CN117384449B - Hollow microsphere reinforced EPDM (ethylene-propylene-diene monomer) heat insulation material as well as preparation method and application thereof - Google Patents

Hollow microsphere reinforced EPDM (ethylene-propylene-diene monomer) heat insulation material as well as preparation method and application thereof Download PDF

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CN117384449B
CN117384449B CN202311214396.5A CN202311214396A CN117384449B CN 117384449 B CN117384449 B CN 117384449B CN 202311214396 A CN202311214396 A CN 202311214396A CN 117384449 B CN117384449 B CN 117384449B
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epdm
hollow microsphere
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CN117384449A (en
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郭梦飞
余凯旋
张攀
张建华
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Xian University of Technology
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
    • C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
    • C08L23/16—Elastomeric ethene-propene or ethene-propene-diene copolymers, e.g. EPR and EPDM rubbers
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B7/00—Mixing; Kneading
    • B29B7/002—Methods
    • B29B7/007—Methods for continuous mixing
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C35/00—Heating, cooling or curing, e.g. crosslinking or vulcanising; Apparatus therefor
    • B29C35/02—Heating or curing, e.g. crosslinking or vulcanizing during moulding, e.g. in a mould
    • 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
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/38—Boron-containing compounds
    • C08K2003/387—Borates
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00—Polymer mixtures characterised by other features
    • C08L2205/14—Polymer mixtures characterised by other features containing polymeric additives characterised by shape
    • C08L2205/16—Fibres; Fibrils

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Abstract

The invention relates to a hollow microsphere reinforced EPDM (ethylene-propylene-diene monomer) heat-insulating material, a preparation method and application thereof, wherein the hollow microsphere reinforced EPDM heat-insulating material is formed by mixing and extruding hollow microspheres and a basic EPDM heat-insulating material, and the hollow microspheres are 3M S32HS or 3M iM16K and can be applied to an engine combustion chamber. The hollow microsphere reinforced EPDM heat insulation material has the characteristics of low density and excellent ablation resistance.

Description

Hollow microsphere reinforced EPDM (ethylene-propylene-diene monomer) heat insulation material as well as preparation method and application thereof
Technical Field
The invention relates to the technical field of heat insulating materials, in particular to a hollow microsphere reinforced EPDM heat insulating material, a preparation method and application thereof.
Background
During the working process of the rocket engine, heat can be conducted to the engine shell from the engine combustion chamber, and the integrity of the shell structure can be jeopardized by the excessively high temperature, so that the normal working of the engine is affected. Accordingly, thermal insulation materials are required to thermally protect the engine housing within the engine combustion chamber, but the insulation materials are of the negative mass of the engine, and the smaller and better the mass occupied within the solid rocket engine combustion chamber, the lower density insulation materials are beneficial to reducing the negative mass of the engine.
In the prior art, the density of the heat insulating material can be reduced by various modes such as foaming technology, introduction of expandable microbeads and the like, and although the density of the heat insulating material can be reduced by both modes, the ablation resistance of the heat insulating material can be reduced at the same time of reducing the density of the heat insulating material.
Disclosure of Invention
Based on the above, it is necessary to provide a hollow microsphere reinforced EPDM thermal insulation material with low density and excellent ablative properties, and a preparation method and application thereof.
In a first aspect, the invention provides a hollow microsphere reinforced EPDM (ethylene-propylene-diene monomer) heat-insulating material, which is formed by mixing and extruding hollow microspheres and a basic EPDM heat-insulating material;
The hollow microsphere is 3M S32HS or 3M iM16K.
In one embodiment, the hollow microsphere reinforced EPDM insulation contains, in parts by weight:
In one embodiment, the hollow microsphere reinforced EPDM insulation contains, in parts by weight:
In one embodiment, the hollow microsphere reinforced EPDM insulation contains, in parts by weight:
In one embodiment, the hollow microsphere reinforced EPDM insulation contains, in parts by weight:
In one embodiment, the resin is a phenolic resin, the fibers are aramid fibers, and the processing aid is paraffin oil.
In one embodiment, the vulcanizing agent consists of 1.5 parts by weight sulfur and 4.5 parts by weight dicumyl peroxide.
In a second aspect, the present invention also provides a method for preparing a hollow bead reinforced EPDM insulation material, for preparing a hollow bead reinforced EPDM insulation material of the first aspect, comprising the steps of:
EPDM rubber is placed on two side rollers of the open type double-roller mixer, and the open type double-roller mixer is started;
sequentially adding raw material fibers, siO 2, resin, zinc borate, hollow microspheres, a processing aid, a vulcanizing agent and EPDM rubber between the two rollers for mixing, and repeatedly mixing until the EPDM rubber and the raw materials are uniformly mixed to obtain a mixed rubber;
and standing the rubber compound for 22-26 hours, then placing the rubber compound into a die, and vulcanizing the rubber compound by using a flat vulcanizing machine to obtain the hollow microsphere reinforced EPDM heat insulation material.
In one embodiment, the temperature of vulcanization is 150-170 ℃, the pressure is 10-14 MPa, and the time is 25-35 min.
In a third aspect, the present invention also provides the use of the hollow bead reinforced EPDM insulation of the first aspect described above or the hollow bead reinforced EPDM insulation of the second aspect described above in an engine combustion chamber.
The beneficial effects of the invention are as follows:
(1) The invention adds the high-strength hollow microsphere as a reinforcement into the basic EPDM heat insulation material, and the obtained hollow microsphere reinforced EPDM heat insulation material has the characteristics of low density and excellent ablation resistance.
(2) According to the invention, the EPDM rubber and other preparation raw materials of the hollow microsphere reinforced EPDM heat insulation material are mixed by using the double-side extrusion method of the EPDM rubber, so that the hollow microsphere is effectively prevented from being directly extruded in the processing process, the breakage rate of the hollow microsphere in the processing process is greatly reduced, and the weakening and even failure of a hollow microsphere reinforcing mechanism can be avoided.
Drawings
FIG. 1 is a schematic view of the microstructure of a hollow microsphere according to the present invention;
FIG. 2 is a schematic flow chart of a method for preparing the hollow microsphere reinforced EPDM insulating material according to the invention;
Fig. 3 is a schematic diagram of an extrusion mode in an embodiment of the present invention, fig. 3 (a) is a schematic diagram of a single-side extrusion mode, fig. 3 (b) is a schematic diagram of a double-side extrusion mode, fig. 3 (c) is a schematic diagram of a partial enlargement of a single-side extrusion mode, and fig. 3 (d) is a schematic diagram of a partial enlargement of a double-side extrusion mode;
FIG. 4 is a bar graph of carbonization rate and density for thermal insulation materials of different formulations in test examples of the present invention.
Detailed Description
In order that the invention may be readily understood, a more complete description of the invention will be rendered by reference to the appended drawings. Preferred embodiments of the present invention are shown in the drawings. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used herein in the description of the invention is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. The term "and/or" as used herein includes any and all combinations of one or more of the associated listed items.
Insulation materials are often used in solid rocket engines that effectively reduce the problem of conduction from the combustion chamber in the engine to the engine casing, protecting the integrity of the engine casing. However, the insulation material is of a negative mass of the engine, and the smaller and better the mass occupied in the combustion chamber of the solid rocket engine, the lower the density of the insulation material is required to be as low as possible to reduce the mass of the insulation material. Methods of reducing the density of insulation materials by foaming techniques and the introduction of expandable microbeads have been attempted in the prior art, but these methods do not address the need for low density and excellent ablative properties well.
The invention provides a hollow microsphere reinforced EPDM (ethylene-propylene-diene monomer) heat-insulating material which can well meet the requirements of low density and excellent ablative performance, and is formed by mixing and extruding hollow microspheres and a basic EPDM heat-insulating material, wherein the types of the hollow microspheres are 3M S32HS or 3M iM16K.
As shown in fig. 1, fig. 1 is a schematic view of the microstructure of the hollow microsphere. The hollow microsphere has the appearance of white powder, the main components of the hollow microsphere are SiO 2 and Al 2O3, siO 2 and Al 2O3 are fired into a hollow sphere structure through a special process, and the hollow sphere structure has the intrinsic characteristics of thin wall hollow and small size, so that the hollow microsphere has the characteristics of light weight, high strength, sound insulation, heat insulation, good chemical stability, low cost and the like.
The hollow microsphere reinforced EPDM (ethylene propylene diene monomer) heat insulation material disclosed by the invention requires the hollow microsphere to have low density and certain compressive strength, so that the hollow microsphere is not broken or is broken as little as possible in the preparation process. According to the invention, hollow microspheres with the model number of 3M S32HS or 3M iM16K are selected as reinforcements to be added into the basic EPDM heat insulation material, so that the density of the heat insulation material is reduced.
In one embodiment, the cenosphere reinforced EPDM insulation contains, in parts by weight:
in this embodiment, the resin is phenolic resin, the fiber is aramid fiber, and the processing aid is paraffin oil. The EPDM heat insulation material reinforced by aramid fiber has good heat insulation and ablation resistance. The vulcanizing agent consists of 1.5 parts by weight of sulfur and 4.5 parts by weight of dicumyl peroxide.
Wherein the phenolic resin is JP763 purchased from Shanghai Jun-Pu chemical industry, the aramid fiber is also called Kevlar fiber, the length is 3mm, the phenolic resin is purchased from DuPont group, the processing aid is paraffin oil, and the vulcanizing agent consists of 1.5 parts by weight of sulfur and 4.5 parts by weight of dicumyl peroxide. EPDM was from 4045m of the triple well group, sio 2 was purchased from Cabot, EH5.
Specifically, the fiber is used for forming a framework of the carbonization layer, so that the mechanical property of the carbonization layer can be improved; the addition of micro-or nano-sized SiO 2 can increase the ablation resistance temperature, improve the carbon structure and reduce the oxidization rate of the charring layer. The zinc borate has the functions of flame retardance, smoke suppression, char formation, flame suppression, molten drop prevention and the like, and has the other characteristics of good retention effect on the strength and the elongation of a plurality of polymers, and no reduction of the aging strength of the polymers. Raw rubber, while also having some useful application characteristics, is low in strength, low in elasticity, stiff in cold, sticky in hot and prone to aging. Under certain conditions, the vulcanizing agent can vulcanize (crosslink) the rubber, and the vulcanization can improve the comprehensive properties of the EPDM heat insulation material, such as ozone resistance, heat resistance, light resistance, weather resistance, chemical resistance and the like. In this procedure, the rubber undergoes a series of complex chemical changes from a plastic compound to a highly elastic or hard crosslinked rubber, thereby obtaining more perfect physical and mechanical properties and chemical properties, and improving and widening the application value and application range of the rubber material.
The 3M iM16K hollow microsphere has the compressive strength of 18000/124.1PSI/MPa and the density of 0.46g/cm 3, and can play a role in reinforcing mechanism and reduce the density of the hollow microsphere reinforced EPDM heat insulation material.
Preferably, the hollow microsphere reinforced EPDM insulation material contains, in parts by weight:
In one embodiment, the cenosphere reinforced EPDM insulation contains, in parts by weight:
In the embodiment, the compression strength of the 3M S32HS hollow microsphere is 6000/41.37PSI/MPa, and the density is 0.32g/cm 3, so that a reinforcing mechanism can be realized, and the density of the hollow microsphere reinforced EPDM heat insulation material is reduced.
Preferably, the hollow microsphere reinforced EPDM insulation material contains, in parts by weight:
preferably, the hollow microsphere reinforced EPDM insulating material comprises the following components in parts by weight:
In a preferred embodiment, the cenosphere reinforced EPDM insulation contains, in parts by weight:
In a specific embodiment, the 3m s32hs cenospheres and the 3m im16k cenospheres may be mixed as a reinforcement of the cenosphere-reinforced EPDM insulation material on the basis of the above embodiment.
Based on the same invention, the invention also provides a preparation method of the hollow microsphere reinforced EPDM heat insulation material, which is used for preparing the hollow microsphere reinforced EPDM heat insulation material, as shown in figure 2, and figure 2 is a flow diagram of the preparation method of the hollow microsphere reinforced EPDM heat insulation material, and the method comprises the following steps:
s101, placing EPDM rubber on two side rollers of the open type double-roller mixer, and starting the open type double-roller mixer.
The key point of preparing the hollow microsphere reinforced EPDM heat insulation material is to press the hollow microsphere into the EPDM under the premise of ensuring that the hollow microsphere is not destroyed as much as possible. In the unilateral extrusion preparation process in the prior art, the hollow microsphere can be directly extruded by the roller, so that the hollow microsphere is extremely easy to damage, and the reinforcing effect is greatly reduced.
FIG. 3 is a schematic illustration of the double-sided extrusion method of the present invention, as shown in FIG. 3. According to the invention, the hollow micro-beads are pressed into the EPDM by adopting a bilateral extrusion method, so that the hollow micro-beads can be prevented from being in direct contact with the rollers, and the hollow micro-beads are effectively protected from being crushed.
Preferably, increasing the distance of the rollers and raising the temperature of the rollers further avoids the hollow microspheres from crushing.
S102, sequentially adding raw material fibers, siO 2, resin, hollow microspheres, a processing aid, a vulcanizing agent and EPDM rubber between the two rollers for mixing, and repeatedly mixing until the EPDM rubber and the raw materials are uniformly mixed to obtain a rubber compound.
S103, standing the rubber compound for 22-26 hours, then placing the rubber compound into a die, and vulcanizing the rubber compound by using a flat vulcanizing machine to obtain the hollow microsphere reinforced EPDM heat insulation material.
In one embodiment, the temperature of vulcanization is 150 ℃ to 170 ℃, the pressure is 10MPa to 14MPa, and the time is 25min to 35min.
The hollow bead reinforced EPDM heat insulation material or the hollow bead reinforced EPDM heat insulation material prepared by the preparation method can be applied to the combustion chamber of the engine, is beneficial to reducing the negative quality of the engine, and has better ablation resistance.
In order to further illustrate the present invention, the hollow microsphere reinforced EPDM thermal insulation material and the method of preparing the same provided by the present invention are described in detail below with reference to specific examples.
Example 1
The hollow microsphere reinforced EPDM heat insulating material comprises the following components in parts by weight:
The preparation method comprises the following steps:
100 parts of EPDM rubber is placed on two side rollers of an open type double-roller mixer, and the open type double-roller mixer is started; sequentially adding 6 parts of aramid fiber, 11 parts of SiO 2, 2 parts of 3M iM16K hollow microspheres, 11 parts of phenolic resin, 6 parts of zinc borate, 6 parts of paraffin oil, 6 parts of vulcanizing agent and 100 parts of EPDM rubber between two rollers, and mixing for multiple times until the EPDM rubber and the raw materials are uniformly mixed to obtain a mixed rubber; and standing the rubber compound for 22 hours, then placing the rubber compound into a mould, and vulcanizing the rubber compound by using a flat vulcanizing machine to obtain the hollow microsphere reinforced EPDM heat insulation material. Wherein the temperature of vulcanization is 151 ℃, the pressure is 11MPa, and the time is 26min.
The hollow microsphere reinforced EPDM heat insulation material in the embodiment has the characteristics of low density and excellent ablation resistance, and the preparation method can greatly reduce the breakage rate of the hollow microsphere in the processing process.
Example 2
The hollow microsphere reinforced EPDM heat insulating material comprises the following components in parts by weight:
The preparation method comprises the following steps:
100 parts of EPDM rubber is placed on two side rollers of an open type double-roller mixer, and the open type double-roller mixer is started; sequentially adding 9 parts of aramid fiber, 19 parts of SiO 2, 48 parts of 3M iM16K hollow microspheres, 19 parts of phenolic resin, 9 parts of zinc borate, 19 parts of paraffin oil, 6 parts of vulcanizing agent and 100 parts of EPDM rubber between two rollers, and mixing for multiple times until the EPDM rubber and the raw materials are uniformly mixed to obtain a mixed rubber; and standing the rubber compound for 25 hours, then placing the rubber compound into a mould, and vulcanizing the rubber compound by using a flat vulcanizing machine to obtain the hollow microsphere reinforced EPDM heat insulation material. Wherein the temperature of vulcanization is 169 ℃, the pressure is 13MPa, and the time is 34min.
The hollow microsphere reinforced EPDM heat insulation material in the embodiment has the characteristics of low density and excellent ablation resistance, and the preparation method can greatly reduce the breakage rate of the hollow microsphere in the processing process.
Example 3
The hollow microsphere reinforced EPDM heat insulating material comprises the following components in parts by weight:
The preparation method comprises the following steps:
100 parts of EPDM rubber is placed on two side rollers of an open type double-roller mixer, and the open type double-roller mixer is started; 8 parts of aramid fiber, 15 parts of SiO 2, 25 parts of 3M iM16K hollow microspheres, 15 parts of phenolic resin, 8 parts of zinc borate, 13 parts of paraffin oil, 6 parts of vulcanizing agent and 100 parts of EPDM rubber are sequentially added between the two rollers for mixing, and the mixture is mixed for multiple times until the EPDM rubber is uniformly mixed with each raw material to obtain a mixed rubber; and standing the rubber compound for 24 hours, then placing the rubber compound into a mould, and vulcanizing the rubber compound by using a flat vulcanizing machine to obtain the hollow microsphere reinforced EPDM heat insulation material. Wherein the temperature of vulcanization is 160 ℃, the pressure is 13MPa, and the time is 30min.
The hollow microsphere reinforced EPDM heat insulation material in the embodiment has the characteristics of low density and excellent ablation resistance, and the preparation method can greatly reduce the breakage rate of the hollow microsphere in the processing process.
Example 4
The hollow microsphere reinforced EPDM heat insulating material comprises the following components in parts by weight:
The preparation method comprises the following steps:
100 parts of EPDM rubber is placed on two side rollers of an open type double-roller mixer, and the open type double-roller mixer is started; sequentially adding 6 parts of aramid fiber, 11 parts of SiO 2, 2 parts of 3M S32HS hollow microspheres, 11 parts of phenolic resin, 6 parts of zinc borate, 6 parts of paraffin oil, 6 parts of vulcanizing agent and 100 parts of EPDM rubber between two rollers, and mixing for multiple times until the EPDM rubber and the raw materials are uniformly mixed to obtain a mixed rubber; and standing the rubber compound for 22 hours, then placing the rubber compound into a mould, and vulcanizing the rubber compound by using a flat vulcanizing machine to obtain the hollow microsphere reinforced EPDM heat insulation material. Wherein the temperature of vulcanization is 151 ℃, the pressure is 11MPa, and the time is 26min.
The hollow microsphere reinforced EPDM heat insulation material in the embodiment has the characteristics of low density and excellent ablation resistance, and the preparation method can greatly reduce the breakage rate of the hollow microsphere in the processing process.
Example 5
The hollow microsphere reinforced EPDM heat insulating material comprises the following components in parts by weight:
The preparation method comprises the following steps:
100 parts of EPDM rubber is placed on two side rollers of an open type double-roller mixer, and the open type double-roller mixer is started; sequentially adding 9 parts of aramid fiber, 19 parts of SiO 2, 29 parts of 3M S32HS hollow microspheres, 19 parts of phenolic resin, 9 parts of zinc borate, 19 parts of paraffin oil, 6 parts of vulcanizing agent and 100 parts of EPDM rubber between two rollers, and mixing for multiple times until the EPDM rubber and the raw materials are uniformly mixed to obtain a mixed rubber; and standing the rubber compound for 25 hours, then placing the rubber compound into a mould, and vulcanizing the rubber compound by using a flat vulcanizing machine to obtain the hollow microsphere reinforced EPDM heat insulation material. Wherein the temperature of vulcanization is 169 ℃, the pressure is 13MPa, and the time is 34min.
The hollow microsphere reinforced EPDM heat insulation material in the embodiment has the characteristics of low density and excellent ablation resistance, and the preparation method can greatly reduce the breakage rate of the hollow microsphere in the processing process.
Example 6
The hollow microsphere reinforced EPDM heat insulating material comprises the following components in parts by weight:
The preparation method comprises the following steps:
100 parts of EPDM rubber is placed on two side rollers of an open type double-roller mixer, and the open type double-roller mixer is started; 8 parts of aramid fiber, 15 parts of SiO 2, 15 parts of 3M S32HS hollow microspheres, 15 parts of phenolic resin, 8 parts of zinc borate, 13 parts of paraffin oil, 6 parts of vulcanizing agent and 100 parts of EPDM rubber are sequentially added between the two rollers to be mixed, and the mixture is mixed for multiple times until the EPDM rubber is uniformly mixed with each raw material to obtain mixed rubber; and standing the rubber compound for 24 hours, then placing the rubber compound into a mould, and vulcanizing the rubber compound by using a flat vulcanizing machine to obtain the hollow microsphere reinforced EPDM heat insulation material. Wherein the temperature of vulcanization is 160 ℃, the pressure is 13MPa, and the time is 30min.
The hollow microsphere reinforced EPDM heat insulation material in the embodiment has the characteristics of low density and excellent ablation resistance, and the preparation method can greatly reduce the breakage rate of the hollow microsphere in the processing process.
Experimental example 1
This test example was used to verify the low density of the inventive cenosphere reinforced EPDM insulation. The density test calculation is specifically carried out on the hollow bead reinforced EPDM heat insulation material prepared by adding 20 parts of 3M iM16K hollow beads, 43 parts of 3M iM16K hollow beads, 20 parts of 3M S32HS hollow beads or 30 parts of 3M S32HS hollow beads into the basic formula 1, and the specific results are shown in table 1.
Wherein, the basic formula 1 comprises 100 parts of EPDM,10 parts of aramid fiber, 20 parts of SiO 2, 20 parts of phenolic resin, 10 parts of zinc borate, 20 parts of paraffin oil and 6 parts of vulcanizing agent by weight. The hollow microsphere reinforced EPDM heat insulation material is prepared for 24 hours, the vulcanizing temperature is 160 ℃, the pressure is 12MPa, and the time is 30 minutes.
TABLE 1 Density Change after addition of cenospheres to basic formulation 1
As can be seen from the table, the iM16K hollow microspheres are not broken; when the added parts are low, the S32HS hollow beads cannot be broken, and when the added parts are increased, the S32HS hollow beads can be partially broken, but still have the function of reducing the density. Wherein, when 20 parts of 3M I16K hollow beads are added, the density of the heat insulation material is reduced by 7.29%, when 43 parts of 3M I16K hollow beads are added, the density of the heat insulation material is reduced by 13.7%, when 20 parts of 3M S32HS hollow beads are added, the density of the heat insulation material is reduced by 6.75%, and when 30 parts of 3M S32HS hollow beads are added, although part of the heat insulation material is broken, the density of the heat insulation material is still reduced by 8.40%.
From the above analysis, the hollow microsphere reinforced EPDM insulation of the present invention has a low density, which is beneficial for reducing the negative mass of the engine.
Experimental example 2
This test example was used to verify the low density of the inventive cenosphere reinforced EPDM insulation. The density test calculation is specifically carried out on the hollow bead reinforced EPDM heat insulation material prepared by adding 50 parts of 3M iM16K hollow beads, 20 parts of 3M S32HS hollow beads or 30 parts of 3M S32HS hollow beads into the basic formula 2, and the specific results are shown in Table 2.
Wherein, based on weight parts, the basic formula 2 comprises 100 parts of EPDM,5 parts of aramid fiber, 10 parts of SiO 2, 10 parts of phenolic resin, 5 parts of zinc borate, 5 parts of paraffin oil and 6 parts of vulcanizing agent. The hollow microsphere reinforced EPDM heat insulation material is prepared for 24 hours, the vulcanizing temperature is 160 ℃, the pressure is 12MPa, and the time is 30 minutes.
TABLE 2 Density Change after hollow microbeads were added to basic formulation 2
As can be seen from the table, the iM16K hollow microspheres are not broken; when the added parts are low, the S32HS hollow beads cannot be broken, and when the added parts are increased, the S32HS hollow beads can be partially broken, but still have the function of reducing the density. Wherein, when 50 parts of 3M iM16K hollow microspheres are added, the density of the heat insulation material is reduced by 16.2%, and when 20 parts of 3M S32HS hollow microspheres are added, the density of the heat insulation material is reduced by 10.8%.
From the above analysis, the hollow microsphere reinforced EPDM insulation of the present invention has a low density, which is beneficial for reducing the negative mass of the engine.
Experimental example 3
This test example was used to verify the ablative properties of the inventive hollow microsphere reinforced EPDM insulation. The ablation performance test is carried out on the EPDM heat insulation material reinforced by the hollow bead, which is prepared by adding 43 parts of iM16K hollow bead or 20 parts of 3M S32HS hollow bead into the basic formula 1.
The experimental example adopts oxygen-acetylene ablation to verify the ablation performance of the hollow microsphere reinforced EPDM heat insulation material. The oxy-acetylene ablation test is the most widely used method for testing the ablation performance at present. The oxyacetylene ablation experiment temperature is high, the cost is low, and the method is safe and reliable, and is a thermal insulation material ablation performance test method specified by the national standard GJB 323A-1996. The oxyacetylene combustion products were calculated thermally from the flow ratios of oxygen to acetylene set by GJB323A-1996, as shown in Table 3. The oxyacetylene combustion product contains oxidizing components including 6.54% H2O, 3.47% O, and 0.86% O2. The presence of the oxidizing component indicates that the oxyacetylene ablation environment is an oxygen-rich environment.
TABLE 3 calculated values for oxygen and acetylene equilibrium combustion products under ablation conditions
The thermal insulation material needs to have excellent ablation resistance, i.e., a low ablation rate. The carbonization rate is used for representing the anti-ablation performance of the heat insulating material, and the lower the carbonization rate is, the stronger the anti-ablation performance of the heat insulating material is. The carbonization rates of the basic formulation and the hollow microsphere formulation are shown, and in order to more clearly compare the influence of the hollow microsphere on the ablation rate of the heat insulation material, the ablation rate of the hollow microsphere is normalized relative to the basic formulation 1 to obtain fig. 4, and fig. 4 is a bar graph of the carbonization rate and the density of the heat insulation material of different formulations in the test example of the invention. As can be seen from fig. 4, the hollow microsphere can reduce the carbonization rate of the heat insulating material, compared with the EPDM heat insulating material of the basic formulation 1, the ablation rate of 20 parts of S32HS is reduced by 11.3%, the ablation rate of 43 parts of iM16K formulation is reduced by 18.6%, and the carbonization rate of 43 parts of the hollow microsphere formulation is lower than that of 20 parts of the hollow microsphere formulation.
It is known from test examples 1 to 3 in combination with the present invention that the hollow microsphere reinforced EPDM insulating material of the present invention can have both low density and excellent ablative properties.
The above examples illustrate only a few embodiments of the invention, which are described in detail and are not to be construed as limiting the scope of the invention. It should be noted that it will be apparent to those skilled in the art that several variations and modifications can be made without departing from the spirit of the invention, which are all within the scope of the invention. Accordingly, the scope of protection of the present invention is to be determined by the appended claims.

Claims (7)

1. The hollow microsphere reinforced EPDM heat insulating material is characterized by being formed by mixing and extruding hollow microspheres and a basic EPDM heat insulating material;
the hollow microsphere is 3M S32HS or 3M iM16K;
the hollow microsphere reinforced EPDM insulation contains:
1-50 parts of 3M iM16K hollow microspheres;
100 parts of EPDM;
5-10 parts of fiber;
10-20 parts of SiO 2;
10-20 parts of resin;
5-10 parts of zinc borate;
5-20 parts of a processing aid;
6 parts of vulcanizing agent;
or hollow microsphere reinforced EPDM insulation comprising:
1-20 parts of 3M S32HS hollow microspheres;
100 parts of EPDM;
5-10 parts of fiber;
10-20 parts of SiO 2;
10-20 parts of resin;
5-10 parts of zinc borate;
5-20 parts of a processing aid;
6 parts of vulcanizing agent;
the resin is phenolic resin, and the fiber is aramid fiber;
the preparation of the hollow microsphere reinforced EPDM heat insulation material comprises the following steps:
EPDM rubber is placed on two side rollers of the open type double-roller mixer, and the open type double-roller mixer is started;
sequentially adding raw material fibers, siO 2, resin, zinc borate, hollow microspheres, a processing aid, a vulcanizing agent and EPDM rubber between the two rollers for mixing, and repeatedly mixing until the EPDM rubber and the raw materials are uniformly mixed to obtain a mixed rubber;
and standing the rubber compound for 22-26 hours, then placing the rubber compound into a die, and vulcanizing the rubber compound by using a flat vulcanizing machine to obtain the hollow microsphere reinforced EPDM heat insulation material.
2. The hollow microsphere reinforced EPDM insulation of claim 1, wherein the hollow microsphere reinforced EPDM insulation contains, in parts by weight:
43 parts of 3M iM16K hollow microsphere;
100 parts of EPDM;
10 parts of fiber;
20 parts of SiO 2;
20 parts of resin;
10 parts of zinc borate;
20 parts of a processing aid;
6 parts of vulcanizing agent.
3. The hollow microsphere reinforced EPDM insulation of claim 1, wherein the hollow microsphere reinforced EPDM insulation contains, in parts by weight:
20 parts of 3M S32HS hollow microsphere;
100 parts of EPDM;
10 parts of fiber;
20 parts of SiO 2;
20 parts of resin;
10 parts of zinc borate;
20 parts of a processing aid;
6 parts of vulcanizing agent.
4. A hollow microsphere reinforced EPDM insulation as claimed in either one of claims 2 or 3, characterized in that the processing aid is paraffin oil.
5. The hollow bead reinforced EPDM insulation of claim 4, wherein the vulcanizing agent is comprised of 1.5 parts by weight sulfur and 4.5 parts by weight dicumyl peroxide.
6. The hollow bead reinforced EPDM insulation material of claim 1, wherein the vulcanizing temperature is 150 ℃ to 170 ℃, the pressure is 10mpa to 14mpa, and the time is 25min to 35 min.
7. Use of the cenosphere-reinforced EPDM insulation of any one of claims 1 to 6 in an engine combustion chamber.
CN202311214396.5A 2023-09-20 2023-09-20 Hollow microsphere reinforced EPDM (ethylene-propylene-diene monomer) heat insulation material as well as preparation method and application thereof Active CN117384449B (en)

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