CN112625447A - Fireproof and fireproof silicon rubber material and preparation method thereof - Google Patents

Fireproof and fireproof silicon rubber material and preparation method thereof Download PDF

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Publication number
CN112625447A
CN112625447A CN202011498028.4A CN202011498028A CN112625447A CN 112625447 A CN112625447 A CN 112625447A CN 202011498028 A CN202011498028 A CN 202011498028A CN 112625447 A CN112625447 A CN 112625447A
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parts
fire
resistant
fireproof
silicon rubber
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郑亚森
臧育锋
张磊
曹俊
秦克良
宋永琦
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Shanghai Keter New Materials Co ltd
Changzhou Woke Technology Co ltd
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Shanghai Keter New Materials Co ltd
Changzhou Woke Technology Co ltd
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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
    • C08L83/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
    • C08L83/04—Polysiloxanes
    • 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
    • C08K2003/2217—Oxides; Hydroxides of metals of magnesium
    • C08K2003/222—Magnesia, i.e. magnesium oxide
    • 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
    • C08K2003/2227—Oxides; Hydroxides of metals of aluminium
    • 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
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00—Properties
    • C08L2201/14—Gas barrier composition
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2203/00—Applications
    • C08L2203/20—Applications use in electrical or conductive gadgets
    • C08L2203/202—Applications use in electrical or conductive gadgets use in electrical wires or wirecoating
    • 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
    • C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
    • C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend

Abstract

The invention relates to the technical field of silicon rubber materials, in particular to a fireproof silicon rubber material and a preparation method thereof. The raw material of the fireproof and fire-resistant silicon rubber material can comprise an A component and a B component. The component A comprises first silicon rubber, white carbon black, aluminum hydroxide, wollastonite, silicon oil and a silane coupling agent. The component B comprises second silicon rubber, magnesium oxide and boric acid. The fireproof and fire-resistant silicon rubber material can be rapidly decomposed to react to release gas, insulate oxygen and resist fire when meeting high temperature or flame above 400 ℃, residues rapidly form a hard shell-shaped substance, has small expansion deformation, good fireproof, fire-resistant and oxygen-insulated flame resistance, can achieve self-extinguishing when being away from fire, and has good processing performance and low cost. The double-layer flame-retardant oxygen-insulating layer can simultaneously play the double-layer effects of the flame-retardant layer and the oxygen-insulating layer when being applied to a wire and cable structure.

Description

Fireproof and fireproof silicon rubber material and preparation method thereof
Technical Field
The invention relates to the technical field of silicon rubber materials, in particular to a fireproof silicon rubber material and a preparation method thereof.
Background
With the development of the country and the improvement of the living standard of people, large public facilities such as high-rise buildings, large supermarkets, subways, tunnels and the like and entertainment places are increasing day by day. The fire accidents cause great casualties and property losses every year, the fire protection and fire prevention are more and more prominent, and the requirements for flame retardance and fire resistance in the aspects of wires and cables are increased.
However, the general fireproof materials have no fireproof function, so that the smoothness of electric power cannot be kept under the condition of a big fire, and the safety of electricity utilization of personnel is ensured; the fire-resistant materials appearing in the current market are expensive and have poor flame retardance, and the fire-resistant electric wire and cable have complex structures. To above problem, this patent development novel oxygen-insulating filling material can solve fire-retardant fire-resistant problem in one step, has very both simplified original fire resisting cable structure, can reduce cost again, guarantees that wire and cable keeps electric power unobstructed under the conflagration condition, leaves more sufficient escape time.
The flame retardant and fire resistant requirements of electric wires and cables are increasing day by day, flame retardant and fire resistant materials are developed more and more in recent years, but few materials can simultaneously meet the two performances of flame retardance and fire resistance. At present, the flame-retardant fire-resistant cable mainly meets the flame-retardant fire-resistant requirements in a mode of adding an oxygen-insulating layer, a flame-retardant layer and a flame-retardant sheath independently. The cable has complex structure, complex processing technique and high manufacturing cost.
Disclosure of Invention
In view of the above-mentioned drawbacks of the prior art, an object of the present invention is to provide a fire-resistant and fire-resistant silicone rubber material and a method for preparing the same, which solve the problems of the prior art.
In order to achieve the above and other related objects, an aspect of the present invention provides a fire-resistant and fire-resistant silicone rubber material, the material of which comprises a group a and a group B;
the component A comprises the following raw materials in parts by weight:
Figure BDA0002842760650000011
the component B comprises the following raw materials in parts by weight:
30-50 parts of second silicon rubber;
1-5 parts of magnesium oxide;
10-30 parts of boric acid.
In some embodiments of the present invention, the raw materials of the component a comprise the following components in parts by weight:
Figure BDA0002842760650000021
the component B comprises the following raw materials in parts by weight:
40-50 parts of second silicon rubber;
1-5 parts of magnesium oxide;
20-30 parts of boric acid.
In some embodiments of the invention, the first and second silicone rubbers are selected from methyl vinyl silicone rubber and/or methyl silicone rubber; the first and second silicone rubbers may be the same or different.
In some embodiments of the present invention, the methyl vinyl silicone rubber has a molecular weight of 50 to 80 ten thousand; the content of vinyl in the methyl vinyl silicone rubber is 0.05-0.3%.
In some embodiments of the present invention, the methyl silicone rubber has a molecular weight of 50 to 80 ten thousand.
In some embodiments of the present invention, the silica has a specific surface area of 10m2/g～180m2/g。
In some embodiments of the invention, the wollastonite has a needle-like structure, a length-diameter ratio of 8:1 to 20:1, and a high-temperature ignition loss of less than 3%.
In some embodiments of the invention, the silicone oil is one or a mixture of two of hydroxyl silicone oil and methoxyl silicone oil; the viscosity is 10-50 mm2/s。
In some embodiments of the invention, the magnesium oxide is active magnesium oxide with a specific surface area of 10-80 m2/g。
In another aspect, the invention provides a preparation method of the fireproof and fire-resistant silicone rubber material, wherein the preparation method comprises the following steps: mixing first silicon rubber, white carbon black, aluminum hydroxide, wollastonite, silicon oil and a silane coupling agent to obtain a component A; mixing the second silicon rubber, magnesium oxide and boric acid to obtain a component B; and mixing the component A and the component B to obtain the fireproof and fire-resistant silicon rubber material.
The invention also provides a fireproof and fire-resistant silicone rubber product, and the raw materials of the fireproof and fire-resistant silicone rubber product comprise the fireproof and fire-resistant silicone rubber material and a vulcanizing agent.
In some embodiments of the invention, the vulcanizing agent is a peroxide vulcanizing agent.
The invention also provides the application of the fireproof and fire-resistant silicone rubber material or the fireproof and fire-resistant silicone rubber product in cables.
Detailed Description
Through a large amount of exploration experiments, the inventor of the invention obtains a component A (base rubber A) by mixing first silicon rubber, white carbon black, aluminum hydroxide, wollastonite, silicon oil and a silane coupling agent in the formula of the silicon rubber; mixing the second silicon rubber, magnesium oxide and boric acid to obtain a component B (base rubber B); and mixing the component A and the component B to prepare the fireproof and fire-resistant silicon rubber material. Wherein the base rubber A is subjected to high-temperature vacuum heat treatment during kneading, and the base rubber B is not subjected to heat treatment during kneading. The raw materials of magnesium oxide and boric acid of the base rubber B can not be heated in the processing process, the sizing material can generate a structuralization phenomenon after high-temperature treatment, and the sizing roller can be glued and cannot be processed. The fireproof and fire-resistant silicon rubber material disclosed by the invention can be rapidly decomposed and reacted to release gas, isolate oxygen and resist flame when meeting high temperature or flame above 400 ℃, residues rapidly form a hard shell-shaped substance, the expansion deformation is small, the fireproof, fire-resistant and oxygen-isolation flame-resistant silicon rubber material has good fireproof, fire-resistant and oxygen-isolation flame-resistant properties, can achieve self-extinguishing when being away from fire, and is good in processing performance and low in cost. The double-layer flame-retardant oxygen-insulating layer can simultaneously play the double-layer effects of the flame-retardant layer and the oxygen-insulating layer when being applied to a wire and cable structure. On the basis of this, the present invention has been completed.
The invention provides a fireproof and fire-resistant silicon rubber material, which can be prepared from the following raw materials of an A component and a B component.
The raw materials of the component A comprise first silicon rubber, white carbon black, aluminum hydroxide, wollastonite, silicone oil and a silane coupling agent.
In the fireproof and fire-resistant silicon rubber material provided by the invention, the component A can comprise 50-70 parts of first silicon rubber according to the parts by weight of raw materials. In some embodiments, the weight part of the first silicone rubber can be 50-60 parts; 60-70 parts; 50-55 parts; 55-60 parts; 60-65 parts; or 65-70 parts. The first silicone rubber is selected from methyl vinyl silicone rubber and/or methyl silicone rubber.
In the first silicon rubber, the vinyl content in the methyl vinyl silicon rubber is 0.05-0.3%. In some embodiments, the methyl vinyl silicone rubber may have a vinyl content of 0.05% to 0.1%; 0.1% -0.15%; 0.15% -0.2%; 0.2% -0.25%; 0.25% -0.3%; or 0.08% -0.28%; 0.1% -0.25%; 0.05% -0.15%; or 0.15 to 0.3 percent and the like. The molecular weight of the methyl vinyl silicone rubber is 50-80 ten thousand. In some embodiments, the methyl vinyl silicone rubber has a molecular weight of 50 to 60, 60 to 70, ten thousand; 70-80 ten thousand; or 50 to 55 ten thousand; 55 ten thousand to 60 ten thousand; 60-65 ten thousand; 65-70 ten thousand; 70-75 ten thousand; or 75 to 80 million.
In the first silicone rubber, the molecular weight of the methyl silicone rubber is 50 to 80 ten thousand. In some embodiments, the methyl silicone rubber has a molecular weight of 50 to 60, 60 to 70, ten thousand; 70-80 ten thousand; or 50 to 55 ten thousand; 55 ten thousand to 60 ten thousand; 60-65 ten thousand; 65-70 ten thousand; 70-75 ten thousand; or 75 to 80 million.
In the fireproof and fire-resistant silicon rubber material provided by the invention, the component A can also comprise 10-30 parts of white carbon black according to the weight parts of the raw materials. In some embodiments, the white carbon black may also be 10 to 20 parts by weight; 20-30 parts of a solvent; 10-15 parts; 15-20 parts of a solvent; 20-25 parts; 25-30 parts of a solvent; 12-28 parts; 15-25 parts; or 18 to 22 parts by weight. The specific surface area of the white carbon black is 10m2/g～180m2(ii) in terms of/g. In some embodiments, the specific surface area of the white carbon black can also be 10m2/g～50m2/g；50m2/g～100m2/g；100m2/g～150m2/g；150m2/g～180m2/g；20m2/g～170m2/g；30m2/g～160m2/g；40m2/g～150m2/g；50m2/g～140m2/g；60m2/g～130m2/g；70m2/g～120m2/g；80m2/g～110m2(ii)/g; or 90m2/g～100m2And/g, etc.
In the fireproof and fire-resistant silicon rubber material provided by the invention, the component A can also comprise 20-80 parts of aluminum hydroxide according to the parts by weight of the raw materials. In some embodiments, the aluminum hydroxide may also be 20-40 parts; 40-80 parts; 20-30 parts of a solvent; 30-40 parts; 40-50 parts; 50-60 parts; 60-70 parts; 70-80 parts; 25-75 parts; 30-70 parts; 35-65 parts; 40-60 parts; or 45-55 parts and the like.
In the fireproof and fire-resistant silicon rubber material provided by the invention, the component A can also comprise 10-20 parts of wollastonite in parts by weight of raw materials. In some embodiments, the wollastonite can also be 10-15 parts; 15-20 parts of a solvent; 10-12 parts; 12-15 parts; 15-18 parts; 18-20 parts; 12-18 parts; or 14-16 parts and the like. The wollastonite is of a needle-like structure, and the length-diameter ratio of the wollastonite can be 8: 1-20: 1, 9: 1-20: 1, 10: 1-20: 1, 11: 1-20: 1, 12: 1-20: 1, 13: 1-20: 1, 14: 1-20: 1, 15: 1-20: 1, 16: 1-20: 1, 17: 1-20: 1, 18: 1-20: 1 and the like. The loss on ignition at high temperature is less than 3 percent. In some embodiments, the high temperature loss on ignition is 0.1 to 2.99%; 0.5-2.99%; 1 to 2.99 percent; 1.5-2.99%; 2 to 2.99 percent; or 2.5-2.99%, etc.
In the fireproof and fire-resistant silicon rubber material provided by the invention, the component A can also comprise 5-15 parts of silicone oil according to the weight parts of the raw materials. In some embodiments, the silicone oil may also be 5-10 parts; 10-15 parts; 5-8 parts; 8-10 parts; 10-12 parts; 12-15 parts; 6-13 parts; 7-12 parts; or 8-11 parts and the like. Wherein, the silicone oil is one or the mixture of hydroxyl silicone oil and methoxyl silicone oil. The viscosity of the silicone oil can be 10-20 mm2/s；20～30mm2/s；30～40mm2/s；40～50mm2/s；15～45mm2/s；20～40mm2S; or 25 to 35mm2And/s, etc. The molecular weight of the hydroxyl silicone oil can be 400-1500; 400-800 parts; 800-1500; 400-600 parts; 600-800 parts; 800-1000 parts; 1000-1200; or 1200 to 1500. The molecular weight of the methoxy silicon oil can be 400-1500; 400-800 parts; 800-1500; 400-600 parts; 600-800 parts; 800-1000 parts; 1000-1200; or 1200 to 1500. Viscosity is used to distinguish the fluidity of the silicone oil, and the viscosity of the hydroxy silicone oil or methoxy silicone oil is also within the range defined by the viscosity of the silicone oil.
In the fireproof and fire-resistant silicon rubber material provided by the invention, the component A can also comprise 0.5-3 parts of silane coupling agent by weight of raw materials. In some embodiments, the silane coupling agent may also be 0.5 to 1 part; 1-3 parts; 1-1.5 parts; 1.5-2 parts; 2-2.5 parts; 2.5-3 parts; 0.5-2.5 parts; 0.8-2.2 parts; or 1-2 parts and the like. The silane coupling agent is selected from A171. A171 has the chemical name vinyltrimethoxysilane.
The raw materials of the component B comprise second silicon rubber, magnesium oxide and boric acid.
In the fireproof and fire-resistant silicon rubber material provided by the invention, the component B can comprise 30-50 parts of second silicon rubber according to the weight parts of raw materials. In some embodiments, the second silicone rubber may also be 30 to 40 parts by weight; 40-50 parts; 30-35 parts of a solvent; 35-40 parts of a solvent; 40-45 parts of a solvent; or 45 to 50 parts by weight. The second silicon rubber is selected from methyl vinyl silicon rubber and/or methyl silicon rubber. The first and second silicone rubbers may be the same or different.
In the second silicon rubber, the vinyl content in the methyl vinyl silicon rubber is 0.05-0.3%. In some embodiments, the methyl vinyl silicone rubber may have a vinyl content of 0.05% to 0.1%; 0.1% -0.15%; 0.15% -0.2%; 0.2% -0.25%; 0.25% -0.3%; or 0.08% -0.28%; 0.1% -0.25%; 0.05% -0.15%; or 0.15 to 0.3 percent and the like. The molecular weight of the methyl vinyl silicone rubber is 50-80 ten thousand. In some embodiments, the methyl vinyl silicone rubber has a molecular weight of 50 to 60, 60 to 70, ten thousand; 70-80 ten thousand; or 50 to 55 ten thousand; 55 ten thousand to 60 ten thousand; 60-65 ten thousand; 65-70 ten thousand; 70-75 ten thousand; or 75 to 80 million.
In the second silicone rubber, the molecular weight of the methyl silicone rubber is 50 to 80 ten thousand. In some embodiments, the methyl silicone rubber has a molecular weight of 50 to 60, 60 to 70, ten thousand; 70-80 ten thousand; or 50 to 55 ten thousand; 55 ten thousand to 60 ten thousand; 60-65 ten thousand; 65-70 ten thousand; 70-75 ten thousand; or 75 to 80 million.
In the fireproof and fire-resistant silicon rubber material provided by the invention, the component B can comprise 1-5 parts of magnesium oxide according to the parts by weight of the raw materials. In some embodiments, the weight parts of magnesium oxide may be 1-2 parts; 2-3 parts of a solvent; 3-4 parts; 4-5 parts; 1-4.5 parts; 1-4 parts; or 1.5-3.5 parts. The magnesium oxide is active magnesium oxide, and the specific surface area can be 10-80m2/g；10～40m2/g；40～80m2/g；10～20m2/g；20～30m2/g；30～40m2/g；40～50m2/g；50～60m2/g；60～70m2/g；70～80m2(ii)/g; or 30m2And/g, etc.
In the fireproof and fire-resistant silicon rubber material provided by the invention, the component B can comprise 10-30 parts of boric acid by weight of raw materials. In some embodiments, the boric acid may also be present in an amount of 10 to 20 parts by weight; 20-30 parts of a solvent; 10-15 parts; 15-20 parts of a solvent; 20-25 parts; 25-30 parts; 12-28 parts; 15-25 parts; or 18-23 parts.
In a specific embodiment, the fireproof and fire-resistant silicon rubber material comprises the following components in parts by weight:
the component A comprises the following raw materials in parts by weight:
Figure BDA0002842760650000051
Figure BDA0002842760650000061
the component B comprises the following raw materials in parts by weight:
30-50 parts of second silicon rubber;
1-5 parts of magnesium oxide;
10-30 parts of boric acid.
As a preferred embodiment, the raw materials of the fireproof and fire-resistant silicon rubber material comprise the following components in parts by weight:
the component A comprises the following raw materials in parts by weight:
Figure BDA0002842760650000062
the component B comprises the following raw materials in parts by weight:
40-50 parts of second silicon rubber;
1-5 parts of magnesium oxide;
20-30 parts of boric acid.
In another aspect, the present invention provides a preparation method of the fireproof and fire-resistant silicone rubber material of the first aspect, the preparation method comprising: mixing first silicon rubber, white carbon black, aluminum hydroxide, wollastonite, silicon oil and a silane coupling agent to obtain a component A; mixing the second silicon rubber, magnesium oxide and boric acid to obtain a component B; and mixing the component A and the component B to prepare the fireproof and fire-resistant silicon rubber material.
In the preparation method of the fireproof and fire-resistant silicon rubber material, the first silicon rubber is added into a first kneading machine and kneaded for 5-10 min, then the white carbon black, the aluminum hydroxide, the wollastonite, the coupling agent and the silicon oil are added for 5-10 times, and the mixture is kneaded for 10-15 min each time to form a mass; continuing kneading and heating to 130 ℃ for vacuum heat treatment, wherein the kneading temperature in the kneading machine is 130-170 ℃, the time is 0.5-1.5 h, and the vacuum degree is-0.06-0.1 Mpa; obtaining the component A (base rubber A) and cooling.
In the preparation method of the fireproof and fire-resistant silicon rubber material, the second silicon rubber is added into a second kneader and kneaded for 5-10 min, then boric acid and magnesium oxide are added for 2-5 times and kneaded for 10min each time, and after agglomeration, a component B (base rubber B) is obtained.
In the preparation method of the fireproof and fire-resistant silicon rubber material, the component A (base rubber A) and the component B (base rubber B) are fully and uniformly mixed in a kneader to obtain the fireproof and fire-resistant silicon rubber material,
the invention also provides a fireproof and fire-resistant silicon rubber product, which comprises the fireproof and fire-resistant silicon rubber material and a vulcanizing agent.
In the fireproof and fire-resistant silicon rubber product provided by the invention, the raw materials can comprise 0.5-3 parts by weight of vulcanizing agent. In some embodiments, the vulcanizing agent may also be 0.5 to 1 part by weight; 1-2 parts; 2-3 parts of a solvent; 0.5-1.5 parts; or 1.5-3 parts, etc. The vulcanizing agent is a peroxide vulcanizing agent, preferably one of bis 24, bis 25 or DCP. The chemical name of the vulcanizing agent bis 24 is 2, 4-dichloro benzoyl peroxide CAS: 133-14-2.
On the other hand, the invention provides a preparation method of the fireproof and fire-resistant silicone rubber product, and a vulcanizing agent is added into the prepared fireproof and fire-resistant silicone rubber material. According to different product performances and application requirements, a corresponding vulcanizing agent can be added, and the fireproof and fire-resistant silicone rubber product can be obtained through high-temperature vulcanization.
The invention further provides application of the fireproof and fire-resistant silicone rubber material and/or the fireproof and fire-resistant silicone rubber product in cables. The fireproof and fire-resistant silicone rubber material and the fireproof and fire-resistant silicone rubber product are mainly applied to a cable filling layer or a fire-resistant layer, silicone rubber extrusion equipment is used for production, drying tunnel vulcanization or sulfur connection process production can be used, the production efficiency is high, the cost can be greatly reduced, through reasonable structural design, a fire-resistant cable using ceramic filling rubber can pass the severe fire-resistant standards such as BS6387 and the like, the heat dissipation of the cable is good under a normal state, and the ceramic rubber can be quickly ablated into a hard shell under the fire condition, so that the smoothness of a line under the fire condition is guaranteed.
As mentioned above, the fireproof and fire-resistant silicone rubber material prepared by the invention has the following technical effects:
the fireproof and fire-resistant silicon rubber material and the fireproof and fire-resistant silicon rubber product can be rapidly decomposed and reacted to release gas, isolate oxygen and resist fire when meeting high temperature or flame above 400 ℃, residues rapidly form hard shell-shaped objects, the expansion deformation is small, the fireproof and fire-resistant silicon rubber material and the fireproof and fire-resistant silicon rubber product have good fireproof, fire-resistant and oxygen-isolating flame resistance, can achieve self-extinguishing when being away from fire, and are good in processing performance and low in cost. The double-layer flame-retardant oxygen-insulating layer can simultaneously play the double-layer effects of the flame-retardant layer and the oxygen-insulating layer when being applied to a wire and cable structure.
The following examples are provided to further illustrate the advantageous effects of the present invention.
In order to make the objects, technical solutions and advantageous technical effects of the present invention more clear, the present invention is further described in detail below with reference to examples. However, it should be understood that the embodiments of the present invention are only for explaining the present invention and are not for limiting the present invention, and the embodiments of the present invention are not limited to the embodiments given in the specification. The examples were prepared under conventional conditions or conditions recommended by the material suppliers without specifying specific experimental conditions or operating conditions.
Furthermore, it is to be understood that one or more method steps mentioned in the present invention does not exclude that other method steps may also be present before or after the combined steps or that other method steps may also be inserted between these explicitly mentioned steps, unless otherwise indicated; it is also to be understood that a combined connection between one or more devices/apparatus as referred to in the present application does not exclude that further devices/apparatus may be present before or after the combined device/apparatus or that further devices/apparatus may be interposed between two devices/apparatus explicitly referred to, unless otherwise indicated. Moreover, unless otherwise indicated, the numbering of the various method steps is merely a convenient tool for identifying the various method steps, and is not intended to limit the order in which the method steps are arranged or the scope of the invention in which the invention may be practiced, and changes or modifications in the relative relationship may be made without substantially changing the technical content.
In the following examples, reagents, materials and instruments used are commercially available unless otherwise specified.
In the following examples and comparative examples, unless otherwise specified, the first silicone rubber and the second silicone rubber were used in a model number of 110-0, both from Hesheng silicon industries, Ltd.
The coupling agent is purchased from Nanjing Endocide New Material technology Co., Ltd. with model number A171.
The hydroxyl silicone oil manufacturer is Sn-free Rahel environmental protection science and technology Co., Ltd, and the model is QLS-203.
Wollastonite was purchased from denna bofa chemical model as ultrafine wollastonite powder 1250.
The white carbon black is purchased from Weifang Sanjia chemical industry with model number SJ-34.
Example 1
Adding 60 parts of first silicon rubber 110-0 into a first kneader, kneading for 10min, then adding 20 parts of white carbon black SJ-34, 50 parts of aluminum hydroxide, 20 parts of wollastonite 1250, 1.6 parts of coupling agent A171 and 8 parts of hydroxy silicone oil QLS-203 for 7 times, kneading for 15min each time, and after agglomeration; continuing kneading and heating to 130 ℃ for vacuum heat treatment, wherein the kneading temperature in the kneader is 160 ℃, the time is 1h, and the vacuum degree is-0.08 Mpa; obtaining the base rubber A and cooling.
And adding 40 parts of second silicon rubber 110-0 into a second kneader, kneading for 10min, adding 20 parts of boric acid and 3 parts of magnesium oxide for 3 times, kneading for 10min each time, and obtaining the base rubber B after agglomeration.
And (3) fully and uniformly mixing the base rubber A and the base rubber B in a kneader to obtain the fireproof and fire-resistant silicon rubber material required by the patent. 1.5 parts of vulcanizing agent bis 24 is added into the fireproof and fire-resistant silicon rubber material on an open mill, and the mixture is uniformly mixed to prepare the fireproof and fire-resistant silicon rubber product.
Example 2
Adding 60 parts of first silicon rubber 110-0 into a first kneader, kneading for 10min, adding 30 parts of white carbon black SJ-34, 50 parts of aluminum hydroxide, 20 parts of wollastonite 1250, 2 parts of coupling agent A171 and 10 parts of hydroxy silicone oil QLS-203 for 8 times, kneading for 15min each time, and after agglomeration; continuing kneading and heating to 130 ℃ for vacuum heat treatment, wherein the kneading temperature in the kneader is 160 ℃, the time is 1h, and the vacuum degree is-0.08 Mpa; obtaining the base rubber A and cooling.
And adding 40 parts of second silicon rubber 110-0 into a second kneader, kneading for 10min, adding 20 parts of boric acid and 3 parts of magnesium oxide for 3 times, kneading for 10min each time, and obtaining the base rubber B after agglomeration.
And (3) fully and uniformly mixing the base rubber A and the base rubber B in a kneader to obtain the fireproof and fire-resistant silicon rubber material required by the patent. 1.5 parts of vulcanizing agent bis 24 is added into the fireproof and fire-resistant silicon rubber material on an open mill, and the mixture is uniformly mixed to prepare the fireproof and fire-resistant silicon rubber product.
Example 3
Adding 60 parts of first silicon rubber 110-0 into a first kneader, kneading for 10min, adding 20 parts of white carbon black SJ-34, 80 parts of aluminum hydroxide, 10 parts of wollastonite 1250, 2.4 parts of coupling agent A171 and 12 parts of hydroxy silicone oil QLS-203 for 9 times, kneading for 15min each time, and after agglomeration; continuing kneading and heating to 130 ℃ for vacuum heat treatment, wherein the kneading temperature in the kneader is 170 ℃, the time is 1h, and the vacuum degree is-0.08 Mpa; obtaining the base rubber A and cooling.
And adding 40 parts of second silicon rubber 110-0 into a second kneader, kneading for 10min, adding 20 parts of boric acid and 3 parts of magnesium oxide for 3 times, kneading for 10min each time, and obtaining the base rubber B after agglomeration.
And (3) fully and uniformly mixing the base rubber A and the base rubber B in a kneader to obtain the fireproof and fire-resistant silicon rubber material required by the patent. 1.5 parts of vulcanizing agent bis 24 is added into the fireproof and fire-resistant silicon rubber material on an open mill, and the mixture is uniformly mixed to prepare the fireproof and fire-resistant silicon rubber product.
Example 4
Adding 60 parts of first silicon rubber 110-0 into a first kneader, kneading for 10min, adding 30 parts of white carbon black SJ-34, 80 parts of aluminum hydroxide, 20 parts of wollastonite 1250, 3 parts of coupling agent A171 and 15 parts of hydroxy silicone oil QLS-203 for 10 times, kneading for 15min each time, and after agglomeration; continuing kneading and heating to 130 ℃ for vacuum heat treatment, wherein the kneading temperature in the kneader is 160 ℃, the time is 1h, and the vacuum degree is-0.08 Mpa; obtaining the base rubber A and cooling.
And adding 40 parts of second silicon rubber 110-0 into a second kneader, kneading for 10min, adding 30 parts of boric acid and 5 parts of magnesium oxide for 4 times, kneading for 10min each time, and obtaining the base rubber B after agglomeration.
And (3) fully and uniformly mixing the base rubber A and the base rubber B in a kneader to obtain the fireproof and fire-resistant silicon rubber material required by the patent. 1.5 parts of vulcanizing agent bis 24 is added into the fireproof and fire-resistant silicon rubber material on an open mill, and the mixture is uniformly mixed to prepare the fireproof and fire-resistant silicon rubber product.
Example 5
Adding 60 parts of first silicon rubber 110-0 into a first kneader, kneading for 10min, adding 30 parts of white carbon black SJ-34, 20 parts of aluminum hydroxide, 20 parts of wollastonite 1250, 1 part of coupling agent A171 and 5 parts of hydroxy silicone oil QLS-203 for 5 times, kneading for 15min each time, and after agglomeration; continuing kneading and heating to 130 ℃ for vacuum heat treatment, wherein the kneading temperature in the kneader is 150 ℃, the time is 1h, and the vacuum degree is-0.08 Mpa; obtaining the base rubber A and cooling.
And adding 40 parts of second silicon rubber 110-0 into a second kneader, kneading for 10min, adding 20 parts of boric acid and 2 parts of magnesium oxide for 2 times, kneading for 10min each time, and obtaining the base rubber B after agglomeration.
And (3) fully and uniformly mixing the base rubber A and the base rubber B in a kneader to obtain the fireproof and fire-resistant silicon rubber material required by the patent. 1.5 parts of vulcanizing agent bis 24 is added into the fireproof and fire-resistant silicon rubber material on an open mill, and the mixture is uniformly mixed to prepare the fireproof and fire-resistant silicon rubber product.
Example 6
Adding 60 parts of first silicon rubber 110-0 into a first kneader, kneading for 10min, adding 30 parts of white carbon black SJ-34, 20 parts of aluminum hydroxide, 15 parts of wollastonite 1250, 1.2 parts of coupling agent A171 and 6 parts of hydroxy silicone oil QLS-203 for 6 times, kneading for 15min each time, and after agglomeration; continuing kneading and heating to 130 ℃ for vacuum heat treatment, wherein the kneading temperature in the kneader is 150 ℃, the time is 1h, and the vacuum degree is-0.08 Mpa; obtaining the base rubber A and cooling.
And adding the rest 40 parts of silicon rubber 110-0 into a second kneader, kneading for 10min, adding 20 parts of boric acid and 5 parts of magnesium oxide for 3 times, kneading for 10min each time, and obtaining the base rubber B after agglomeration.
And (3) fully and uniformly mixing the base rubber A and the base rubber B in a kneader to obtain the fireproof and fire-resistant silicon rubber material required by the patent. 1.5 parts of vulcanizing agent bis 24 is added into the fireproof and fire-resistant silicon rubber material on an open mill, and the mixture is uniformly mixed to prepare the fireproof and fire-resistant silicon rubber product.
Example 7
Adding 60 parts of first silicon rubber 110-0 into a first kneader, kneading for 10min, adding 15 parts of white carbon black SJ-34, 40 parts of aluminum hydroxide, 15 parts of wollastonite 1250, 1.2 parts of coupling agent A171 and 6 parts of hydroxy silicone oil QLS-203 for 6 times, kneading for 15min each time, and after agglomeration; continuing kneading and heating to 130 ℃ for vacuum heat treatment, wherein the kneading temperature in the kneader is 160 ℃, the time is 1h, and the vacuum degree is-0.08 Mpa; obtaining the base rubber A and cooling.
And adding 40 parts of second silicon rubber 110-0 into a second kneader, kneading for 10min, adding 15 parts of boric acid and 2 parts of magnesium oxide 3 times, kneading for 10min each time, and obtaining the base rubber B after agglomeration.
And (3) fully and uniformly mixing the base rubber A and the base rubber B in a kneader to obtain the fireproof and fire-resistant silicon rubber material required by the patent. 1.5 parts of vulcanizing agent bis 24 is added into the fireproof and fire-resistant silicon rubber material on an open mill, and the mixture is uniformly mixed to prepare the fireproof and fire-resistant silicon rubber product.
Example 8
Adding 60 parts of first silicon rubber 110-0 into a first kneader, kneading for 10min, adding 25 parts of white carbon black SJ-34, 40 parts of aluminum hydroxide, 15 parts of wollastonite 1250, 1.6 parts of coupling agent A171 and 8 parts of hydroxy silicone oil QLS-203 for 6 times, kneading for 15min each time, and after agglomeration; continuing kneading and heating to 130 ℃ for vacuum heat treatment, wherein the kneading temperature in the kneader is 160 ℃, the time is 1h, and the vacuum degree is-0.08 Mpa; obtaining the base rubber A and cooling.
And adding 40 parts of second silicon rubber 110-0 into a second kneader, kneading for 10min, adding 25 parts of boric acid and 2 parts of magnesium oxide 3 times, kneading for 10min each time, and obtaining the base rubber B after agglomeration.
And (3) fully and uniformly mixing the base rubber A and the base rubber B in a kneader to obtain the fireproof and fire-resistant silicon rubber material required by the patent. 1.5 parts of vulcanizing agent bis 24 is added into the fireproof and fire-resistant silicon rubber material on an open mill, and the mixture is uniformly mixed to prepare the fireproof and fire-resistant silicon rubber product.
Example 9
Adding 60 parts of first silicon rubber 110-0 into a first kneader, kneading for 10min, then adding 10 parts of white carbon black SJ-34, 60 parts of aluminum hydroxide, 10 parts of wollastonite 1250, 1.6 parts of coupling agent A171 and 8 parts of hydroxy silicone oil QLS-203 for 6 times, kneading for 15min each time, and after agglomeration; continuing kneading and heating to 130 ℃ for vacuum heat treatment, wherein the kneading temperature in the kneader is 160 ℃, the time is 1h, and the vacuum degree is-0.08 Mpa; obtaining the base rubber A and cooling.
And adding 40 parts of second silicon rubber 110-0 into a second kneader, kneading for 10min, adding 20 parts of boric acid and 3 parts of magnesium oxide for 3 times, kneading for 10min each time, and obtaining the base rubber B after agglomeration.
And (3) fully and uniformly mixing the base rubber A and the base rubber B in a kneader to obtain the fireproof and fire-resistant silicon rubber material required by the patent. 1.5 parts of vulcanizing agent bis 24 is added into the fireproof and fire-resistant silicon rubber material on an open mill, and the mixture is uniformly mixed to prepare the fireproof and fire-resistant silicon rubber product.
Example 10
Adding 60 parts of first silicon rubber 110-0 into a first kneader, kneading for 10min, adding 20 parts of white carbon black SJ-34, 60 parts of aluminum hydroxide, 20 parts of wollastonite 1250, 2 parts of coupling agent A171 and 10 parts of hydroxy silicone oil QLS-203 for 6 times, kneading for 15min each time, and after agglomeration; continuing kneading and heating to 130 ℃ for vacuum heat treatment, wherein the kneading temperature in the kneader is 170 ℃, the time is 1h, and the vacuum degree is-0.08 Mpa; obtaining the base rubber A and cooling.
And adding 40 parts of second silicon rubber 110-0 into a second kneader, kneading for 10min, adding 20 parts of boric acid and 3 parts of magnesium oxide for 3 times, kneading for 10min each time, and obtaining the base rubber B after agglomeration.
And (3) fully and uniformly mixing the base rubber A and the base rubber B in a kneader to obtain the fireproof and fire-resistant silicon rubber material required by the patent. 1.5 parts of vulcanizing agent bis 24 is added into the fireproof and fire-resistant silicon rubber material on an open mill, and the mixture is uniformly mixed to prepare the fireproof and fire-resistant silicon rubber product.
Comparative example 1
Preparation of a fire-resistant and fire-resistant silicone rubber material was provided following the procedure in example 1, but no boric acid was added in the procedure.
Comparative example 2
The procedure of example 1 was followed to provide a preparation of a fire-resistant and fire-resistant silicone rubber material, but no aluminum hydroxide was added in the procedure.
Comparative example 3
Preparation of a fire-resistant and fire-resistant silicone rubber material was provided according to the procedure in example 1, but without adding white carbon black in the procedure.
Comparative example 4
The procedure of example 1 was followed to provide a preparation of a fire-resistant and fire-resistant silicone rubber material, but in this procedure no wollastonite was added.
The data of the performance test are given by combining examples 1 to 10 and comparative examples 1 to 4. See table 1 for details.
TABLE 1
Figure BDA0002842760650000121
Figure BDA0002842760650000131
Remarking:
hardness: reference is made to the standard GB/T531.
Tensile strength: reference standard GB/T528
Elongation at break: reference standard GB/T528
3mm flame retardant: strips 12.5mm wide and 3mm thick were taken and, using an alcohol burner, after a 10 second flame was applied, the flame was removed and the time for the sample to self-extinguish was recorded.
And (3) porcelain forming strength: and taking a silicon rubber sample strip with the thickness of 3mm, the length of 50mm and the width of 8mm, sintering the silicon rubber sample strip in a muffle furnace at 750 ℃ for 4 hours, taking out the silicon rubber sample strip, testing and calculating the strength.
In conclusion, the present invention effectively overcomes various disadvantages of the prior art and has high industrial utilization value.
While the invention has been described with respect to a preferred embodiment, it will be understood by those skilled in the art that the foregoing and other changes, omissions and deviations in the form and detail thereof may be made without departing from the scope of this invention. Those skilled in the art can make various changes, modifications and equivalent arrangements, which are equivalent to the embodiments of the present invention, without departing from the spirit and scope of the present invention, and which may be made by utilizing the techniques disclosed above; meanwhile, any changes, modifications and variations of the above-described embodiments, which are equivalent to those of the technical spirit of the present invention, are within the scope of the technical solution of the present invention.

Claims (10)

1. A fireproof and fire-resistant silicon rubber material comprises a component A and a component B;
the component A comprises the following raw materials in parts by weight:
Figure FDA0002842760640000011
the component B comprises the following raw materials in parts by weight:
30-50 parts of second silicon rubber;
1-5 parts of magnesium oxide;
10-30 parts of boric acid.
2. The fireproof and fire-resistant silicone rubber material of claim 1, wherein the component A comprises the following raw materials in parts by weight:
Figure FDA0002842760640000012
the component B comprises the following raw materials in parts by weight:
40-50 parts of second silicon rubber;
1-5 parts of magnesium oxide;
20-30 parts of boric acid.
3. A fire and fire resistant silicone rubber material as in claim 1 or 2, wherein said first and second silicone rubbers are selected from the group consisting of methyl vinyl silicone rubber and/or methyl silicone rubber; the first and second silicone rubbers may be the same or different.
4. The fireproof and fire-resistant silicone rubber material according to claim 3, wherein the methyl vinyl silicone rubber has a molecular weight of 50 to 80 ten thousand; the content of vinyl in the methyl vinyl silicone rubber is 0.05-0.3%.
5. The fireproof and fire-resistant silicone rubber material of claim 3, wherein the methyl silicone rubber has a molecular weight of 50 to 80 ten thousand.
6. The fireproof and fire-resistant silicone rubber material according to claim 1 or 2, wherein the white carbon black has a specific surface area of 10m2/g～180m2/g；
And/or the wollastonite is of a needle-shaped structure, the length-diameter ratio is 8: 1-20: 1, and the high-temperature ignition loss is less than 3%;
and/or the silicone oil is one or a mixture of hydroxyl silicone oil and methoxyl silicone oil; the viscosity is 10-50 mm2/s；
And/or the magnesium oxide is active magnesium oxide with the specific surface area of 10-80 m2/g。
7. A method for preparing a fire-resistant and fire-resistant silicone rubber material as claimed in any one of claims 1 to 6, said method comprising: mixing first silicon rubber, white carbon black, aluminum hydroxide, wollastonite, silicon oil and a silane coupling agent to obtain a component A; mixing the second silicon rubber, magnesium oxide and boric acid to obtain a component B; and mixing the component A and the component B to prepare the fireproof and fire-resistant silicon rubber material.
8. A fireproof and fire-resistant silicone rubber product, the raw materials of which comprise the fireproof and fire-resistant silicone rubber material as claimed in any one of claims 1 to 6 and a vulcanizing agent.
9. The flame-resistant, fire-resistant silicone rubber article of claim 8, wherein the vulcanizing agent is a peroxide vulcanizing agent.
10. Use of the fire-resistant and fire-resistant silicone rubber material according to any one of claims 1 to 6 or the fire-resistant and fire-resistant silicone rubber product according to any one of claims 8 to 9 in a cable.
CN202011498028.4A 2020-12-17 2020-12-17 Fireproof and fireproof silicon rubber material and preparation method thereof Pending CN112625447A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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CN105368054A (en) * 2015-12-07 2016-03-02 无锡市华美电缆有限公司 Silicone rubber for electric wires and cables
CN105694471A (en) * 2016-04-17 2016-06-22 北京化工大学 Preparation method of ceramizing fire-resistant silicon rubber
CN112029289A (en) * 2020-07-28 2020-12-04 东莞市朗晟材料科技有限公司 Ceramic fire-resistant flame-retardant silicone rubber and preparation method and use method thereof

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Publication number Priority date Publication date Assignee Title
CN105017776A (en) * 2015-07-08 2015-11-04 上海大学 Halogen-free flame-retardant high-strength ceramizable silicone rubber
CN105368054A (en) * 2015-12-07 2016-03-02 无锡市华美电缆有限公司 Silicone rubber for electric wires and cables
CN105694471A (en) * 2016-04-17 2016-06-22 北京化工大学 Preparation method of ceramizing fire-resistant silicon rubber
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* Cited by examiner, † Cited by third party
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Application publication date: 20210409