CN113512294A - Heat-resistant sealing material and preparation method thereof - Google Patents

Heat-resistant sealing material and preparation method thereof Download PDF

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Publication number
CN113512294A
CN113512294A CN202110375630.7A CN202110375630A CN113512294A CN 113512294 A CN113512294 A CN 113512294A CN 202110375630 A CN202110375630 A CN 202110375630A CN 113512294 A CN113512294 A CN 113512294A
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China
Prior art keywords
parts
heat
sealing material
resistant sealing
agent
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CN202110375630.7A
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Chinese (zh)
Inventor
王莹
殷盼
冯旭东
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Shaanxi Cologne New Material Technology Co ltd
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Shaanxi Cologne New Material Technology Co ltd
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Priority to CN202110375630.7A priority Critical patent/CN113512294A/en
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20Oxides; Hydroxides
    • C08K3/22Oxides; Hydroxides of metals
    • C08K3/2279Oxides; Hydroxides of metals of antimony
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/02Elements
    • C08K3/04Carbon
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/16Halogen-containing compounds
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/34Silicon-containing compounds
    • C08K3/36Silica
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00Use of organic ingredients
    • C08K5/04Oxygen-containing compounds
    • C08K5/14Peroxides
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00Properties
    • C08L2201/02Flame or fire retardant/resistant
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00Properties
    • C08L2201/08Stabilised against heat, light or radiation or oxydation

Abstract

The invention relates to a heat-resistant sealing material and a preparation method thereof, wherein the heat-resistant sealing material comprises the following raw materials in parts by weight: 100 parts of methyl vinyl silicone rubber; 20-40 parts of an inorganic filler; 2-10 parts of a micropore auxiliary agent; 3-12 parts of a flame retardant; 0.02-0.2 parts of a coloring agent; 0.5-5 parts of bis 2,5 vulcanizing agent. In the embodiment, by reasonably selecting the formula raw materials and setting the specific proportion, the tensile strength, the elongation at break and the hardness of the prepared heat-resistant sealing material after a heat-resistant test are not greatly changed, and the heat-resistant sealing material has excellent mechanical properties, better flame retardance and ablation resistance and lower density.

Description

Heat-resistant sealing material and preparation method thereof
Technical Field
The invention relates to the technical field of rubber materials, in particular to a heat-resistant sealing material and a preparation method thereof.
Background
The aviation kerosene is burnt in water at 450-550 ℃, so that the sealing performance of the equipment is guaranteed, a material which is flame-retardant and ablation-resistant under the high-temperature condition is needed, the material is required to have flame-retardant performance within a certain time, a sintering layer can be formed to prevent water from immersing, and the effect of protecting components inside the equipment is achieved.
At present, the flexible heat-resistant materials comprise nitrile rubber, ethylene propylene diene monomer rubber, silicone rubber and polyphosphazene elastomers. The nitrile rubber has alkene reaction activity, low decomposition rate, strong binding power and excellent ablation resistance, but has high density, high hardness and poor rebound resilience. And the cold resistance of the NBR structure is deteriorated due to the increase of the content of CAN in the NBR structure. The ethylene propylene diene monomer rubber has excellent ablation resistance and mechanical property, good chemical stability, lowest density, weak polarity, low surface energy, low bonding strength with metal, and poor self-adhesion and mutual adhesion. The silicon rubber has organic and inorganic properties, the Si-O bond energy of the silicon rubber is higher than that of C-C, the silicon rubber is not easy to break and decompose at high temperature, and the low-temperature performance is good. The organic part of the silicon rubber is decomposed into light non-condensation particles at high temperature, and the signal transmittance of the mineral part is high. The silicone rubber has good oxidation resistance and flame retardance, and is strong in micromolecule migration resistance, but the mechanical property of the silicone rubber is poor. To increase the flame retardant and ablation resistance, the amount of inorganic filler is increased, which results in an increased density of the material.
Accordingly, there is a need to ameliorate one or more of the problems with the related art solutions described above.
It is noted that this section is intended to provide a background or context to the disclosure as recited in the claims. The description herein is not admitted to be prior art by inclusion in this section.
Disclosure of Invention
An object of the present invention is to provide a heat-resistant sealing material and a method of manufacturing the same, which overcome, at least to some extent, one or more of the problems due to the limitations and disadvantages of the related art.
According to a first aspect, the invention provides a heat-resistant sealing material, which comprises the following raw materials in parts by weight:
100 parts of methyl vinyl silicone rubber;
20-40 parts of an inorganic filler;
2-10 parts of a micropore auxiliary agent;
3-12 parts of a flame retardant;
0.02-0.2 parts of a coloring agent;
0.5-5 parts of bis 2,5 vulcanizing agent.
In the invention, the flame retardant is antimony trioxide and chloroplatinic acid hexahydrate.
The invention comprises the following raw materials in parts by weight:
100 parts of methyl vinyl silicone rubber;
30 parts of inorganic filler;
5 parts of a micropore auxiliary agent;
8 parts of antimony trioxide;
0.2 part of chloroplatinic acid hexahydrate;
0.1 part of a coloring agent;
2 parts of a bis 2,5 vulcanizing agent.
In the present invention, the inorganic filler is at least one of silica and calcium carbonate.
In the invention, the micropore auxiliary agent is expanded microspheres.
In the invention, the flame retardant is at least one of magnesium hydroxide, aluminum hydroxide, calcium hydroxide, antimony trioxide and ammonium polyphosphate.
In the present invention, the coloring agent is carbon black.
According to a second aspect, the invention provides a heat-resistant sealing material, which comprises the following raw materials in parts by weight:
100 parts of methyl vinyl silicone rubber;
20-40 parts of an inorganic filler;
2-10 parts of a micropore auxiliary agent;
3-12 parts of a flame retardant;
0.02-0.2 parts of a coloring agent;
0.5-5 parts of bis 2,5 vulcanizing agent.
According to a third aspect, the present invention provides a method for preparing a heat-resistant sealing material, comprising the steps of:
uniformly mixing the methyl vinyl silicone rubber and the micropore auxiliary agent in an open mill, and then adding the inorganic filler, the flame retardant and the coloring agent for mixing;
and adding a bis 2,5 vulcanizing agent into the mixed material for vulcanization, and curing and molding to obtain the heat-resistant sealing material.
In the invention, the mixing time is 30-120 min.
In the invention, the vulcanization temperature is 160-180 ℃, and the vulcanization time is 5-15 min.
The technical scheme provided by the embodiment of the disclosure can have the following beneficial effects:
according to the heat-resistant sealing material, the formula raw materials are reasonably selected and the specific proportion is set, so that the tensile strength, the elongation at break and the hardness of the prepared heat-resistant sealing material are not greatly changed after a heat-resistant test, the heat-resistant sealing material has excellent mechanical properties, better flame retardance and ablation resistance and lower density.
Detailed Description
Example embodiments will now be described more fully. Example embodiments may, however, be embodied in many different forms and should not be construed as limited to the examples set forth herein; rather, these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the concept of example embodiments to those skilled in the art. The described features, structures, or characteristics may be combined in any suitable manner in one or more embodiments.
Example 1
The heat-resistant sealing material provided in the present example embodiment may include the following raw materials in parts by weight:
100 parts of methyl vinyl silicone rubber, 30 parts of inorganic filler, 5 parts of micropore auxiliary agent, 8 parts of flame retardant, 0.1 part of coloring agent and 2 parts of bis 2,5 vulcanizing agent.
Example 2
The heat-resistant sealing material provided in the present example embodiment may include the following raw materials in parts by weight:
100 parts of methyl vinyl silicone rubber, 30 parts of inorganic filler, 5 parts of micropore auxiliary agent, 8 parts of antimony trioxide, 0.2 part of chloroplatinic acid hexahydrate, 0.1 part of carbon black and 2 parts of bis 2,5 vulcanizing agent.
Example 3
The heat-resistant sealing material provided in the present example embodiment may include the following raw materials in parts by weight:
100 parts of methyl vinyl silicone rubber, 25 parts of silicon dioxide, 8 parts of micropore auxiliary agent, 10 parts of antimony trioxide, 0.4 part of chloroplatinic acid hexahydrate, 0.08 part of coloring agent and 3 parts of bis 2,5 vulcanizing agent.
Example 4
In the present exemplary embodiment, there is provided a method of preparing a heat-resistant sealing material, including the steps of:
(1) 100 parts of methyl vinyl silicone rubber and 8 parts of micropore auxiliary agent are put into an open mill to be mixed uniformly, and then 25 parts of silicon dioxide, 10 parts of antimony trioxide, 0.4 part of chloroplatinic acid hexahydrate and 0.08 part of coloring agent are added to be mixed for 60 min.
(2) And adding 3 parts of bis 2,5 vulcanizing agent into the mixed material, vulcanizing at 170 ℃ for 10min, and curing and molding to obtain the heat-resistant sealing material.
Example 5
In the present exemplary embodiment, there is provided a method of preparing a heat-resistant sealing material, including the steps of:
(1) 100 parts of methyl vinyl silicone rubber and 8 parts of micropore auxiliary agent are put into an open mill to be mixed uniformly, and then 25 parts of silicon dioxide, 10 parts of antimony trioxide, 0.4 part of chloroplatinic acid hexahydrate and 0.08 part of carbon black are added to be mixed for 90 min.
(2) And adding 3 parts of bis 2,5 vulcanizing agent into the mixed material, vulcanizing at 165 ℃ for 10min, and curing and molding to obtain the heat-resistant sealing material.
The heat-resistant sealing materials obtained in the above examples were subjected to the following performance tests:
fire resistance test
The test method refers to the GJB 323A ablation material ablation test method, the GB/T13488 rubber combustion performance measurement and vertical combustion method, and the GB/T2941 rubber sample environment regulation and test standard temperature, humidity and time.
1.1 principle of the test
The fire resistance of the material is measured by measuring the appearance, weight and performance changes of the sample before and after temperature (fire) resistance.
1.2 test specimens
(1) Sample size: the length is 135 + -3 mm, the width is 115 + -3 mm, and the thickness is 2 + -0.2 mm.
Note: other sample sizes may be used, but the minimum size of the cut piece that can be made tear resistant is guaranteed.
(2) One set of 2 samples.
1.3 test procedures
a. The number of the test sample and the filling of the test record.
b. The original thickness d1 of the test specimen was measured to the nearest 0.01mm and recorded.
c. The original weight m1 of the sample was weighed to the nearest 0.01g and recorded.
d. The steel plate, the sample and the steel plate are fixed in sequence by a clamp, the three parts are aligned on one side of the clamp to ensure temperature (fire) resistance, and a torque wrench is used for screwing and recording a torque value.
e. Then a thermocouple is connected at a temperature-resistant position, and a temperature measuring system is connected.
f. The alcohol burner is ignited, and the flame size is adjusted.
g. And adjusting the distance from the initial surface of the sample to the flame to ensure that the surface temperature of the initial sample is 450-550 ℃.
h. Keeping the temperature of the mixture at 450-550 ℃ for 30 min. The weight, thickness, tensile strength, elongation and hardness were measured and recorded after the sample was removed and left to stand in the laboratory for 24 hours.
1.4 test results
Test results are shown in table 1.
TABLE 1 fire (temp.) resistance data for refractory sealing materials
Figure DEST_PATH_IMAGE002
As can be seen from Table 1, the color changed from sea gray to gray black after burning; the thickness is not changed greatly, the weight is reduced by 0.08g, the tensile strength, the elongation at break and the hardness are not changed greatly, the flame retardant and the ablation resistance have excellent mechanical properties and lower density.
In the description herein, references to the description of the term "one embodiment," "some embodiments," "an example," "a specific example," or "some examples," etc., mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the present disclosure. In this specification, the schematic representations of the terms used above are not necessarily intended to refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Furthermore, various embodiments or examples described in this specification can be combined and combined by those skilled in the art.
Other embodiments of the disclosure will be apparent to those skilled in the art from consideration of the specification and practice of the disclosure disclosed herein. This application is intended to cover any variations, uses, or adaptations of the disclosure following, in general, the principles of the disclosure and including such departures from the present disclosure as come within known or customary practice within the art to which the disclosure pertains. It is intended that the specification and examples be considered as exemplary only, with a true scope and spirit of the disclosure being indicated by the following claims.

Claims (10)

1. The heat-resistant sealing material is characterized by comprising the following raw materials in parts by weight:
100 parts of methyl vinyl silicone rubber;
20-40 parts of an inorganic filler;
2-10 parts of a micropore auxiliary agent;
3-12 parts of a flame retardant;
0.02-0.2 parts of a coloring agent;
0.5-5 parts of bis 2,5 vulcanizing agent.
2. The heat-resistant sealing material according to claim 1, wherein the flame retardant is antimony trioxide and chloroplatinic acid hexahydrate.
3. The heat-resistant sealing material according to claim 2, characterized by comprising the following raw materials in parts by weight:
100 parts of methyl vinyl silicone rubber;
30 parts of inorganic filler;
5 parts of a micropore auxiliary agent;
8 parts of antimony trioxide;
0.2 part of chloroplatinic acid hexahydrate;
0.1 part of a coloring agent;
2 parts of a bis 2,5 vulcanizing agent.
4. The heat-resistant sealing material according to claim 1, wherein the inorganic filler is at least one of silica and calcium carbonate.
5. The heat resistant seal material of claim 1 wherein the cell site agent is expanded microspheres.
6. The heat-resistant sealing material according to claim 1, wherein the flame retardant is at least one of magnesium hydroxide, aluminum hydroxide, calcium hydroxide, antimony trioxide and ammonium polyphosphate.
7. The heat-resistant sealing material is characterized by comprising the following raw materials in parts by weight:
100 parts of methyl vinyl silicone rubber;
20-40 parts of an inorganic filler;
2-10 parts of a micropore auxiliary agent;
3-12 parts of a flame retardant;
0.02-0.2 parts of a coloring agent;
0.5-5 parts of bis 2,5 vulcanizing agent.
8. A method of preparing a heat resistant sealing material according to any of claims 1 to 7, characterized by comprising the steps of:
uniformly mixing the methyl vinyl silicone rubber and the micropore auxiliary agent in an open mill, and then adding the inorganic filler, the flame retardant and the coloring agent for mixing;
and adding a bis 2,5 vulcanizing agent into the mixed material for vulcanization, and curing and molding to obtain the heat-resistant sealing material.
9. The heat-resistant sealing material according to claim 8, wherein the kneading time is 30 to 120 min.
10. The heat-resistant sealing material according to claim 8, wherein the vulcanization temperature is 160 to 180 ℃ and the vulcanization time is 5 to 15 min.
CN202110375630.7A 2021-04-08 2021-04-08 Heat-resistant sealing material and preparation method thereof Pending CN113512294A (en)

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Application Number Priority Date Filing Date Title
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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2017070893A1 (en) * 2015-10-29 2017-05-04 国家纳米科学中心 Ceramic silicone rubber, preparation method and use thereof
CN107760038A (en) * 2017-10-31 2018-03-06 中国人民武装警察部队学院 Expansion can porcelain SiClx rubber composite and preparation method thereof
CN107778870A (en) * 2016-08-30 2018-03-09 沈阳顺风新材料有限公司 A kind of novel fire resistant silicon rubber and preparation method thereof
CN108587181A (en) * 2018-03-21 2018-09-28 上海大学 One kind can porcelain SiClx rubber thermally protective materials and preparation method thereof
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
CN111004511A (en) * 2019-12-30 2020-04-14 广东聚合科技股份有限公司 High-strength high-temperature-resistant flame-retardant silicone rubber and preparation method thereof

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2017070893A1 (en) * 2015-10-29 2017-05-04 国家纳米科学中心 Ceramic silicone rubber, preparation method and use thereof
CN107778870A (en) * 2016-08-30 2018-03-09 沈阳顺风新材料有限公司 A kind of novel fire resistant silicon rubber and preparation method thereof
CN107760038A (en) * 2017-10-31 2018-03-06 中国人民武装警察部队学院 Expansion can porcelain SiClx rubber composite and preparation method thereof
CN108587181A (en) * 2018-03-21 2018-09-28 上海大学 One kind can porcelain SiClx rubber thermally protective materials and preparation method thereof
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
CN111004511A (en) * 2019-12-30 2020-04-14 广东聚合科技股份有限公司 High-strength high-temperature-resistant flame-retardant silicone rubber and preparation method thereof

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Application publication date: 20211019