of 0.107 to 0.344g/cm3Light, high strength and conductive polybutylene succinate (PBS/Carbon Black (CB) nanocomposite foam, and the research on PBS/CB nanocompositeMorphology, thermodynamic and dynamic mechanical properties and rheological behavior. Polymer,2019,185:121967, prepared by condensation polymerization of an ionic organic compound containing phosphoric acid groups and polybutylene succinate, researches the relationship between the content of the phosphoric acid ion groups (PCIG) in PBSIs microporous foams (FPBSIs-K) with different contents of the phosphoric acid ion groups (PCIG) and the structure and the performance of the FPBSIs-K, including thermal conductivity, compressive strength and thermal safety, and the foams are expected to have high thermal conductivity and compression property. Common to the above literature methods are:
1) other substances are introduced into the bio-based material, so that the degradation performance of the bio-based material is influenced, and the production cost is increased;
2) based on the theoretical basis of physical crosslinking or chemical crosslinking, the bio-based material is further processed, and the process is complex;
3) the bio-based material matrix is physically or chemically modified, so that the process flow is increased, and the production expansion difficulty is increased.
Therefore, the characteristics of the method are all limited in large-scale production of high-performance bio-based rigid foam materials from the industrial scale, and are not beneficial to industrialization. Therefore, the continuous research and development of other simple alternative methods to avoid complex processing and reduce production cost, and simultaneously, the mechanical property of the bio-based rigid foam material is still significant.
Disclosure of Invention
In view of the above, an object of the present invention is to provide a method for preparing a negative poisson's ratio bio-based rigid foam material; the other purpose is to provide a negative poisson's ratio bio-based rigid foam material.
In order to achieve the purpose, the invention provides the following technical scheme:
1. a method of making a negative poisson's ratio bio-based rigid foam material, the method comprising the steps of:
(1) placing a bio-based material in a high-pressure reaction kettle, sealing the high-pressure reaction kettle, introducing carbon dioxide until the air in the high-pressure reaction kettle is exhausted, continuously introducing the carbon dioxide until the pressure in the high-pressure reaction kettle is more than 7.5MPa, stopping introducing the carbon dioxide, heating to a temperature higher than the melting point of the bio-based material, keeping for 2-3h, then cooling to a temperature lower than the melting point of the bio-based material by 10-20 ℃, keeping for 10-15min, then instantly releasing pressure, taking out a product, and cooling to room temperature to obtain the bio-based rigid foam material;
(2) heating the bio-based rigid foam material prepared in the step (1) to a temperature between the softening temperature and the melting point of the bio-based material, keeping for 0.5-1h, and then compressing the bio-based rigid foam material in the axial direction and the circumferential direction to obtain the negative Poisson ratio bio-based rigid foam material.
Preferably, in the step (1), the bio-based material is one of polybutylene succinate, polylactic acid, polyhydroxyalkanoate, or bio-based polyurethane.
Preferably, in the step (1), the inner cavity of the high-pressure reaction kettle is cylindrical.
Preferably, in step (1), the instantaneous pressure relief is specifically: the pressure in the autoclave was reduced to atmospheric level within 3 s.
Preferably, in the step (2), the compression rate in both the axial direction and the circumferential direction is 10 to 30%.
2. A negative poisson's ratio bio-based rigid foam material produced by the method.
The invention has the beneficial effects that: the invention provides a preparation method and a product of a negative Poisson ratio bio-based rigid foam material, and the foam material is light in weight and degradable, has excellent mechanical properties such as compression, shock resistance and the like, and has a good application prospect in the fields of aerospace, automobiles, ships, encapsulation and the like. Wherein, when the bio-based rigid foam material is prepared, the heating is limited to be heated to the temperature above the melting point of the bio-based material and then is kept for 2-3h, so that the saturation amount of carbon dioxide in the bio-based material can be ensured, further ensuring the aperture ratio of the bio-based rigid foam material prepared in the later stage, limiting the temperature reduction to 10-20 ℃ below the melting point of the high bio-based material in the later stage, keeping for 10-15min, then instantly releasing the pressure, can ensure that the bio-based rigid foam material prepared in the later stage has proper aperture ratio, narrower aperture distribution (100-250 mu m) and aperture uniformity, therefore, the defect of cell damage caused by a large amount of broken cell walls can be well avoided when heating-three-dimensional axial compression is carried out at the later stage, and the finally prepared negative Poisson's ratio bio-based rigid foam material has excellent mechanical properties such as compression, shock resistance and the like. The preparation method of the foam material is simple and easy to operate, has low requirements on equipment, is low in cost, and is suitable for expanded production.
Additional advantages, objects, and features of the invention will be set forth in part in the description which follows and in part will become apparent to those having ordinary skill in the art upon examination of the following or may be learned from practice of the invention. The objectives and other advantages of the invention may be realized and attained by the means of the instrumentalities and combinations particularly pointed out hereinafter.
Drawings
For the purposes of promoting a better understanding of the objects, aspects and advantages of the invention, reference will now be made to the following detailed description taken in conjunction with the accompanying drawings in which:
FIG. 1 is an SEM image of bio-based rigid foam and negative Poisson's ratio bio-based rigid foam of example 1;
FIG. 2 is a graph of the shock resistance of the bio-based rigid foam and the bio-based rigid foam with a negative Poisson's ratio in the constant temperature frequency conversion mode of the dynamic mechanical analyzer in example 1;
FIG. 3 is a stress-strain plot of the bio-based rigid foam and the negative Poisson ratio bio-based rigid foam of example 1.
Detailed Description
The embodiments of the present invention are described below with reference to specific embodiments, and other advantages and effects of the present invention will be easily understood by those skilled in the art from the disclosure of the present specification. The invention is capable of other and different embodiments and of being practiced or of being carried out in various ways, and its several details are capable of modification in various respects, all without departing from the spirit and scope of the present invention.
Example 1
Preparation of negative Poisson ratio bio-based rigid foam material
(1) Placing polybutylene succinate in a high-pressure reaction kettle with a cylindrical inner cavity, sealing the high-pressure reaction kettle, introducing carbon dioxide into the high-pressure reaction kettle, exhausting air in the high-pressure reaction kettle, continuously introducing the carbon dioxide into the high-pressure reaction kettle until the pressure is 8MPa, stopping introducing the carbon dioxide, heating to 120 ℃, keeping for 2 hours, then cooling to 96 ℃, keeping for 10 minutes, reducing the pressure in the high-pressure reaction kettle to the atmospheric pressure level within 3 seconds, taking out a product, and cooling to room temperature to obtain the bio-based rigid foam material;
(2) heating the bio-based rigid foam material prepared in the step (1) to 102 ℃, keeping the temperature for 0.5h, and then compressing the bio-based rigid foam material in the axial direction and the circumferential direction, wherein the axial compression ratio is 30%, and the circumferential compression ratio is 17%, so that the bio-based rigid foam material with a Poisson ratio of-0.2 is obtained.
Example 2
Preparation of negative Poisson ratio bio-based rigid foam material
(1) Placing polylactic acid in a high-pressure reaction kettle with a cylindrical inner cavity, sealing the high-pressure reaction kettle, introducing carbon dioxide into the high-pressure reaction kettle, exhausting air in the high-pressure reaction kettle, continuously introducing the carbon dioxide until the pressure in the high-pressure reaction kettle is 9MPa, stopping introducing the carbon dioxide, heating to 170 ℃, keeping for 3h, then cooling to 155 ℃, keeping for 12min, reducing the pressure in the high-pressure reaction kettle to the atmospheric pressure level within 3s, taking out a product, and cooling to room temperature to obtain the bio-based rigid foam material;
(2) heating the bio-based rigid foam material prepared in the step (1) to 55 ℃, keeping the temperature for 0.5h, and then compressing the bio-based rigid foam material in the axial direction and the circumferential direction, wherein the axial compression ratio is 10%, and the circumferential compression ratio is 30%, so that the bio-based rigid foam material with the Poisson ratio of-0.18 is obtained.
Example 3
Preparation of negative Poisson ratio bio-based rigid foam material
(1) Placing polyhydroxyalkanoate in a high-pressure reaction kettle with a cylindrical inner cavity, sealing the high-pressure reaction kettle, introducing carbon dioxide into the high-pressure reaction kettle, exhausting air, continuously introducing the carbon dioxide into the high-pressure reaction kettle until the pressure in the high-pressure reaction kettle is 8.5MPa, stopping introducing the carbon dioxide, heating to 180 ℃, keeping for 2.5h, then cooling to 168 ℃, keeping for 15min, reducing the pressure in the high-pressure reaction kettle to the atmospheric pressure level within 3s, taking out a product, and cooling to room temperature to obtain the bio-based rigid foam material;
(2) heating the bio-based rigid foam material prepared in the step (1) to 110 ℃, keeping the temperature for 1h, and then compressing the bio-based rigid foam material in the axial direction and the circumferential direction, wherein the axial compression ratio is 20%, and the circumferential compression ratio is 10%, so that the bio-based rigid foam material with the Poisson ratio of-0.12 is obtained.
FIG. 1 is an SEM image of bio-based rigid foam and bio-based rigid foam with negative Poisson's ratio in example 1, wherein the left image is an SEM image of bio-based rigid foam in example 1, and it can be seen that the bio-based rigid foam has a net topology, the cells of the net topology are circular, the pore size is distributed between 100-250 μm, and the net topology has high closed cell rate, and the unique structures make the bio-based rigid foam have excellent performances in impact strength, toughness, fatigue resistance, etc.; the right figure is an SEM (scanning electron microscope) figure of the negative Poisson ratio bio-based rigid foam material in example 1, and it can be known that the negative Poisson ratio bio-based rigid foam material not only has a net topology structure, but also has a cell structure which is changed compared with the bio-based rigid foam material, and is changed from a circular shape to an irregular shape with cell walls folded inwards for multiple times, and the special cell structure causes a macroscopic "auxetic effect", namely a negative Poisson ratio effect, of the negative Poisson ratio bio-based rigid foam material, and finally causes the performance of the negative Poisson ratio bio-based rigid foam material in the aspects of impact strength, toughness, fatigue resistance and the like to be further enhanced.
FIG. 2 is a graph of the shock resistance of the bio-based rigid foam and the negative Poisson ratio bio-based rigid foam in example 1 in the constant temperature frequency conversion mode of the dynamic mechanical analyzer, and it can be seen from FIG. 2 that the bio-based rigid foam and the negative Poisson ratio bio-based rigid foam show different shock resistance in the constant temperature frequency conversion compression mode, and the loss modulus of the bio-based rigid foam varies greatly and is much higher than that of the negative Poisson ratio bio-based rigid foam in the range of 0-100 Hz; the loss modulus of the negative Poisson ratio bio-based rigid foam material changes nearly to a straight line with small change. The smaller the loss modulus, the smaller the damping loss factor of the material, and the closer the material is to the ideal elastic material, so that the negative Poisson ratio bio-based rigid foam material has better buffering performance and shock resistance than the bio-based rigid foam material.
Fig. 3 is a stress-strain graph of bio-based rigid foam and negative poisson's ratio bio-based rigid foam of example 1. as can be seen from fig. 3, negative poisson's ratio bio-based rigid foam requires more stress for the same strain, and negative poisson's ratio bio-based rigid foam has higher stiffness and better compressive properties than bio-based rigid foam.
Finally, the above embodiments are only intended to illustrate the technical solutions of the present invention and not to limit the present invention, and although the present invention has been described in detail with reference to the preferred embodiments, it will be understood by those skilled in the art that modifications or equivalent substitutions may be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions, and all of them should be covered by the claims of the present invention.
Claims (6)
1. A method for preparing a negative poisson's ratio bio-based rigid foam material, the method comprising the steps of:
(1) placing a bio-based material in a high-pressure reaction kettle, sealing the high-pressure reaction kettle, introducing carbon dioxide until the air in the high-pressure reaction kettle is exhausted, continuously introducing the carbon dioxide until the pressure in the high-pressure reaction kettle is more than 7.5MPa, stopping introducing the carbon dioxide, heating to a temperature higher than the melting point of the bio-based material, keeping for 2-3h, then cooling to a temperature lower than the melting point of the bio-based material by 10-20 ℃, keeping for 10-15min, then instantly releasing pressure, taking out a product, and cooling to room temperature to obtain the bio-based rigid foam material;
(2) heating the bio-based rigid foam material prepared in the step (1) to a temperature between the softening temperature and the melting point of the bio-based material, keeping for 0.5-1h, and then compressing the bio-based rigid foam material in the axial direction and the circumferential direction to obtain the negative Poisson ratio bio-based rigid foam material.
2. The method of claim 1, wherein in step (1), the bio-based material is one of polybutylene succinate, polylactic acid, polyhydroxyalkanoate, or bio-based polyurethane.
3. The method of claim 1, wherein in step (1), the autoclave has a cylindrical inner cavity.
4. The method according to claim 1, wherein in step (1), the instantaneous pressure relief is specifically: the pressure in the autoclave was reduced to atmospheric level within 3 s.
5. The method according to claim 1, wherein in the step (2), the compression is performed with a compression ratio of 10 to 30% in both the axial direction and the circumferential direction.
6. A negative Poisson's ratio bio-based rigid foam prepared by the method of any of claims 1-5.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113708659A (en) * | 2021-08-27 | 2021-11-26 | 重庆纳研新材料科技有限公司 | Application of composite negative Poisson's ratio structural material in enhancing friction power generation performance |
| CN113831695A (en) * | 2021-09-07 | 2021-12-24 | 广州纳研新材料科技有限公司 | Preparation method of environment-friendly light negative Poisson ratio flexible piezoresistive sensing metamaterial, product and application thereof |
| CN115403903A (en) * | 2022-10-10 | 2022-11-29 | 吉林省博砚科技有限公司 | Foam material with negative Poisson's ratio and preparation method thereof |
| CN115433386A (en) * | 2022-10-10 | 2022-12-06 | 吉林省博砚科技有限公司 | Negative Poisson's ratio polylactic acid foam material and preparation method thereof |
| CN115521596A (en) * | 2022-10-10 | 2022-12-27 | 吉林省博砚科技有限公司 | Polyhydroxyalkanoate auxetic foam and preparation method thereof |
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| CN115521596B (en) * | 2022-10-10 | 2023-06-23 | 吉林省博砚科技有限公司 | Polyhydroxyalkanoate auxetic foam and preparation method thereof |
| CN115433386B (en) * | 2022-10-10 | 2023-10-27 | 吉林省博砚科技有限公司 | Negative poisson ratio polylactic acid foam material and preparation method thereof |
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Effective date of registration: 20221117 Address after: 400023 10-3, Building 4, No. 36, Wulidian, Jiangbei District, Chongqing Patentee after: Huang Yi Address before: 401147 floor 20, building 5, Xingmao Shengshi Beichen, No. 6, bailing Road, Longshan street, Yubei District, Chongqing Patentee before: CHONGQING NAYAN NEW MATERIAL TECHNOLOGY CO.,LTD. |
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Effective date of registration: 20230531 Address after: 402760 No.92 Donglin Avenue, Biquan street, Bishan District, Chongqing Patentee after: Carbon Heng (Chongqing) Biomass New Materials Co.,Ltd. Address before: 400023 10-3, Building 4, No. 36, Wulidian, Jiangbei District, Chongqing Patentee before: Huang Yi |