CN111410843B - Preparation method of silicone rubber composite material with vibration fireproof performance - Google Patents
Preparation method of silicone rubber composite material with vibration fireproof performance Download PDFInfo
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- CN111410843B CN111410843B CN202010296600.2A CN202010296600A CN111410843B CN 111410843 B CN111410843 B CN 111410843B CN 202010296600 A CN202010296600 A CN 202010296600A CN 111410843 B CN111410843 B CN 111410843B
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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
- C08K13/04—Ingredients characterised by their shape and organic or inorganic ingredients
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- 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
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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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
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- C—CHEMISTRY; METALLURGY
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
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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
- C08K7/02—Fibres or whiskers
- C08K7/04—Fibres or whiskers inorganic
- C08K7/08—Oxygen-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
- C08K7/00—Use of ingredients characterised by shape
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- C08K7/20—Glass
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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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2265—Oxides; Hydroxides of metals of iron
- C08K2003/2272—Ferric oxide (Fe2O3)
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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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
- C08K2003/265—Calcium, strontium or barium carbonate
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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
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
Abstract
The invention discloses a preparation method of a silicone rubber composite material with vibration fireproof performance, which comprises the following steps: (1) banburying calcium carbonate, glass beads, silicon rubber and mullite fiber in an internal mixer, and taking out to obtain a product A; (2) milling the product A in a double-roller mill, and adding the product B into the mill during milling; (3) standing the product B, and eliminating internal stress to obtain a product C; (4) and vulcanizing the product C in a two-stage vulcanization mode to obtain the vulcanized silicone rubber composite material. The invention has the characteristics of fire prevention and vibration prevention.
Description
Technical Field
The invention relates to a preparation method of a silicone rubber composite material, in particular to a preparation method of a silicone rubber composite material with vibration fireproof performance.
Background
The organic silicon rubber is widely used as a sealing material in the aerospace field, and the silicone rubber sealing element of the large airplane nacelle is a high-added-value and high-tech product developed by enterprises, the fireproof and flame-retardant performance cannot meet the requirement, the production and processing are difficult, and the high product cost is a main bottleneck restricting the product development at present.
The sintered layer formed by the fiber filler at high temperature of thousands of degrees blocks flame, but is easy to collapse under vibration, and needs larger addition amount, and the processing property is deteriorated due to poor bonding, uneven dispersion, entanglement and the like. During flying, the aircraft mainly bears the aerodynamic load and plays a role in rectification. The nacelle serves as a structure for wrapping the fan fire area and the core fire area, bears the function of a firewall and meets the fireproof requirement. If the flame escapes from the engine nacelle, the flame may spread to a wing oil tank, causing a serious accident of machine damage and death.
Disclosure of Invention
The invention aims to provide a preparation method of a silicone rubber composite material with vibration fireproof performance. The invention has the characteristics of fire prevention and vibration prevention.
The technical scheme of the invention is as follows: a preparation method of a silicone rubber composite material with vibration fireproof performance comprises the following steps:
(1) banburying calcium carbonate, glass beads, silicon rubber and mullite fiber in an internal mixer, and taking out to obtain a product A;
(2) milling the product A in a double-roller mill, and adding the product B into the mill during milling;
(3) standing the product B, and eliminating internal stress to obtain a product C;
(4) and vulcanizing the product C in a two-stage vulcanization mode to obtain the vulcanized silicone rubber composite material.
In the step 1), the silicon rubber composite material comprises 1150 parts by weight of calcium carbonate 1100-.
In the step 1), the silicon rubber composite material comprises 1125 parts by weight of calcium carbonate, 750 parts by weight of glass beads and 15000 parts by weight of silicon rubber, wherein the mullite fiber accounts for 40% of the silicon rubber.
In the preparation method of the silicone rubber composite material with vibration fireproof performance, in the step 1), the banburying temperature is 95-105 ℃, the rotating speed is 75-85r/min, and the time is 10-20 min.
In the step 2), the adding amount of the twenty-five compound is 0.6-0.7% of the mass of the silicone rubber, and the adding amount of the iron oxide red is 1.5-2.5% of the mass of the silicone rubber.
In the step 2), the adding amount of the twenty-five compound is 0.67% of the mass of the silicone rubber, and the adding amount of the iron oxide red is 2% of the mass of the silicone rubber.
In the preparation method of the silicone rubber composite material with the vibration fireproof performance, in the step 3), the standing time is 20-30 hours.
In the preparation method of the silicone rubber composite material with vibration fireproof performance, in the step 4), the two-stage vulcanization is performed by first vulcanizing at 150 ℃ for 1-3 hours in an oven at 110-.
The invention has the advantages of
Compared with the prior art, the invention has obvious effect. According to the scheme, the mullite fiber, the calcium carbonate and the glass bead filling materials are added into the silicon rubber composite material, so that the tensile strength of the silicon rubber can be enhanced by the filling materials, and the fireproof performance of the silicon rubber composite material is greatly improved. In the vibration combustion process of the silicon rubber composite material, a compact ceramic structure with certain strength is generated on the surface of the silicon rubber composite material, so that the silicon rubber composite material is prevented from collapsing and burning inside a vibration framework. In a vibration combustion experiment, the glass beads are melted into a molten state at 1150 ℃, and an amorphous silica layer generated by combustion, unburned mullite fiber and calcium oxide generated by oxidation are bonded, so that the loose amorphous silica layer becomes compact and has certain strength; the unburned mullite fibers play a skeleton role in the mullite fiber, and the collapse of the ceramic layer is prevented; the calcium carbonate is oxidized and decomposed into calcium oxide at the temperature of 600-800 ℃, the process absorbs heat, and the calcium oxide is filled in gaps of the amorphous silicon dioxide layer, so that the ceramic layer is more compact. At 1150 ℃ flame burning, vibration at a frequency of 50Hz and an acceleration of 8g, the sample did not burn through for fifteen minutes and the ceramic layer was still present. The addition of the filler is proved to greatly improve the fireproof and anti-vibration performance of the silicon rubber, and the flame is prevented from jumping out of the engine nacelle at the position of the engine nacelle of the airplane.
Drawings
FIG. 1 is a digital graph of the front of a composite material obtained in examples 1 to 5 of the present invention;
FIG. 2 is a digital graph of the back of the vibration combustion of the composite materials prepared in examples 1-5 of the present invention.
Detailed Description
The present invention is further illustrated by the following examples, which are not to be construed as limiting the invention.
Examples of the invention
Example 1: a preparation method of a silicone rubber composite material with vibration fireproof performance comprises the following steps:
(1) banburying 11.25g of calcium carbonate, 7.5g of glass beads, 150g of silicone rubber and 37.5g of mullite fiber in an internal mixer at 100 ℃ for 15min at a speed of 80r/min, and taking out to obtain a product A;
(2) milling the product A in a double-roller mill, and adding 1g of Shuangerwu and 3g of iron oxide red during milling to obtain a product B;
(3) standing the product B for 24h, and eliminating internal stress to obtain a product C;
(4) and vulcanizing the product C in a two-stage vulcanization mode, namely vulcanizing the product C in an oven at the temperature of 110-150 ℃ for 1-3 hours, and then heating to the temperature of 170-220 ℃ for vulcanizing for 30min to obtain the vulcanized silicone rubber composite material.
Example 2: a preparation method of a silicone rubber composite material with vibration fireproof performance comprises the following steps:
(1) banburying 11.25g of calcium carbonate, 7.5g of glass beads, 150g of silicone rubber and 45g of mullite fiber in a banbury mixer at 100 ℃ for 15min at a speed of 80r/min, and taking out to obtain a product A;
(2) milling the product A in a double-roller mill, and adding 1g of Shuangerwu and 3g of iron oxide red during milling to obtain a product B;
(3) standing the product B for 24h, and eliminating internal stress to obtain a product C;
(4) and vulcanizing the product C in a two-stage vulcanization mode, namely vulcanizing the product C in an oven at the temperature of 110-150 ℃ for 1-3 hours, and then heating to the temperature of 170-220 ℃ for vulcanizing for 30min to obtain the vulcanized silicone rubber composite material.
Example 3: a preparation method of a silicone rubber composite material with vibration fireproof performance comprises the following steps:
(1) banburying 11.25g of calcium carbonate, 7.5g of glass beads, 150g of silicone rubber and 52.5g of mullite fiber in an internal mixer at 100 ℃ for 15min at a speed of 80r/min, and taking out to obtain a product A;
(2) milling the product A in a double-roller mill, and adding 1g of Shuangerwu and 3g of iron oxide red during milling to obtain a product B;
(3) standing the product B for 24h, and eliminating internal stress to obtain a product C;
(4) and vulcanizing the product C in a two-stage vulcanization mode, namely vulcanizing the product C in an oven at the temperature of 110-150 ℃ for 1-3 hours, and then heating to the temperature of 170-220 ℃ for vulcanizing for 30min to obtain the vulcanized silicone rubber composite material.
Example 4: a preparation method of a silicone rubber composite material with vibration fireproof performance comprises the following steps:
(1) banburying 11.25g of calcium carbonate, 7.5g of glass beads, 150g of silicone rubber and 60g of mullite fiber in a banbury mixer at 100 ℃ for 15min at a speed of 80r/min, and taking out to obtain a product A;
(2) milling the product A in a double-roller mill, and adding 1g of Shuangerwu and 3g of iron oxide red during milling to obtain a product B;
(3) standing the product B for 24h, and eliminating internal stress to obtain a product C;
(4) and vulcanizing the product C in a two-stage vulcanization mode, namely vulcanizing the product C in an oven at the temperature of 110-150 ℃ for 1-3 hours, and then heating to the temperature of 170-220 ℃ for vulcanizing for 30min to obtain the vulcanized silicone rubber composite material.
Example 5: a preparation method of a silicone rubber composite material with vibration fireproof performance comprises the following steps:
(1) banburying 11.25g of calcium carbonate, 7.5g of glass beads, 150g of silicone rubber and 67.5g of mullite fiber in an internal mixer at 100 ℃ for 15min at a speed of 80r/min, and taking out to obtain a product A;
(2) milling the product A in a double-roller mill, and adding 1g of Shuangerwu and 3g of iron oxide red during milling to obtain a product B;
(3) standing the product B for 24h, and eliminating internal stress to obtain a product C;
(4) and vulcanizing the product C in a two-stage vulcanization mode, namely vulcanizing the product C in an oven at the temperature of 110-150 ℃ for 1-3 hours, and then heating to the temperature of 170-220 ℃ for vulcanizing for 30min to obtain the vulcanized silicone rubber composite material.
The composite materials prepared in examples 1-5 were fired at a frequency of 50HZ, an acceleration of 4-8g, and a temperature of 1150 ℃ for 15min, and the final front and back views correspond to (1) - (5) in fig. 1-2, in sequence, and it can be seen that the performance of fig. 1(4) and fig. 2(4) is the best, and the samples do not burn through.
Example 6: a preparation method of a silicone rubber composite material with vibration fireproof performance comprises the following steps:
(1) 1100 parts of calcium carbonate, 700 parts of glass beads, 14000 parts of silicon rubber and 35 percent of mullite fiber of the silicon rubber are banburying in a 95 ℃ internal mixer at 75r/min for 10min and then taken out to obtain a product A;
(2) milling the product A in a double-roller mill, and adding 0.6 percent of bis-di-penta and 1.5 percent of iron oxide red in mass of the silicon rubber during milling to obtain a product B;
(3) standing the product B for 20h, and eliminating internal stress to obtain a product C;
(4) and vulcanizing the product C in a two-stage vulcanization mode, vulcanizing the product C in an oven at 110 ℃ for 1 hour, and then heating to 170 ℃ for vulcanizing for 30min to obtain the vulcanized silicone rubber composite material.
Example 7: a preparation method of a silicone rubber composite material with vibration fireproof performance comprises the following steps:
(1) according to the parts by weight, 1150 parts of calcium carbonate, 800 parts of glass beads, 16000 parts of silicon rubber and 42 percent of mullite fiber of the silicon rubber are banburied for 20min at 85r/min in a 105 ℃ internal mixer and then taken out to obtain a product A;
(2) milling the product A in a double-roller mill, and adding 0.7 percent of bis-di-penta and 2.5 percent of iron oxide red in terms of mass of the silicon rubber during milling to obtain a product B;
(3) standing the product B for 30h, and eliminating internal stress to obtain a product C;
(4) and vulcanizing the product C in a two-stage vulcanization mode, vulcanizing the product C in an oven at 150 ℃ for 3 hours, and then heating to 220 ℃ for vulcanizing the product C for 30min to obtain the vulcanized silicone rubber composite material.
The above description is only for the purpose of illustrating the present invention and the appended claims, and the scope of the present invention is not limited thereto, and any person skilled in the art can substitute or change the technical solution and the inventive concept of the present invention within the technical scope of the present invention.
Claims (3)
1. The preparation method of the silicone rubber composite material with the vibration fireproof performance is characterized by comprising the following steps:
(1) banburying calcium carbonate, glass beads, silicon rubber and mullite fiber in an internal mixer, and taking out to obtain a product A;
(2) milling the product A in a double-roller mill, and adding the product B into the mill during milling;
(3) standing the product B, and eliminating internal stress to obtain a product C;
(4) vulcanizing the product C in a two-stage vulcanization mode to obtain a vulcanized silicone rubber composite material;
in the step (1), the material comprises 1150 parts by weight of calcium carbonate 1100-;
in the step (2), the adding amount of the Shuangerwu is 0.6-0.7% of the mass of the silicon rubber, and the adding amount of the iron oxide red is 1.5-2.5% of the mass of the silicon rubber;
in the step (3), the standing time is 20-30 h;
in the step (4), the second-stage vulcanization is carried out in an oven at 110-150 ℃ for 1-3 hours, and then the temperature is raised to 170-220 ℃ for vulcanization for 30 min.
2. The method for preparing the silicone rubber composite material with shock-proof and fire-proof properties as claimed in claim 1, wherein: in the step 1), the silicon rubber comprises 1125 parts of calcium carbonate, 750 parts of glass beads and 15000 parts of silicon rubber by weight, wherein the mullite fiber accounts for 40% of the silicon rubber.
3. The method for preparing the silicone rubber composite material with shock-proof and fire-proof properties as claimed in claim 1, wherein: in the step 2), the adding amount of the bis-di-five is 0.67% of the mass of the silicon rubber, and the adding amount of the iron oxide red is 2% of the mass of the silicon rubber.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH08127716A (en) * | 1994-10-31 | 1996-05-21 | Shin Etsu Chem Co Ltd | Fire-resistant silicone rubber composition |
| CN106977925A (en) * | 2017-04-10 | 2017-07-25 | 武汉理工大学 | A kind of silicon rubber base heat-resisting composite and preparation method thereof |
| CN107556028A (en) * | 2017-07-28 | 2018-01-09 | 天津大学 | A kind of preparation method of mullite fiber high temperature insulating watt |
| CN110128831A (en) * | 2019-04-29 | 2019-08-16 | 华南理工大学 | It is a kind of with excellent at porcelain and the Ceramic silicon rubber of anti-flammability and the preparation method and application thereof |
| CN110643183A (en) * | 2019-10-10 | 2020-01-03 | 高静静 | Fire-resistant silicone rubber and preparation method thereof |
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2020
- 2020-04-15 CN CN202010296600.2A patent/CN111410843B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH08127716A (en) * | 1994-10-31 | 1996-05-21 | Shin Etsu Chem Co Ltd | Fire-resistant silicone rubber composition |
| CN106977925A (en) * | 2017-04-10 | 2017-07-25 | 武汉理工大学 | A kind of silicon rubber base heat-resisting composite and preparation method thereof |
| CN107556028A (en) * | 2017-07-28 | 2018-01-09 | 天津大学 | A kind of preparation method of mullite fiber high temperature insulating watt |
| CN110128831A (en) * | 2019-04-29 | 2019-08-16 | 华南理工大学 | It is a kind of with excellent at porcelain and the Ceramic silicon rubber of anti-flammability and the preparation method and application thereof |
| CN110643183A (en) * | 2019-10-10 | 2020-01-03 | 高静静 | Fire-resistant silicone rubber and preparation method thereof |
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