CN111534078A - Temperature-resistant polyurethane-based rubber and preparation method thereof - Google Patents
Temperature-resistant polyurethane-based rubber and preparation method thereof Download PDFInfo
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- CN111534078A CN111534078A CN202010378255.7A CN202010378255A CN111534078A CN 111534078 A CN111534078 A CN 111534078A CN 202010378255 A CN202010378255 A CN 202010378255A CN 111534078 A CN111534078 A CN 111534078A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
- C08K13/06—Pretreated ingredients and ingredients covered by the main groups C08K3/00 - C08K7/00
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/16—Nitrogen-containing compounds
- C08K5/29—Compounds containing one or more carbon-to-nitrogen double bonds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/56—Organo-metallic compounds, i.e. organic compounds containing a metal-to-carbon bond
- C08K5/57—Organo-tin compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/22—Expanded, porous or hollow particles
- C08K7/24—Expanded, porous or hollow particles inorganic
- C08K7/26—Silicon- containing compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/02—Ingredients treated with inorganic substances
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
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Abstract
The invention relates to a temperature-resistant polyurethane rubber and a preparation method thereof, belonging to the field of polyurethane materials, the technical field of rubber performance improvement and the field of thermal protection materials. The invention aims to improve the temperature resistance and other comprehensive properties of polyurethane rubber, and adopts fumed silica treated by supercritical carbon dioxide, then adds the treated fumed silica into the polyurethane rubber, and tests the comprehensive properties, particularly the temperature resistance, of the polyurethane rubber added with the fumed silica.
Description
Technical Field
The invention relates to a temperature-resistant polyurethane rubber and a preparation method thereof, belonging to the field of polyurethane materials, the technical field of rubber performance improvement and the field of thermal protection materials. Temperature resistance means resistance to 150 ℃.
Background
The polyurethane rubber is a series of elastomer materials containing more urethane groups on a polymer main chain, and is actually polyurethane rubber, which is simply referred to as polyurethane rubber or urethane rubber or polyurethane elastomer. The polymer chain contains, in addition to urethane groups, ester groups, ether groups, urea groups, aromatic groups, aliphatic chains, and the like. The main advantages of polyurethane rubber are: has the advantages of good mechanical property (high hardness and good strength), good aging resistance (ozone resistance, radiation resistance and damp-heat resistance), good conductivity and the like, which cannot be compared with common rubber. Although the polyurethane rubber has many advantages, the polyurethane rubber has the defect of poor temperature resistance, the application range of the polyurethane rubber in a relatively high-temperature environment is obviously limited due to the fact that the using temperature ranges are about minus 30 ℃ to plus 80 ℃, at present, the polyurethane rubber is improved in temperature resistance by adding compounding agents, the common heat-resistant and heat-transfer compounding agents comprise asbestos powder, mica powder, graphite powder, carbon black, pottery clay, zinc oxide, magnesium carbonate and the like, and under special conditions, aluminum powder or lead powder can be used.
On the other hand, the fumed silica has porosity, is nontoxic, tasteless, pollution-free and high-temperature resistant, and simultaneously has chemical inertness and special thixotropic property, so that the tensile strength, the tear resistance and the wear resistance of the silicon rubber product are obviously improved, and the strength of the improved rubber is improved by tens of times. Although fumed silica has wide application in rubbers such as silicone rubber, it is rarely used in urethane rubber. This is mainly because the surface inertness of fumed silica is harder to mix with the polyurethane rubber, and because it is difficult to form a good interfacial bond and pin-anchor effect between the two. In addition, when carbon dioxide is heated above the critical temperature Tc of 31.26 ℃ and the critical pressure Pc of 72.9atm, the properties of carbon dioxide change, the density of carbon dioxide is close to liquid, the viscosity of carbon dioxide is close to gas, the diffusion coefficient of carbon dioxide is 100 times that of liquid, and thus the carbon dioxide has a surprising dissolving capacity, and at the same time, functional groups can be oxidized on the surface of substances, such as: hydroxyl, carboxyl, and carbonyl groups, and the like.
In the present invention, fumed silica is treated with supercritical carbon dioxide, and the treated fumed silica is added to urethane rubber, and then the urethane rubber is tested for comprehensive properties, particularly temperature resistance.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: overcomes the defects of the prior art and provides a temperature-resistant polyurethane-based rubber and a preparation method thereof.
The technical solution of the invention is as follows:
the raw materials of the temperature-resistant polyurethane-based rubber comprise a polyurethane rubber matrix, a vulcanizing agent, a filler and a catalyst; the mass of the filler is 25-45% of that of the polyurethane rubber matrix; the mass ratio of the vulcanizing agent to the polyurethane rubber matrix is 1: 5-7; the mass of the catalyst is 0.05-0.25% of that of the polyurethane rubber matrix;
the polyurethane rubber substrate is polyurethane rubber AU2200 or polyurethane rubber EU 2400;
the vulcanizing agent is toluene diisocyanate;
the filler is fumed silica treated by supercritical carbon dioxide;
the catalyst is dibutyltin dilaurate;
the method for treating the fumed silica by the supercritical carbon dioxide comprises the following steps: treating for 2-3 h at the temperature of 100-150 ℃ and under the pressure of 18-20 MPa.
A preparation method of temperature-resistant polyurethane-based rubber comprises the following steps:
firstly, mixing and stirring the filler and the polyurethane rubber matrix at the stirring speed of 200-300 revolutions per minute for 10-20min to obtain a mixture;
secondly, adding a vulcanizing agent into the mixture obtained in the first step, and stirring at the stirring speed of 100-;
and thirdly, adding a catalyst into the temperature-resistant polyurethane-based rubber raw rubber obtained in the second step, stirring at the stirring speed of 100-200 revolutions per minute for 10-15min, and then heating at the heating temperature of 60-70 ℃ for 10-20min to obtain the temperature-resistant polyurethane-based rubber.
And curing the obtained crude rubber of the temperature-resistant polyurethane-based rubber by using dibutyltin dilaurate as a catalyst to obtain the temperature-resistant polyurethane-based rubber.
The comprehensive performance, especially the temperature resistance, of the obtained temperature-resistant polyurethane-based rubber is tested. The temperature resistance is determined by taking the highest temperature when the tensile strength begins to reduce as the upper temperature use limit, the hardness test adopts the measurement of the hardness of GB/T6031-1998 vulcanized rubber or thermoplastic rubber, the strength test adopts the measurement of the tensile stress strain performance of GB/T528-1998 vulcanized rubber or thermoplastic rubber, and the ozone aging resistance and the air aging resistance adopt the GB/T7762-2003 vulcanized rubber or thermoplastic rubber ozone crack resistance static tensile test and the GB/T3512-2001 vulcanized rubber or thermoplastic rubber hot air accelerated aging and heat resistance test respectively. In the current invention, the test analysis is for comparison, so the rubber synthesized in the first step has 100% performance, and the increase or decrease is relative percentage.
Advantageous effects
The invention aims to improve the temperature resistance and other comprehensive properties of polyurethane rubber, and adopts fumed silica treated by supercritical carbon dioxide, then adds the treated fumed silica into the polyurethane rubber, and tests the comprehensive properties, particularly the temperature resistance, of the polyurethane rubber added with the fumed silica.
Detailed Description
The invention is further illustrated by the following examples, without restricting its application to the examples given.
1. AU2200 and EU2400 and toluene diisocyanate are main rubber bodies, usually 5 parts of AU2200 and 1 part of toluene diisocyanate are mixed to form polyurethane rubber with better comprehensive performance, usually 7 parts of EU2400 and 1 part of toluene diisocyanate are mixed to form polyurethane rubber with better comprehensive performance, the comprehensive performance of the polyurethane rubber is tested, and then fumed silica which is not subjected to supercritical treatment is added and the comprehensive performance of the polyurethane rubber added with the fumed silica which is not subjected to supercritical treatment is tested;
2. supercritical carbon dioxide at 100 deg.C and 180atm (Tc 31.26 deg.C, Pc 72.9atm) for 2 h;
3. adding the treated fumed silica into the polyurethane rubber, wherein the adding proportion of the fumed silica to the polyurethane rubber is 25%;
4. and testing the comprehensive performance, particularly the temperature resistance, of the polyurethane rubber after the fumed silica is mixed. The temperature resistance is determined by taking the highest temperature when the tensile strength begins to reduce as the upper temperature use limit, the hardness test adopts the measurement of the hardness of GB/T6031-1998 vulcanized rubber or thermoplastic rubber, the strength test adopts the measurement of the tensile stress strain performance of GB/T528-1998 vulcanized rubber or thermoplastic rubber, and the ozone aging resistance and the air aging resistance adopt the GB/T7762-2003 vulcanized rubber or thermoplastic rubber ozone crack resistance static tensile test and the GB/T3512-2001 vulcanized rubber or thermoplastic rubber hot air accelerated aging and heat resistance test respectively.
Example 1
A preparation method of temperature-resistant polyurethane-based rubber comprises the following steps:
firstly, mixing 25g of fumed silica treated by supercritical carbon dioxide with 100g of polyurethane rubber AU2200, and stirring at the stirring speed of 200 revolutions per minute for 20min to obtain a mixture; the method for treating the fumed silica by the supercritical carbon dioxide comprises the following steps: treating at 100 deg.C under 20MPa for 2 hr;
and secondly, adding 20g of toluene diisocyanate into the mixture obtained in the first step, and stirring at the stirring speed of 100 revolutions per minute for 20 minutes to obtain the heat-resistant polyurethane-based rubber raw rubber.
And thirdly, adding 0.15g of dibutyltin dilaurate into the temperature-resistant polyurethane-based rubber crude rubber obtained in the second step, stirring at the stirring speed of 100 revolutions per minute for 10min, and then heating at the heating temperature of 60 ℃ for 10min to obtain the temperature-resistant polyurethane-based rubber.
Example 2
A preparation method of temperature-resistant polyurethane-based rubber comprises the following steps:
step one, mixing 25g of fumed silica treated by supercritical carbon dioxide with 100g of polyurethane rubber EU2400, and stirring at the stirring speed of 200 revolutions per minute for 20min to obtain a mixture; the method for treating the fumed silica by the supercritical carbon dioxide comprises the following steps: treating at 100 deg.C under 20MPa for 2 hr;
and secondly, adding 14.3g of toluene diisocyanate into the mixture obtained in the first step, and stirring at the stirring speed of 100 revolutions per minute for 20 minutes to obtain the heat-resistant polyurethane-based rubber raw rubber.
And thirdly, adding 0.15g of dibutyltin dilaurate into the temperature-resistant polyurethane-based rubber crude rubber obtained in the second step, stirring at the stirring speed of 100 revolutions per minute for 10min, and then heating at the heating temperature of 60 ℃ for 10min to obtain the temperature-resistant polyurethane-based rubber.
The ozone aging test is carried out by adopting a tensile ratio of 20 percent and the volume fraction of the ozone concentration of (50 +/-5) × 10-8Observing the time of crack occurrence, namely observing once every minute after 2 hours to see whether the crack occurs or not; the hot air accelerated aging was conducted by testing the change in tensile strength after 168 hours of aging.
Comparative example 1
Firstly, adding 20g of toluene diisocyanate into 100g of polyurethane rubber AU2200, and stirring at the stirring speed of 100 revolutions per minute for 20min to obtain raw polyurethane-based rubber;
and secondly, adding 0.15g of dibutyltin dilaurate into the crude polyurethane-based rubber obtained in the first step, stirring at the stirring speed of 100 revolutions per minute for 10 minutes, and then heating at the heating temperature of 60 ℃ for 10 minutes to obtain the polyurethane-based rubber.
Comparative example 2
A preparation method of temperature-resistant polyurethane-based rubber comprises the following steps:
firstly, mixing 25g of fumed silica which is not treated by supercritical carbon dioxide with 100g of polyurethane rubber AU2200, and stirring at the stirring speed of 200 revolutions per minute for 20min to obtain a mixture;
and secondly, adding 20g of toluene diisocyanate into the mixture obtained in the first step, and stirring at the stirring speed of 100 revolutions per minute for 20 minutes to obtain the polyurethane-based raw rubber.
And thirdly, adding 0.15g of dibutyltin dilaurate into the temperature-resistant polyurethane-based rubber crude rubber obtained in the second step, stirring at the stirring speed of 100 revolutions per minute for 10min, and then heating at the heating temperature of 60 ℃ for 10min to obtain the polyurethane-based rubber.
The test result shows that: the test was carried out on the products obtained in comparative example 1 and comparative example 2 and the products obtained in example 1 and example 2.
The product obtained in the comparative example 1 has the Shore hardness of 40, the tensile strength of 35MPa, the maximum use temperature of 73 ℃, the ozone aging resistance of 150 minutes and the hot air aging resistance of 33 MPa;
the hardness of the product obtained in the comparative example 2 is 42, the tensile strength is 28MPa, the maximum use temperature is 68 ℃, the ozone aging resistance is 127 minutes, and the hot air aging resistance is 28 MPa;
the Shore hardness of the product obtained in the embodiment 1 is improved by 45 percent, the tensile strength is improved by 130 percent when the tensile strength is 80.5MPa, the ozone aging resistance is improved by 56 percent when the time is 234 minutes, and the maximum use temperature is 149 ℃;
the shore hardness of the product obtained in example 2 is increased by 143% when the shore hardness is 97%, the tensile strength is increased by 290% when the tensile strength is 136MPa, the ozone aging resistance is increased by 108% when the tensile strength is 312 minutes, and the maximum use temperature is 153 ℃.
Claims (10)
1. A temperature-resistant polyurethane-based rubber is characterized in that: the raw materials of the temperature-resistant polyurethane-based rubber comprise a polyurethane rubber matrix, a vulcanizing agent, a filler and a catalyst; the mass of the filler is 25-45% of that of the polyurethane rubber matrix; the mass ratio of the vulcanizing agent to the polyurethane rubber matrix is 1: 5-7; the mass of the catalyst is 0.05-0.25% of that of the polyurethane rubber matrix;
the filler is fumed silica treated by supercritical carbon dioxide.
2. The temperature-resistant polyurethane-based rubber according to claim 1, wherein: the polyurethane rubber substrate is polyurethane rubber AU2200 or polyurethane rubber EU 2400.
3. The temperature-resistant polyurethane-based rubber according to claim 1, wherein: the vulcanizing agent is toluene diisocyanate.
4. The temperature-resistant polyurethane-based rubber according to claim 1, wherein: the catalyst is dibutyltin dilaurate.
5. The temperature-resistant polyurethane-based rubber according to claim 1, wherein: the method for treating the fumed silica by the supercritical carbon dioxide comprises the following steps: treating for 2-3 h at the temperature of 100-150 ℃ and under the pressure of 18-20 MPa.
6. A preparation method of temperature-resistant polyurethane-based rubber is characterized by comprising the following steps:
firstly, mixing a filler and a polyurethane rubber matrix, and stirring to obtain a mixture;
secondly, adding a vulcanizing agent into the mixture obtained in the first step, and stirring to obtain the heat-resistant polyurethane-based rubber crude rubber;
and thirdly, adding a catalyst into the temperature-resistant polyurethane-based rubber raw rubber obtained in the second step, stirring, and then heating at the temperature of 60-70 ℃ for 10-20min to obtain the temperature-resistant polyurethane-based rubber.
7. The method for preparing a temperature-resistant polyurethane-based rubber according to claim 6, wherein the method comprises the following steps: in the first step, the stirring speed is 200-300 r/min.
8. The method for preparing a temperature-resistant polyurethane-based rubber according to claim 6, wherein the method comprises the following steps: in the first step, the stirring time is 10-20 min.
9. The method for preparing a temperature-resistant polyurethane-based rubber according to claim 6, wherein the method comprises the following steps: in the second step, the stirring speed is 100-150 r/min, and the stirring time is 10-20 min.
10. The method for preparing a temperature-resistant polyurethane-based rubber according to claim 6, wherein the method comprises the following steps: in the third step, the stirring speed is 100-200 r/min, and the stirring time is 10-15 min.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2022111289A1 (en) * | 2020-11-30 | 2022-06-02 | 北京宇航系统工程研究所 | Ablation-resistant silicon-boron-nitrogen rubber and preparation method therefor |
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| WO2022111289A1 (en) * | 2020-11-30 | 2022-06-02 | 北京宇航系统工程研究所 | Ablation-resistant silicon-boron-nitrogen rubber and preparation method therefor |
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Application publication date: 20200814 |