CN115466517A - Flame-retardant ceramic silicon rubber and preparation method thereof - Google Patents
Flame-retardant ceramic silicon rubber and preparation method thereof Download PDFInfo
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- CN115466517A CN115466517A CN202211144177.XA CN202211144177A CN115466517A CN 115466517 A CN115466517 A CN 115466517A CN 202211144177 A CN202211144177 A CN 202211144177A CN 115466517 A CN115466517 A CN 115466517A
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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
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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
- C08K2003/2296—Oxides; Hydroxides of metals of zinc
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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
- C08K3/38—Boron-containing compounds
- C08K2003/387—Borates
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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 belongs to the field of silicone rubber preparation, and discloses flame-retardant ceramic silicone rubber and a preparation method thereof. The silicone rubber comprises the following components: 90-105 parts of methyl vinyl silicone rubber, 30-50 parts of white carbon black, 5-15 parts of hydroxyl silicone oil, 0.1-5 parts of silane coupling agent, 1-50 parts of ceramic filler, 1-50 parts of zinc borate, 1-50 parts of zinc oxide, 0-50 parts of talcum powder, 0.000001-1 part of platinum complex by mass and 0.1-0.5 part of internal mold release agent. The flame-retardant ceramic silicon rubber has the advantages of high ceramic layer strength, stable structure and excellent flame-retardant property after flame ablation.
Description
Technical Field
The invention belongs to the field of silicone rubber preparation, and particularly relates to flame-retardant ceramic silicone rubber and a preparation method thereof.
Background
In recent years, people have increasingly stronger awareness of fire hazard, and particularly in electric wires and cables, once a fire hazard occurs, immeasurable loss is caused to lives and properties of people, so that higher requirements are put on the flame retardant property of the electric wires and cables. At present, mica tape wound fire-resistant cables and magnesium oxide mineral fireproof cables are mostly adopted at home and abroad, but the mica tape wound cables are complex in process and easy to fall off after burning in case of fire, and the magnesium oxide mineral fireproof cables are expensive in manufacturing cost and difficult to popularize. The ceramic silicon rubber is produced by the method.
The ceramic silicon rubber can form a ceramic layer with certain strength after flame ablation, is halogen-free, low-smoke, low-toxicity, environment-friendly and low in cost, and can be well applied to fire-resistant cables, but the existing ceramic silicon rubbers in the market all have the defects of low strength of the ceramic layer after ablation and poor flame retardant property (not reaching UL 94V-0 level), so that the application is limited to a certain extent.
Disclosure of Invention
The invention aims to provide a flame-retardant ceramic silicon rubber and a preparation method thereof aiming at the defects of the prior art. The flame-retardant ceramic silicon rubber has the advantages of high ceramic layer strength, stable structure and excellent flame-retardant property after flame ablation.
In order to achieve the above object, an aspect of the present invention provides a flame retardant ceramicized silicone rubber comprising the following components: 90-105 parts of methyl vinyl silicone rubber, 30-50 parts of white carbon black, 5-15 parts of hydroxyl silicone oil, 0.1-5 parts of silane coupling agent, 1-50 parts of ceramic filler, 1-50 parts of zinc borate, 1-50 parts of zinc oxide, 0-50 parts of talcum powder, 0.000001-1 part of platinum complex by mass and 0.1-0.5 part of internal mold release agent by mass.
According to the present invention, preferably, the silicone rubber comprises the following components: 100 parts of methyl vinyl silicone rubber, 35-45 parts of white carbon black, 5-10 parts of hydroxyl silicone oil, 3-4 parts of silane coupling agent, 10-30 parts of ceramic filler, 3-25 parts of zinc borate, 3-25 parts of zinc oxide, 3-25 parts of talcum powder, 0.000001-0.01 part of platinum complex by mass and 0.1-0.5 part of internal mold release agent by mass.
According to the present invention, preferably, the methyl vinyl silicone rubber has a vinyl content of 0.01 to 0.3% and a molecular weight of 40 to 80 ten thousand.
According to the present invention, preferably, the white carbon black is fumed white carbon black and/or precipitated white carbon black.
According to the present invention, preferably, the silane coupling agent is selected from at least one of aminopropyltriethoxysilane, glycidoxypropyltrimethoxysilane, and vinyltrimethoxysilane.
According to the present invention, preferably, the ceramized filler is at least one of mica powder, kaolin and wollastonite.
According to the present invention, preferably, the platinum complex is a complex of platinum and divinyltetramethylsiloxane.
According to the present invention, preferably, the internal mold release agent is at least one of stearic acid, zinc stearate, and calcium stearate.
The invention also provides a preparation method of the flame-retardant ceramic silicon rubber, which comprises the following steps:
(1) Kneading the methyl vinyl silicone rubber, the white carbon black, the hydroxyl silicone oil, the silane coupling agent and the internal mold release agent to obtain a basic rubber material, and standing;
(2) And kneading the base rubber after standing with the ceramic filler, zinc borate, zinc oxide, talcum powder and platinum complex to obtain rubber, remilling and filtering to obtain the flame-retardant ceramic silicone rubber.
According to the present invention, it is preferred that in step (1), the kneading temperature is 150 to 180 ℃ and the kneading time is 1 to 3 hours.
According to the invention, the temperature of the standing is preferably 25-35 ℃ and the time is 12-48 h.
According to the present invention, it is preferred that in the step (2), the kneading temperature is 150 to 180 ℃ for 0.5 to 2 hours and the degree of vacuum is-0.05 to-0.08 MPa.
According to the invention, preferably, the filtering is to filter the sizing material by a 300-350 mesh filter screen.
In the invention, the silane coupling agent is added in the step (1) to react with the white carbon black to form chemical bond energy combination, so that the physical property of the sizing material is greatly improved; the experimental result shows that the hydroxyl on the surface of the fumed silica can be better treated after the base rubber is placed for 12-48 h and is subjected to standing treatment, so that the fumed silica and the raw rubber are more uniformly mixed, and the tearing performance, the deformation resistance and other physical properties of the rubber compound are improved; the zinc borate, the zinc oxide and the talcum powder added in the step (2) can reduce the melting temperature of the ceramic silicon rubber, so that a ceramic layer is formed at a lower temperature, the ceramic layer is more compact, and the fire resistance is improved.
The technical scheme of the invention has the following beneficial effects:
the flame retardant grade of the silicone rubber material reaches UL 94V-0 grade, the characteristics of the rubber are maintained at normal temperature, the silicone rubber material can be vitrified at high temperature to form a hard ceramic layer, and the ceramic layer has certain strength, can bear certain impact force and can ensure that a product can continuously and normally work in a fire disaster.
Additional features and advantages of the invention will be set forth in the detailed description which follows.
Detailed Description
Preferred embodiments of the present invention will be described in more detail below. While the following describes preferred embodiments of the present invention, it should be understood that the present invention may be embodied in various forms and should not be limited by the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the scope of the invention to those skilled in the art.
The methyl vinyl silicone rubber used in the following examples was 110-2S manufactured by Taoju Silicone Co., ltd, and the hydroxy silicone oil was JS-209 manufactured by Liyang Ju Shen science materials Co., ltd.
Example 1
The embodiment provides a flame-retardant ceramic silicone rubber, which comprises the following components:
100 parts of methyl vinyl silicone rubber;
35 parts of precipitated white carbon black;
5 parts of hydroxyl silicone oil;
4 parts of vinyl trimethoxy silane;
20 parts of kaolin;
4 parts of zinc borate;
8 parts of zinc oxide;
0.00001 part by mass of a platinum complex based on the mass of platinum;
0.2 part of zinc stearate.
The preparation method of the flame-retardant ceramic silicon rubber comprises the following steps:
(1) Adding the methyl vinyl silicone rubber, the precipitated white carbon black, the hydroxyl silicone oil, the vinyl trimethoxy silane and the zinc stearate into a kneader, kneading for 2 hours at 160 ℃, and then discharging to obtain a basic rubber material; standing at 25 deg.C for 24h;
(2) Kneading the base rubber material after standing, kaolin, zinc borate, zinc oxide and platinum complex into a large mass in a kneading machine to obtain rubber material, heating to 160 ℃, vacuumizing for 1h, wherein the vacuum degree is-0.05 to-0.08 MPa, then using an open rubber mixing mill to remix the mixed rubber material, and filtering the obtained rubber material by a 300-mesh filter screen to obtain the flame-retardant ceramic silicon rubber.
Example 2
The embodiment provides a flame-retardant ceramic silicone rubber, which comprises the following components:
100 parts of methyl vinyl silicone rubber;
35 parts of fumed silica;
10 parts of hydroxyl silicone oil;
4 parts of aminopropyltriethoxysilane;
25 parts of kaolin;
4 parts of zinc borate;
8 parts of zinc oxide;
0.00001 part by mass of a platinum complex based on the mass of platinum;
0.2 part of zinc stearate.
The preparation method of the flame-retardant ceramic silicon rubber comprises the following steps:
(1) Adding the methyl vinyl silicone rubber, the fumed silica, the hydroxyl silicone oil, the aminopropyl triethoxysilane and the zinc stearate into a kneader, kneading for 2 hours at 160 ℃, and then discharging to obtain a basic rubber material; standing at 25 deg.C for 24h;
(2) Kneading the base rubber material after standing, kaolin, zinc borate, zinc oxide and a platinum complex into a large mass in a kneading machine to obtain a rubber material, heating to 180 ℃, vacuumizing for 1h with the vacuum degree of-0.05 to-0.08 MPa, then remilling the mixed rubber material by using an open rubber mixing mill, and filtering the obtained rubber material by using a 300-mesh filter screen to obtain the flame-retardant ceramic silicon rubber.
Example 3
The embodiment provides a flame-retardant ceramic silicone rubber, which comprises the following components:
100 parts of methyl vinyl silicone rubber;
35 parts of fumed silica;
10 parts of hydroxyl silicone oil;
4 parts of glycidyl ether oxypropyltrimethoxysilane;
24 parts of wollastonite;
3 parts of zinc borate;
10 parts of zinc oxide;
0.00001 part by mass of a platinum complex based on the mass of platinum;
0.2 part of calcium stearate.
The preparation method of the flame-retardant ceramic silicon rubber comprises the following steps:
(1) Adding the methyl vinyl silicone rubber, the fumed silica, the hydroxyl silicone oil, the aminopropyl triethoxysilane and the zinc stearate into a kneader, kneading for 2 hours at 160 ℃, and then discharging to obtain a basic rubber material; standing at 25 ℃ for 18h;
(2) Kneading the base rubber material after standing, kaolin, zinc borate, zinc oxide and platinum complex into a large mass in a kneading machine to obtain rubber material, heating to 180 ℃, vacuumizing for 1h, wherein the vacuum degree is-0.05 to-0.08 MPa, then using an open rubber mixing mill to remix the mixed rubber material, and filtering the obtained rubber material by a 300-mesh filter screen to obtain the flame-retardant ceramic silicon rubber.
Example 4
The embodiment provides a flame-retardant ceramic silicone rubber, which comprises the following components:
100 parts of methyl vinyl silicone rubber;
35 parts of fumed silica;
10 parts of hydroxyl silicone oil;
4 parts of vinyl trimethoxy silane;
12 parts of wollastonite;
8 parts of zinc borate;
4 parts of zinc oxide;
12 parts of talcum powder;
0.00001 part by mass of a platinum complex based on the mass of platinum;
0.2 part of zinc stearate.
The preparation method of the flame-retardant ceramic silicon rubber comprises the following steps:
(1) Adding the methyl vinyl silicone rubber, the fumed silica, the hydroxyl silicone oil, the aminopropyl triethoxysilane and the zinc stearate into a kneader, kneading for 2 hours at 160 ℃, and then discharging to obtain a basic rubber material; standing at 25 deg.C for 24h;
(2) Kneading the base rubber material after standing, kaolin, zinc borate, zinc oxide and a platinum complex into a large mass in a kneading machine to obtain a rubber material, heating to 180 ℃, vacuumizing for 1h with the vacuum degree of-0.05 to-0.08 MPa, then remilling the mixed rubber material by using an open rubber mixing mill, and filtering the obtained rubber material by using a 300-mesh filter screen to obtain the flame-retardant ceramic silicon rubber.
Test example
The ceramic silicone rubbers obtained in examples 1 to 4 were compared with domestic ceramic silicone rubbers (Liyang sky insulation Co., ltd.) in performance tests, and the test data are shown in Table 1 below:
TABLE 1
From the test data in the table above, it can be seen that: compared with domestic ceramic silicone rubber, the ceramic silicone rubber prepared by the embodiment of the invention has better flame retardant property and better ceramic effect.
Having described embodiments of the present invention, the foregoing description is intended to be exemplary, not exhaustive, and not limited to the embodiments disclosed. Many modifications and variations will be apparent to those of ordinary skill in the art without departing from the scope and spirit of the described embodiments.
Claims (10)
1. The flame-retardant ceramic silicone rubber is characterized by comprising the following components: 90-105 parts of methyl vinyl silicone rubber, 30-50 parts of white carbon black, 5-15 parts of hydroxyl silicone oil, 0.1-5 parts of silane coupling agent, 1-50 parts of ceramic filler, 1-50 parts of zinc borate, 1-50 parts of zinc oxide, 0-50 parts of talcum powder, 0.000001-1 part of platinum complex by mass and 0.1-0.5 part of internal mold release agent.
2. The flame retardant ceramic silicone rubber according to claim 1, wherein the silicone rubber comprises the following components: 100 parts of methyl vinyl silicone rubber, 35-45 parts of white carbon black, 5-10 parts of hydroxyl silicone oil, 3-4 parts of silane coupling agent, 10-30 parts of ceramic filler, 3-25 parts of zinc borate, 3-25 parts of zinc oxide, 3-25 parts of talcum powder, 0.000001-0.01 part of platinum complex by mass and 0.1-0.5 part of internal mold release agent by mass.
3. The flame-retardant ceramified silicone rubber according to claim 1 or 2, wherein the methyl vinyl silicone rubber has a vinyl content of 0.01 to 0.3% and a molecular weight of 40 to 80 ten thousand.
4. The flame-retardant ceramified silicone rubber according to claim 1 or 2, wherein the white carbon black is fumed silica and/or precipitated silica.
5. The flame-retardant ceramified silicone rubber according to claim 1 or 2, wherein the silane coupling agent is selected from at least one of aminopropyltriethoxysilane, glycidoxypropyltrimethoxysilane and vinyltrimethoxysilane.
6. The flame retardant ceramified silicone rubber according to claim 1 or 2, wherein the ceramified filler is at least one of mica powder, kaolin and wollastonite.
7. The flame-retardant ceramified silicone rubber according to claim 1 or 2, wherein the platinum complex is a complex of platinum and divinyltetramethylsiloxane.
8. The flame-retardant ceramified silicone rubber according to claim 1 or 2, wherein the internal mold release agent is at least one of stearic acid, zinc stearate, and calcium stearate.
9. The method for preparing a flame-retardant ceramic silicone rubber according to any one of claims 1 to 8, characterized in that it comprises the following steps:
(1) Kneading the methyl vinyl silicone rubber, the white carbon black, the hydroxyl silicone oil, the silane coupling agent and the internal mold release agent to obtain a basic rubber material, and standing;
(2) And kneading the base rubber after standing with the ceramic filler, zinc borate, zinc oxide, platinum complex and optional talc powder to obtain rubber, and performing remilling and filtering to obtain the flame-retardant ceramic silicon rubber.
10. The method for producing a flame-retardant ceramified silicone rubber according to claim 9,
in the step (1), the kneading temperature is 150-180 ℃ and the kneading time is 1-3 h;
the standing temperature is 25-35 ℃, and the standing time is 12-48 h;
in the step (2), the kneading temperature is 150-180 ℃, the kneading time is 0.5-2 h, and the vacuum degree is-0.05-0.08 MPa;
the filtering is to filter the rubber material by a filter screen of 300-350 meshes.
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| CN202211144177.XA CN115466517A (en) | 2022-09-20 | 2022-09-20 | Flame-retardant ceramic silicon rubber and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115819981A (en) * | 2022-12-14 | 2023-03-21 | 安徽东爵有机硅有限公司 | High-strength low-smoke flame-retardant silicone rubber compound and preparation method thereof |
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2022
- 2022-09-20 CN CN202211144177.XA patent/CN115466517A/en not_active Withdrawn
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115819981A (en) * | 2022-12-14 | 2023-03-21 | 安徽东爵有机硅有限公司 | High-strength low-smoke flame-retardant silicone rubber compound and preparation method thereof |
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Application publication date: 20221213 |
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