CN115433386B - Negative poisson ratio polylactic acid foam material and preparation method thereof - Google Patents
Negative poisson ratio polylactic acid foam material and preparation method thereof Download PDFInfo
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- CN115433386B CN115433386B CN202211233919.6A CN202211233919A CN115433386B CN 115433386 B CN115433386 B CN 115433386B CN 202211233919 A CN202211233919 A CN 202211233919A CN 115433386 B CN115433386 B CN 115433386B
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- 229920000747 poly(lactic acid) Polymers 0.000 title claims abstract description 63
- 239000004626 polylactic acid Substances 0.000 title claims abstract description 63
- 239000006261 foam material Substances 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 238000006243 chemical reaction Methods 0.000 claims abstract description 74
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 42
- 238000002844 melting Methods 0.000 claims abstract description 28
- 230000008018 melting Effects 0.000 claims abstract description 28
- 239000000463 material Substances 0.000 claims abstract description 24
- 229910052786 argon Inorganic materials 0.000 claims abstract description 21
- 239000006260 foam Substances 0.000 claims abstract description 17
- 238000010438 heat treatment Methods 0.000 claims abstract description 15
- 238000001816 cooling Methods 0.000 claims abstract description 14
- DIOQZVSQGTUSAI-UHFFFAOYSA-N decane Chemical compound CCCCCCCCCC DIOQZVSQGTUSAI-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000000203 mixture Substances 0.000 claims abstract description 6
- 239000000654 additive Substances 0.000 claims abstract description 5
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical group CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 claims description 12
- SNRUBQQJIBEYMU-UHFFFAOYSA-N dodecane Chemical compound CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 7
- 229910001649 dickite Inorganic materials 0.000 claims description 4
- 229910052625 palygorskite Inorganic materials 0.000 claims description 4
- 239000000843 powder Substances 0.000 claims description 4
- 230000000996 additive effect Effects 0.000 claims description 2
- 239000012752 auxiliary agent Substances 0.000 claims description 2
- 238000002156 mixing Methods 0.000 abstract description 2
- 230000000694 effects Effects 0.000 description 6
- 230000006835 compression Effects 0.000 description 4
- 238000007906 compression Methods 0.000 description 4
- 239000010410 layer Substances 0.000 description 4
- 238000009413 insulation Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 230000001681 protective effect Effects 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008602 contraction Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/04—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
- C08J9/12—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a physical blowing agent
- C08J9/14—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a physical blowing agent organic
- C08J9/141—Hydrocarbons
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/0066—Use of inorganic compounding ingredients
- C08J9/0071—Nanosized fillers, i.e. having at least one dimension below 100 nanometers
-
- 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
- C08J2201/00—Foams characterised by the foaming process
- C08J2201/02—Foams characterised by the foaming process characterised by mechanical pre- or post-treatments
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2203/00—Foams characterized by the expanding agent
- C08J2203/14—Saturated hydrocarbons, e.g. butane; Unspecified hydrocarbons
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- 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
Abstract
The invention relates to a polylactic acid foam material with negative poisson ratio and a preparation method thereof, comprising the following steps: uniformly mixing polylactic acid, decane, additives and auxiliaries according to a proportion, and placing the mixture in a reaction kettle; argon is introduced into the reaction kettle, air is exhausted, the reaction kettle is closed, and the reaction kettle is heated to 10-15 ℃ below the melting point of polylactic acid; argon in the reaction kettle is pumped out, and the vacuum degree reaches-75 Kpa to-85 Kpa; heating to the melting point of polylactic acid, and preserving heat for 2-5 hours; slowly cooling to 100-120 ℃ below the melting point of polylactic acid, vacuumizing the reaction kettle again, and then introducing argon into the reaction kettle to enable the pressure to reach 3-6 MPa; heating the reaction kettle to the melting point of the polylactic acid, preserving heat for 4-9 hours, and then slowly cooling and decompressing to obtain the polylactic acid foam material with negative poisson ratio. The negative poisson ratio in the material is consistent, the same auxetic foam structure is generated, and the phenomenon that the foam surface and the internal structure are inconsistent due to mechanical pressurization is effectively avoided.
Description
Technical Field
The invention relates to a negative poisson ratio material and a preparation method thereof, in particular to a negative poisson ratio polylactic acid foam material and a preparation method thereof.
Background
Poisson's ratio refers to the ratio of the transverse shrinkage strain to the longitudinal tensile strain of a material when it is in unidirectional tension or compression. In most materials, poisson's ratio is generally positive, while negative poisson's ratio refers to expansion in the transverse direction when stretched and contraction in the transverse direction when compressed, mainly due to the specificity of its internal structure. The negative poisson ratio material has unique advantages such as high notch resistance, fracture resistance, high shear modulus, high rebound toughness, high energy absorption performance and the like, and has wide application prospects in the aspects of cushioning materials, sports protection equipment, fastener manufacturing or safety belts and the like.
The foam material is fully distributed with numerous mutually communicated or non-communicated micropores so as to obviously reduce the apparent density, has the advantages of high specific strength, light weight, good insulation, sound insulation and heat insulation performances and the like, and is widely applied to various fields of packaging and transportation, biomedical treatment, aerospace, automobile parts and the like. In recent years, with the improvement of the requirements of the related fields and industries on sports protective materials, related researchers at home and abroad pay attention to the preparation of novel auxetic foam with negative poisson ratio, and a great deal of research is carried out on the novel auxetic foam with negative poisson ratio, so that the auxetic foam with negative poisson ratio is rapidly developed. In the preparation methods of the novel negative poisson ratio foam materials disclosed at present, a common method is to obtain the negative poisson ratio foam materials by taking the positive poisson ratio foam materials as base materials, and carrying out steps such as mechanical compression, heating and the like on the positive poisson ratio foam materials. However, during mechanical compression, the surface and the interior of the compressed foam are not consistent due to the influence of foam pressure conduction, and the surface and the interior poisson ratio values of the negative poisson ratio foam materials can be different, so that the overall performance of the materials is influenced; meanwhile, mechanical compression also changes the performance of the foam material, and influences the use effect.
The polylactic acid foam material is a novel biodegradable material, has environmental protection property, can be used as a substitute material of fossil fuel-based plastic material, and has wide application prospect. However, the existing polylactic acid foam does not have a negative poisson ratio effect, and the polylactic acid foam material with the negative poisson ratio effect prepared by the existing method has the defects of uneven structure and inconsistent negative poisson ratio of the inner layer and the outer layer.
Disclosure of Invention
In order to solve the technical problems, the invention provides a preparation method of a polylactic acid foam material with negative poisson ratio, which comprises the following steps:
polylactic acid, decane, additives and assistants are mixed according to the mass ratio of 80-100: 15-40: 3-8: 5-27, and placing the mixture in a reaction kettle;
argon is introduced into the reaction kettle, the air in the reaction kettle is exhausted, the reaction kettle is closed, and the reaction kettle is heated to 10-15 ℃ below the melting point of polylactic acid;
argon in the reaction kettle is pumped out, so that the relative vacuum degree in the reaction kettle reaches-75 Kpa to-85 Kpa; heating to the melting point of polylactic acid, and preserving heat for 2-5 hours;
then slowly cooling to 100-120 ℃ below the melting point of polylactic acid at the speed of 0.5-1 ℃/min, vacuumizing the reaction kettle again, and then introducing argon into the reaction kettle to ensure that the pressure in the reaction kettle reaches 3-6 MPa;
heating the reaction kettle to the melting point of the polylactic acid, preserving heat for 4-9 hours, then slowly cooling at the speed of 0.5-1 ℃/min, and releasing pressure to normal temperature and normal pressure to obtain the polylactic acid foam material with negative poisson ratio.
The additive is nano dickite or nano palygorskite powder, and the average grain diameter is smaller than 300 nanometers; the auxiliary agent is n-heptane or dodecane.
The polylactic acid foam material with the negative poisson ratio is prepared by the preparation method; the negative poisson ratio of the negative poisson ratio polylactic acid foam material is between-0.3 and-0.7.
The invention has the beneficial effects that:
compared with the existing preparation method of the negative poisson ratio foam material, the novel preparation method of the negative poisson ratio polylactic acid foam is developed, the preparation process is optimized in terms of technology, the material is uniformly pressurized by means of air pressure without mechanical pressurization, and the concave structural unit of the auxetic foam is formed in the polymerization process of the polylactic acid monomer by matching with high-temperature treatment, so that the polylactic acid foam has the characteristic of negative poisson ratio; because the invention adopts gas pressurization to replace mechanical pressurization, in the process of forming the polylactic acid foam with negative poisson ratio, the internal and external structures of the material are uniform and consistent, the same auxetic foam structure is generated, and the phenomenon of inconsistent foam surface and internal structure caused by mechanical pressurization is effectively avoided; the negative poisson ratio polylactic acid foam prepared by the preparation method has excellent negative poisson ratio effect, the surface and the internal poisson ratio values of the material are the same, the internal pore size of the material is uniform, the porosity is higher, and the dimensional change of the material in the stretching and compressing processes is facilitated; the material can be used for manufacturing precision equipment such as biomedical and aerospace, and also can be used as a sports protective tool material for manufacturing sports protective tools, and comprises the following components: good stretching effect, strong impact resistance, light weight and the like.
Detailed Description
Example 1,
Polylactic acid (6 ten thousand molecular weight), decane, nano dickite (average grain diameter is less than 300 nanometers) and n-heptane are mixed according to the mass ratio of 80:40:3:27, and placing the mixture in a reaction kettle;
argon is introduced into the reaction kettle, the air in the reaction kettle is exhausted, the reaction kettle is closed, and the reaction kettle is heated to 10 ℃ below the melting point of polylactic acid;
argon in the reaction kettle is pumped out, so that the relative vacuum degree in the reaction kettle reaches 75Kpa below zero; heating to the melting point of polylactic acid, and preserving heat for 3 hours;
then slowly cooling to 100 ℃ below the melting point of the polylactic acid at the speed of 0.5 ℃/min, vacuumizing the reaction kettle again, and then introducing argon into the reaction kettle to enable the pressure in the reaction kettle to reach 6MPa;
heating the reaction kettle to the melting point of the polylactic acid, preserving heat for 5 hours, then slowly cooling at the speed of 1 ℃/min, and releasing pressure to normal temperature and normal pressure to obtain the polylactic acid foam material with negative poisson ratio.
EXAMPLE 2,
Polylactic acid (6 ten thousand molecular weight), decane, nano palygorskite powder (average grain diameter is smaller than 300 nanometers) and n-heptane are mixed according to the mass ratio of 100:15:8:5, uniformly mixing the materials in proportion, and placing the materials in a reaction kettle;
argon is introduced into the reaction kettle, the air in the reaction kettle is exhausted, the reaction kettle is closed, and the reaction kettle is heated to 12 ℃ below the melting point of polylactic acid;
argon in the reaction kettle is pumped out, so that the relative vacuum degree in the reaction kettle reaches-85 Kpa; heating to the melting point of polylactic acid, and preserving heat for 5 hours;
then slowly cooling to 120 ℃ below the melting point of the polylactic acid at the speed of 0.5 ℃/min, vacuumizing the reaction kettle again, and then introducing argon into the reaction kettle to enable the pressure in the reaction kettle to reach 5MPa;
heating the reaction kettle to the melting point of the polylactic acid, preserving heat for 8 hours, then slowly cooling at the speed of 1 ℃/min, and releasing pressure to normal temperature and normal pressure to obtain the polylactic acid foam material with negative poisson ratio.
EXAMPLE 3,
Polylactic acid (6 ten thousand molecular weight), decane, nano dickite (average grain diameter is less than 300 nanometers) and dodecane are mixed according to the mass ratio of 90:20:5:19, and placing the mixture in a reaction kettle;
argon is introduced into the reaction kettle, the air in the reaction kettle is exhausted, the reaction kettle is closed, and the reaction kettle is heated to 15 ℃ below the melting point of polylactic acid;
argon in the reaction kettle is pumped out, so that the relative vacuum degree in the reaction kettle reaches-80 Kpa; heating to the melting point of polylactic acid, and preserving heat for 2 hours;
then slowly cooling to 110 ℃ below the melting point of the polylactic acid at the speed of 0.5 ℃/min, vacuumizing the reaction kettle again, and then introducing argon into the reaction kettle to enable the pressure in the reaction kettle to reach 4MPa;
heating the reaction kettle to the melting point of the polylactic acid, preserving heat for 9 hours, then slowly cooling at the speed of 1 ℃/min, and releasing pressure to normal temperature and normal pressure to obtain the polylactic acid foam material with negative poisson ratio.
EXAMPLE 4,
Polylactic acid (6 ten thousand molecular weight), decane, nano palygorskite powder (average grain diameter is smaller than 300 nanometers) and dodecane are mixed according to a mass ratio of 85:25:4:21, and placing the mixture in a reaction kettle;
argon is introduced into the reaction kettle, the air in the reaction kettle is exhausted, the reaction kettle is closed, and the reaction kettle is heated to 11 ℃ below the melting point of polylactic acid;
argon in the reaction kettle is pumped out, so that the relative vacuum degree in the reaction kettle reaches-85 Kpa; heating to the melting point of polylactic acid, and preserving heat for 4 hours;
then slowly cooling to 100 ℃ below the melting point of the polylactic acid at the speed of 0.5 ℃/min, vacuumizing the reaction kettle again, and then introducing argon into the reaction kettle to ensure that the pressure in the reaction kettle reaches 3MPa;
heating the reaction kettle to the melting point of the polylactic acid, preserving heat for 4 hours, then slowly cooling at the speed of 1 ℃/min, and releasing pressure to normal temperature and normal pressure to obtain the polylactic acid foam material with negative poisson ratio.
Poisson's ratio tests were carried out on the top and bottom layers of the polylactic acid foam materials prepared in examples 1 to 4, and the results are shown in table 1 below. From the results, it can be seen that all samples obtain a negative poisson ratio effect, i.e. the poisson ratio of the material is negative, and the poisson ratio values of the surface layer and the inner layer are consistent.
Poisson's ratio of the polymeric materials prepared in Table 1
| Sample of | Example 1 | Example 2 | Example 3 | Example 4 |
| Surface Poisson's ratio | -0.36 | -0.51 | -0.69 | -0.57 |
| Inner poisson's ratio | -0.35 | -0.49 | -0.68 | -0.55 |
Claims (4)
1. A preparation method of a polylactic acid foam material with negative poisson ratio is characterized by comprising the following steps: the method comprises the following steps:
polylactic acid, decane, additives and assistants are mixed according to the mass ratio of 80-100: 15-40: 3-8: 5-27, and placing the mixture in a reaction kettle; the auxiliary agent is n-heptane or dodecane;
argon is introduced into the reaction kettle, the air in the reaction kettle is exhausted, the reaction kettle is closed, and the reaction kettle is heated to 10-15 ℃ below the melting point of polylactic acid;
argon in the reaction kettle is pumped out, so that the relative vacuum degree in the reaction kettle reaches-75 Kpa to-85 Kpa; heating to the melting point of polylactic acid, and preserving heat for 2-5 hours;
then slowly cooling to 100-120 ℃ below the melting point of polylactic acid at the speed of 0.5-1 ℃/min, vacuumizing the reaction kettle again, and then introducing argon into the reaction kettle to ensure that the pressure in the reaction kettle reaches 3-6 MPa;
heating the reaction kettle to the melting point of the polylactic acid, preserving heat for 4-9 hours, then slowly cooling at the speed of 0.5-1 ℃/min, and releasing pressure to normal temperature and normal pressure to obtain the polylactic acid foam material with negative poisson ratio.
2. The method for preparing the polylactic acid foam material with the negative poisson ratio according to claim 1, which is characterized in that: the additive is nano dickite or nano palygorskite powder, and the average grain diameter is smaller than 300 nanometers.
3. A negative poisson's ratio polylactic acid foam prepared by the method of any of claims 1 or 2.
4. The negative poisson's ratio polylactic acid foam according to claim 3, wherein: the negative poisson ratio value of the negative poisson ratio polylactic acid foam material is between-0.3 and-0.7, and the internal and external structures of the material are uniform.
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