CN110607049A - Novel open-cell foam material and preparation method thereof - Google Patents
Novel open-cell foam material and preparation method thereof Download PDFInfo
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- CN110607049A CN110607049A CN201910928880.1A CN201910928880A CN110607049A CN 110607049 A CN110607049 A CN 110607049A CN 201910928880 A CN201910928880 A CN 201910928880A CN 110607049 A CN110607049 A CN 110607049A
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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
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/0061—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof characterized by the use of several polymeric components
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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
- C08J2205/00—Foams characterised by their properties
- C08J2205/04—Foams characterised by their properties characterised by the foam pores
- C08J2205/05—Open cells, i.e. more than 50% of the pores are open
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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
- C08J2345/00—Characterised by the use of homopolymers or copolymers of compounds having no unsaturated aliphatic radicals in side chain, and having one or more carbon-to-carbon double bonds in a carbocyclic or in a heterocyclic ring system; Derivatives of such polymers
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2409/00—Characterised by the use of homopolymers or copolymers of conjugated diene hydrocarbons
- C08J2409/06—Copolymers with styrene
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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
- C08J2423/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2423/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
- C08J2423/16—Ethene-propene or ethene-propene-diene copolymers
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Abstract
The novel open-cell foam material comprises the following raw material components in parts by weight: 100 parts of dicyclopentadiene, 0.1-3 parts of anti-aging agent, 0.1-3 parts of ultraviolet absorbent, 0.2-5 parts of tackifier and grubbs catalyst with the molar ratio of the dicyclopentadiene to the dicyclopentadiene of 1/100000-1/500. The preparation method comprises the following steps: dissolving the anti-aging agent in the dicyclopentadiene monomer at room temperature; dissolving an ultraviolet absorbent in the dicyclopentadiene monomer in the first step at room temperature; dissolving tackifier in the dicyclopentadiene monomer at room temperature; adding a certain proportion of catalyst solution into dicyclopentadiene monomer; pouring the obtained mixed solution into a mould, pumping for a period of time, carrying out vacuum heat preservation molding, cooling, and demoulding to obtain the open-cell foam material. The foam material obtained by the invention has the properties of high strength, low density, heat insulation and sound insulation; the production process is simple, the process is environment-friendly, and the operation is convenient.
Description
Technical Field
The invention relates to a foamed plastic, in particular to a novel open-cell foamed material and a preparation method thereof.
Background
Currently, the concept of material weight reduction is receiving more and more attention. In the case of polymeric materials, it is common to introduce a cellular structure within the material to replace the originally solid polymeric portion with gas bubbles in order to reduce the density of the material. The polymer foam material is a microporous material based on a polymer (plastic, rubber, elastomer, or natural polymer material) and having numerous bubbles inside, and can be considered as a composite material using a gas as a filler. The polymer foaming material with the holes has wide application in the fields of biology, medical treatment, environmental engineering and the like, and can be used for tissue engineering, solvent extraction, heat preservation and insulation, sound absorption, water stopping and retention, oil absorption, controlled drug release and the like.
The foaming technology of supercritical fluid (N2, CO2, etc.) has the advantages of green, no pollution, etc., and thus has been increasingly regarded as important in preparing porous tissue engineering scaffold materials. Taking supercritical carbon dioxide foaming as an example: the supercritical CO2 is firstly diffused and dissolved into the polymer matrix, and the acceleration effect of the supercritical CO2 can reduce the glass transition temperature of the polymer and make the glass transition temperature lower than the test temperature; then, due to the fact that the system is decompressed or heated, thermodynamic instability of the system is caused, and a large number of gas nuclei are formed and grow in the polymer matrix; in the process of cell growth, a large amount of gas diffuses into cells or escapes out of a polymer foaming system, so that the driving force for cell growth is continuously reduced, and simultaneously, the rigidity of a polymer matrix is gradually improved, and the two effects can inhibit cell growth, so that the cell structure is finally fixed. However, in the conventional supercritical fluid foaming process, because a large temperature gradient exists between the surface layer and the inside of the center of the polymer material, that is, the surface layer temperature is low, and the temperature inside the material is high, CO2 gas cannot be dissolved (or less dissolved) into the surface layer of the material, so that a compact and hard skin layer is formed on the surface, and the internal porous structure is wrapped, so that the surface of the polymer foaming material is difficult to open pores or has low opening rate, which severely restricts the application range of the foaming technology, and therefore, an improved scheme is urgently needed to overcome the defect.
Polydicyclopentadiene (PDCPD) material prepared by Ring-opening metathesis polymerization (ROMP) of dicyclopentadiene monomer (DCPD) under the action of catalyst is gradually developed into novel engineering plastic due to excellent mechanical property and low cost. The DCPD has two unsaturated rings, wherein a norbornene ring is opened to form a linear PDCPD chain, and a part of cyclopentene ring is opened to form a cross-linked network structure, so that the DCPD has high modulus and high impact strength. Industrially, thermosetting crosslinked PDCPD-RIM articles are mainly prepared by Reaction Injection Molding (RIM). In order to obtain a light PDCPD-based porous material, a number of researchers have conducted related studies. The PDCPD-based porous material inherits the characteristics of the PDCPD material, generally has higher mechanical strength, and has wider application prospect and market competitiveness. The preparation methods of PDCPD-based porous materials can be mainly summarized into the following types of sol-gel combined supercritical drying method, high internal phase emulsion method, chemical induced phase separation method and chemical foaming method. The method improves the foaming multiplying power of the PDCPD and enlarges the application range of the PDCPD; however, these methods have various disadvantages, mainly including the following aspects:
1) the preparation process is complex and the price is high;
2) a large amount of solvent is needed to pollute the environment;
3) a tungsten catalyst is mostly adopted, and the requirement on test conditions is severe;
4) the prepared porous material has obvious performance reduction and cannot highlight the high-strength characteristic of the PDCPD material;
5) the prepared porous material has peculiar smell.
The prior patent applications CN 104327436A and CN 107722243A both disclose a preparation method of polydicyclopentadiene foam material, which can reduce the density of the material on the basis of ensuring the high strength of the raw material; chemical foaming agents are used, the dissolubility of the foaming agents is relatively poor, and the foaming multiplying power is not easy to adjust.
Disclosure of Invention
The invention aims to provide a novel open-cell foam material and a preparation method thereof, the open-cell foam material is prepared by a PDCPD material self-foaming process, and the obtained foam material has the properties of high strength, low density, heat insulation and sound insulation; the production process is simple, the process is environment-friendly, the operation is convenient, and the method is suitable for large-scale industrial production and solves the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme: a novel open-cell foam material comprises the following raw material components in parts by weight: 100 parts of dicyclopentadiene, 0.1-3 parts of anti-aging agent, 0.1-3 parts of ultraviolet absorbent, 0.2-5 parts of tackifier and grubbs catalyst with the molar ratio of the dicyclopentadiene to the dicyclopentadiene of 1/100000-1/500.
Further, the anti-aging agent is one or a compound of more of bis (3, 5-di-tert-butyl-4-hydroxyphenyl) sulfide, 2, 6-di-tert-butyl-4-methylphenol, 2, 6-di-tert-butyl-p-cresol, tris (2, 4-di-tert-butylphenyl) phosphite and pentaerythritol tetrakis (beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate).
Further, the ultraviolet absorbent is one or a compound of more of UV-326, UV-1164, UV-531, UV-327, UV-360, UV-1157 and UV-234.
Further, the tackifier is any one or combination of more of styrene butadiene rubber, ethylene propylene diene monomer, ethylene propylene copolymer, ethylene vinyl acetate copolymer, styrene-butadiene block copolymer and chloroprene rubber.
Further, the grubbs catalyst is any one or combination of a first-generation grubbs catalyst and a second-generation grubbs catalyst.
The invention provides another technical scheme as follows: a preparation method of a novel open-cell foam material comprises the following steps:
the first step is as follows: dissolving the anti-aging agent in the dicyclopentadiene monomer at room temperature, and stirring for 3-5 min;
the second step is that: dissolving an ultraviolet absorbent in the dicyclopentadiene monomer in the first step at room temperature, and stirring for 3-5 min;
the third step: dissolving a tackifier in the dicyclopentadiene monomer obtained in the second step at room temperature, and stirring for 5-10 min;
the fourth step: adding a certain proportion of catalyst solution into the dicyclopentadiene monomer in the third step, and uniformly stirring for 2-3 min;
the fifth step: pouring the mixed liquid obtained in the fourth step into a mould, pumping for a period of time, carrying out vacuum heat preservation molding for 10min, cooling, and demoulding to obtain the open-cell foam material.
And the catalyst solution in the fourth step is prepared by proportioning a grubbs catalyst and a catalyst solution solvent.
Further, the catalyst solution solvent is any one combination of dichloromethane and toluene.
And further, the temperature of the die in the fifth step is 35-100 ℃, and the heat preservation time is 3-20 min.
Compared with the prior art, the invention has the beneficial effects that:
in the invention, a certain amount of anti-aging agent, ultraviolet absorbent and tackifier are dissolved in 1000mL of dicyclopentadiene monomer, and the mixture is uniformly stirred; adding a catalyst solution (dissolved in a dichloromethane or toluene solution) in a certain proportion into the monomer, and dispersing uniformly; pouring the mixture into a constant-temperature mold at a certain temperature, vacuumizing, reacting for a period of time, preserving heat in the mold for 10min, and then cooling and demolding to obtain the open-cell foamed PDCPD material, wherein the obtained PDCPD open-cell foamed material has the properties of high strength, low density, heat insulation and sound insulation; the production process is simple, the process is environment-friendly, the operation is convenient, and the method is suitable for large-scale industrial production.
Detailed Description
The following examples will explain the present invention in detail, but the present invention is not limited thereto. 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.
Example 1
A novel open-cell foam material and a preparation method thereof are as follows: dissolving 1% of 2, 6-di-tert-butyl-4-methylphenol in 1000mL of dicyclopentadiene monomer, stirring for 5min, dissolving 1% of UV-531 in the monomer in which the 2, 6-di-tert-butyl-4-methylphenol is dissolved, stirring for 4min, dissolving 1% of styrene butadiene rubber in the monomer in which the 2, 6-di-tert-butyl-4-methylphenol and UV-531 are dissolved, adding 1/10000grubbs catalyst solution (dissolved in dichloromethane or toluene solution), and uniformly stirring for 2 min; pouring into a mold with the temperature of 50 ℃, vacuumizing, reacting for 30min, preserving heat for 10min, cooling and demolding to obtain the open-cell foamed PDCPD material.
Example 2
Dissolving 0.5% bis (3, 5-di-tert-butyl-4-hydroxyphenyl) sulfide in 1000mL dicyclopentadiene monomer, stirring for 5min, dissolving 1% UV-326 in the monomer in which bis (3, 5-di-tert-butyl-4-hydroxyphenyl) sulfide is dissolved, stirring for 3min, dissolving 2% styrene-butadiene rubber in the monomer in which bis (3, 5-di-tert-butyl-4-hydroxyphenyl) sulfide and UV-326 are dissolved, stirring for 9min, adding 1/10000grubbs catalyst solution (dissolved in dichloromethane or toluene solution), and stirring uniformly for 3 min; pouring into a mold with the temperature of 50 ℃, vacuumizing, reacting for 30min, preserving heat for 10min, cooling and demolding to obtain the open-cell foamed PDCPD material.
Example 3
A novel open-cell foam material and a preparation method thereof are disclosed, wherein 0.5 percent of 2, 6-di-tert-butyl-4-methylphenol is dissolved in 1000mL of dicyclopentadiene monomer, the mixture is stirred for 4min, 2 percent of UV-326 is dissolved in the monomer dissolved with the 2, 6-di-tert-butyl-4-methylphenol, the mixture is stirred for 5min, 3 percent of styrene butadiene rubber is dissolved in the monomer dissolved with the 2, 6-di-tert-butyl-4-methylphenol and the UV-326, the mixture is stirred for 8min, 1/10000grubbs catalyst solution (dissolved in dichloromethane or toluene solution) is added, and the mixture is stirred uniformly for 3 min; pouring into a mold with the temperature of 50 ℃, vacuumizing, reacting for 30min, preserving heat for 10min, cooling and demolding to obtain the open-cell foamed PDCPD material.
Example 4
Dissolving 2% of 2, 6-di-tert-butyl-4-methylphenol in 1000mL of dicyclopentadiene monomer, stirring for 5min, dissolving 1% of UV-326 in the monomer in which the 2, 6-di-tert-butyl-4-methylphenol is dissolved, stirring for 5min, dissolving 5% of styrene-butadiene rubber in the monomer in which the 2, 6-di-tert-butyl-4-methylphenol and UV-326 are dissolved, stirring for 6min, adding 1/10000grubbs catalyst solution (dissolved in dichloromethane or toluene solution), and uniformly stirring for 3 min; pouring into a mold with the temperature of 50 ℃, vacuumizing, reacting for 30min, preserving heat for 10min, cooling and demolding to obtain the open-cell foamed PDCPD material.
Example 5
A novel open-cell foam material and a preparation method thereof are provided, wherein 2% of pentaerythritol tetra (beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate) is dissolved in 1000mL of dicyclopentadiene monomer, stirring is carried out for 5min, 1% of UV-326 is dissolved in the monomer dissolved with the pentaerythritol tetra (beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate), stirring is carried out for 3min, 2% of ethylene propylene copolymer is dissolved in the monomer dissolved with the pentaerythritol tetra (beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate) and the UV-326, stirring is carried out for 10min, 1/10000grubbs catalyst solution (dissolved in dichloromethane or toluene solution) is added, and stirring is carried out for 3 min; pouring into a mold with the temperature of 50 ℃, vacuumizing, reacting for 30min, preserving heat for 10min, cooling and demolding to obtain the open-cell foamed PDCPD material.
Example 6
A novel open-cell foam material and a preparation method thereof are provided, wherein 1% of pentaerythritol tetra (beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate) is dissolved in 1000mL of dicyclopentadiene monomer, stirring is carried out for 4min, 1% of UV-326 is dissolved in the monomer dissolved with the pentaerythritol tetra (beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate), stirring is carried out for 4min, 2% of ethylene propylene copolymer is dissolved in the monomer dissolved with the pentaerythritol tetra (beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate) and the UV-326, stirring is carried out for 6min, 1/100000grubbs catalyst solution (dissolved in dichloromethane or toluene solution) is added, and stirring is carried out for 3 min; pouring into a 70 ℃ mold, vacuumizing, reacting for 50min, keeping the temperature for 10min, cooling and demolding to obtain the open-cell foamed PDCPD material.
Example 7
A novel open-cell foam material and a preparation method thereof are disclosed, wherein 0.3% of pentaerythritol tetrakis (beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate) is dissolved in 1000mL of dicyclopentadiene monomer, the mixture is stirred for 5min, 2% of UV-944 is dissolved in the monomer in which the pentaerythritol tetrakis (beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate) is dissolved, the mixture is stirred for 5min, 2% of ethylene propylene copolymer is dissolved in the monomer in which the pentaerythritol tetrakis (beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate) and the UV-944 are dissolved, the mixture is stirred for 5min, 1/500grubbs catalyst solution (dissolved in dichloromethane or toluene solution) is added, and the mixture is stirred uniformly for 2 min; pouring into a mold with the temperature of 35 ℃, vacuumizing, reacting for 30min, preserving heat for 10min, cooling and demolding to obtain the open-cell foamed PDCPD material.
Comparative example
Dissolving 1% pentaerythritol tetrakis (beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate) in 1000mL dicyclopentadiene monomer, stirring for 5min, dissolving 1% UV-326 in the monomer dissolved with pentaerythritol tetrakis (beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate), stirring for 3min, dissolving 2% ethylene propylene copolymer in the monomer dissolved with pentaerythritol tetrakis (beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate) and UV-326, stirring for 5min, adding 1/10000grubbs catalyst solution (dissolved in dichloromethane or toluene solution), and stirring uniformly for 2 min; and (3) vacuumizing, pouring into a mold at 50 ℃, reacting for 30min, preserving heat for 10min, cooling and demolding to obtain the PDCPD material.
The PDCPD open-cell foamed material of the embodiment and the PDCPD material of the comparative example are subjected to performance test, and the test results are as follows:
TABLE 1 PDCPD open-cell foam of the examples and PDCPD material of the comparative examples test results
As the comparative example adopts the steps of firstly extracting vacuum and then pouring into the mould, while the invention firstly pours into the mould and then extracts vacuum, the PDCPD material of the comparative example has higher density, and the strength and the notch impact strength are weaker than those of the PDCPD open-cell foaming material of the embodiment, and the obtained PDCPD open-cell foaming material has the properties of high strength, low density, heat insulation and sound insulation; the production process is simple, the process is environment-friendly, the operation is convenient, and the method is suitable for large-scale industrial production.
In summary, the following steps: according to the novel open-cell foam material and the preparation method thereof, a certain amount of anti-aging agent, ultraviolet absorbent and tackifier are dissolved in 1000mL of dicyclopentadiene monomer, and the mixture is uniformly stirred; adding a catalyst solution (dissolved in a dichloromethane or toluene solution) in a certain proportion into the monomer, and dispersing uniformly; pouring the mixture into a constant-temperature mold at a certain temperature, vacuumizing, reacting for a period of time, preserving heat in the mold for 10min, and then cooling and demolding to obtain the open-cell foamed PDCPD material, wherein the obtained PDCPD open-cell foamed material has the properties of high strength, low density, heat insulation and sound insulation; the production process is simple, the process is environment-friendly, the operation is convenient, and the method is suitable for large-scale industrial production.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (9)
1. The novel open-cell foam material is characterized by comprising the following raw material components in parts by weight: 100 parts of dicyclopentadiene, 0.1-3 parts of anti-aging agent, 0.1-3 parts of ultraviolet absorbent, 0.2-5 parts of tackifier and grubbs catalyst with the molar ratio of the dicyclopentadiene to the dicyclopentadiene of 1/100000-1/500.
2. The open-cell foam material as claimed in claim 1, wherein the aging inhibitor is one or more of bis (3, 5-di-tert-butyl-4-hydroxyphenyl) sulfide, 2, 6-di-tert-butyl-4-methylphenol, 2, 6-di-tert-butyl-p-cresol, tris (2, 4-di-tert-butylphenyl) phosphite, and pentaerythritol tetrakis (β - (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate).
3. The novel open-cell foam material as claimed in claim 1, wherein the ultraviolet absorber is one or more of UV-326, UV-1164, UV-531, UV-327, UV-360, UV-1157 and UV-234.
4. The novel open-cell foam material as claimed in claim 1, wherein the tackifier is any one or more of styrene-butadiene rubber, ethylene-propylene-diene monomer rubber, ethylene-propylene copolymer, ethylene-vinyl acetate copolymer, styrene-butadiene block copolymer and chloroprene rubber.
5. The novel open-cell foam material of claim 1, wherein said grubbs catalyst is any one or combination of first generation and second generation grubbs catalysts.
6. A method for preparing a novel open-cell foamed material according to any one of claims 1 to 5, comprising the steps of:
the first step is as follows: dissolving the anti-aging agent in the dicyclopentadiene monomer at room temperature, and stirring for 3-5 min;
the second step is that: dissolving an ultraviolet absorbent in the dicyclopentadiene monomer in the first step at room temperature, and stirring for 3-5 min;
the third step: dissolving a tackifier in the dicyclopentadiene monomer obtained in the second step at room temperature, and stirring for 5-10 min;
the fourth step: adding a certain proportion of catalyst solution into the dicyclopentadiene monomer in the third step, and uniformly stirring for 2-3 min;
the fifth step: pouring the mixed liquid obtained in the fourth step into a mould, pumping for a period of time, carrying out vacuum heat preservation molding for 10min, cooling, and demoulding to obtain the open-cell foam material.
7. The method as claimed in claim 6, wherein the catalyst solution in the fourth step is prepared by mixing grubbs catalyst and catalyst solution solvent.
8. The method for preparing the novel open-cell foam material as claimed in claim 7, wherein the catalyst solution solvent is any one combination of dichloromethane and toluene.
9. The method for preparing the novel open-cell foam material according to claim 6, wherein the temperature of the mold in the fifth step is 35-100 ℃, and the holding time is 3-20 min.
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| CN112521706A (en) * | 2020-12-04 | 2021-03-19 | 广东聚航新材料研究院有限公司 | Deep sea solid buoyancy material and preparation method thereof |
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Application publication date: 20191224 |
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