CN109401328A - The preparation method of novel fire resistant flame-proof silicon rubber - Google Patents
The preparation method of novel fire resistant flame-proof silicon rubber Download PDFInfo
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- CN109401328A CN109401328A CN201811451919.7A CN201811451919A CN109401328A CN 109401328 A CN109401328 A CN 109401328A CN 201811451919 A CN201811451919 A CN 201811451919A CN 109401328 A CN109401328 A CN 109401328A
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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
- C08K2003/2217—Oxides; Hydroxides of metals of magnesium
- C08K2003/2224—Magnesium hydroxide
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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
- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
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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
- C08K2201/00—Specific properties of additives
- C08K2201/014—Additives containing two or more different additives of the same subgroup in C08K
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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
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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
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The present invention discloses a kind of preparation method of novel fire resistant flame-proof silicon rubber, the following steps are included: Step 1: filler, 3wt% zinc oxide, 2wt% antioxidant, 1wt% crosslinking accelerator and the 20wt% fire retardant that 35wt% is added thereto are mixed to form mixture by small-sized internal mixer using methyl vinyl silicone rubber as substrate；Vulcanize 20 minutes Step 2: being put into 175 DEG C of vulcanizing presses after the mixture of step 1 is sufficiently mixed；The fire retardant is mixed by aluminium hydroxide, magnesium hydroxide and melamine cyanurate, and the inorganic filler is the mixture of precipitated silica, superfine silicon dioxide.The novel fire resistant flame-proof silicon rubber that preparation method of the present invention obtains not only ensure that it will not occur in certain time significantly to soften under the high temperature conditions or brittle failure, and mechanical properties decrease is unobvious, is provided simultaneously with outstanding flame retardant property.
Description
Technical field
The present invention relates to technical field of rubber material more particularly to a kind of preparation sides of long-term High-temperature-resandant andant flame-retardant silicone rubber
Method.
Background technique
Raw rubber type mainly has methyl silicone rubber, methyl vinyl silicone rubber, methyl phenyl vinyl silicone rubber and fluorine silicon
Rubber.Further, it is also possible to introduce phenylene group on main chain.Maximum dosage is methyl ethylene silicon raw rubber.Since crosslinking is used
Active group vinyl introducing, greatly improve the cross-linking efficiency of silicon raw rubber peroxide crosslinking.It is almost all of
Commodity silicon rubber all contains a certain amount of vinyl.
High-temperature silicon disulfide rubber, which refers to the process of that polysiloxanes becomes elastomer, to be sulfided by high temperature (110-170 DEG C)
Type.It is mixed into reinforced filling, vulcanizing agent etc. mainly using the Polymethyl methacrylate of high molecular weight as raw rubber, is heating
Pressurization is lower to vulcanize elastomer-forming.The reinforcement of silicon rubber is mainly various types of white carbon blacks, and the intensity of vulcanizate can be made to increase number
Ten times.Sometimes for reducing cost or improving properties of rubber and the imparting various special performances of vulcanizate, also it is added corresponding each
Kind additive.Vulcanizing agent is various organic peroxides or addition reaction catalyst.
Methyl vinyl silicone rubber abbreviation vinylsiloxane rubber.Such rubber due to contain a small amount of vinyl sidechain, therefore
Vulcanization easier than methyl silicone rubber has been allowed to a greater variety of peroxide and has used for vulcanization, and can greatly reduce peroxidating
The dosage of object.It is compared using the silicon rubber containing a small amount of vinyl with dimethyl silicone rubber, incompressible permanent deformation performance can be made to obtain
It must be markedly improved, low compressive deformation reflects it has preferable supportive as sealing element at high temperature, this is O-ring
With the institute such as washer is prerequisite one of requires.Methyl vinyl silicone rubber processing performance is preferable, easy to operate, can be made into thick system
Product and extrusion, calendering surface of semi-finished are smooth, are a kind of more common silicon rubber.
Summary of the invention
It is obtained the object of the present invention is to provide a kind of preparation method of novel fire resistant flame-proof silicon rubber, the preparation method
Novel fire resistant flame-proof silicon rubber not only ensure that it will not occur in certain time significantly to soften under the high temperature conditions or crisp
Disconnected, mechanical properties decrease is unobvious, is provided simultaneously with outstanding flame retardant property.
To achieve the above object of the invention, the technical solution adopted by the present invention is that: a kind of novel fire resistant flame-proof silicon rubber
Preparation method, comprising the following steps:
Step 1: filler, 3wt% zinc oxide, the 2wt% antioxygen of 35wt% are added thereto using methyl vinyl silicone rubber as substrate
Agent, 1wt% crosslinking accelerator and 20wt% fire retardant are mixed to form mixture by small-sized internal mixer；
Vulcanize 20 minutes Step 2: being put into 175 DEG C of vulcanizing presses after the mixture of step 1 is sufficiently mixed；
The fire retardant is mixed by aluminium hydroxide, magnesium hydroxide and melamine cyanurate；The inorganic filler
For the mixture of precipitated silica, the mixture of superfine silicon dioxide or Nano carbon white, superfine silicon dioxide.
The further improved technical solution of above-mentioned technical proposal is as follows:
1. in above scheme, the antioxidant is antioxidant 1010, in irgasfos 168, antioxidant 1076, anti-oxidant DLTP
At least one.
2. in above scheme, the crosslinking accelerator is cumyl peroxide (DCP), benzoyl peroxide (BPO) or
At least one of -2,5 di-t-butyl hexane peroxide kind of 2,5- dimethyl.
Due to the application of the above technical scheme, compared with the prior art, the invention has the following advantages:
The preparation method of novel fire resistant flame-proof silicon rubber of the present invention, under the collective effect of self-control fire retardant and zinc oxide,
The flame retardant property of silicon rubber is improved；By the collective effect of crosslinking accelerator and antioxidant, may be implemented efficient
Crosslinking and high-temperature resistant result；And the inorganic filler based on use silica can effectively increase the mechanical property of silicon rubber,
By above-mentioned technical controlling, the high temperature resistance and flame retardant effect of silicon rubber can be substantially improved.
Specific embodiment
The present invention will be further described below with reference to examples:
A kind of embodiment: preparation method of novel fire resistant flame-proof silicon rubber, comprising the following steps:
Step 1: filler, 3wt% zinc oxide, the 2wt% antioxygen of 35wt% are added thereto using methyl vinyl silicone rubber as substrate
Agent, 1wt% crosslinking accelerator and 20wt% fire retardant are mixed to form mixture by small-sized internal mixer；
Vulcanize 5 minutes Step 2: being put into 180 DEG C of vulcanizing presses after the mixture of step 1 is sufficiently mixed.
Above-mentioned fire retardant is matched by a certain percentage by aluminium hydroxide, magnesium hydroxide and melamine cyanurate [MCA]
It makes.
Above-mentioned antioxidant of stating is at least one in antioxidant 1010, irgasfos 168, antioxidant 1076, anti-oxidant DLTP
Kind.
Above-mentioned inorganic filler is at least one of precipitated silica, Nano carbon white, superfine silicon dioxide.
Above-mentioned crosslinking accelerator is cumyl peroxide (DCP), benzoyl peroxide (BPO) or 2,5- dimethyl -2,5
At least one of di-t-butyl hexane peroxide.
A kind of embodiment 1: preparation method of novel fire resistant flame-proof silicon rubber, comprising the following steps:
Step 1: filler, 3wt% zinc oxide, the 2wt% antioxygen of 35wt% are added thereto using methyl vinyl silicone rubber as substrate
[double 25] and 20wt% fire retardant [MCA, aluminium hydroxide] pass through for agent [irgasfos 168,1010 and DLTP], 1wt% crosslinking accelerator
Small-sized internal mixer is mixed to form mixture；
Vulcanize 20 minutes Step 2: being put into 175 DEG C of vulcanizing presses after the mixture of step 1 is mixed.
Above-mentioned fire retardant is mixed by melamine cyanurate, aluminium hydroxide according to 3:1 parts by weight；
Above-mentioned filler is mixed by Nano carbon white, superfine silicon dioxide according to 1:1 parts by weight.
According to GB/T2951.11-2008 and GB/T2406.2-2009, the 250 DEG C of * 7d agings of vulcanization crosslinking silicon rubber are measured
The physical property and oxygen index (OI) of front and back, the result is shown in tables 1.
Physical property and oxygen index (OI) comparison before and after 1 vulcanization crosslinking of table:
| Tensile strength [Mpa] | Elongation rate of tensile failure [%] | Tensile strength [250 DEG C of * 60d] [Mpa] | Elongation rate of tensile failure [250 DEG C of * 60d] [%] | Oxygen index (OI) | |
| After vulcanization | 5.2 | 210 | 4.7 | 150 | 31 |
As shown in Table 1, the physical property fall after vulcanization after 250 DEG C of * 60d of silicon rubber is smaller, this illustrates that the rubber has
Good high temperature resistance, oxygen index (OI) reach 31 > 27, belong to nonflammable material, have good flame retardant property.
A kind of embodiment 2: preparation method of novel fire resistant flame-proof silicon rubber, comprising the following steps:
Step 1: filler, 3wt% zinc oxide, the 2wt% antioxygen of 35wt% are added thereto using methyl vinyl silicone rubber as substrate
[double 25] and 20wt% fire retardant are mixed to form mixture by small-sized internal mixer for agent [antioxidant 1010], 1wt% crosslinking accelerator；
Vulcanize 5 minutes Step 2: being put into 180 DEG C of vulcanizing presses after the mixture of step 1 is sufficiently mixed.
Above-mentioned fire retardant is mixed by melamine cyanurate, magnesium hydroxide according to 3:1 parts by weight；
Above-mentioned filler is mixed by precipitated silica, superfine silicon dioxide according to 1:1 parts by weight.
According to GB/T2951.11-2008 and GB/T2406.2-2009, the 250 DEG C of * 7d agings of vulcanization crosslinking silicon rubber are measured
The physical property and oxygen index (OI) of front and back, the result is shown in tables 2.
Physical property and oxygen index (OI) comparison before and after 2 vulcanization crosslinking of table:
| Tensile strength [Mpa] | Elongation rate of tensile failure [%] | Tensile strength [250 DEG C of * 7d] [Mpa] | Elongation rate of tensile failure [250 DEG C of * 7d] [%] | Oxygen index (OI) | |
| After vulcanization | 6 | 230 | 4.9 | 130 | 28 |
As shown in Table 2, change filler and fire retardant model, type, can slightly promote tensile strength, and oxygen index (OI) is dropped
It is low, but 27 are still greater than, belong to nonflammable material.
The above embodiments merely illustrate the technical concept and features of the present invention, and its object is to allow person skilled in the art
Scholar cans understand the content of the present invention and implement it accordingly, and it is not intended to limit the scope of the present invention.It is all according to the present invention
Equivalent change or modification made by Spirit Essence, should be covered by the protection scope of the present invention.
Claims (3)
1. a kind of preparation method of novel fire resistant flame-proof silicon rubber, it is characterised in that: the following steps are included:
Step 1: filler, 3wt% zinc oxide, the 2wt% antioxygen of 35wt% are added thereto using methyl vinyl silicone rubber as substrate
Agent, 1wt% crosslinking accelerator and 20wt% fire retardant are mixed to form mixture by small-sized internal mixer；
Vulcanize 20 minutes Step 2: being put into 175 DEG C of vulcanizing presses after the mixture of step 1 is sufficiently mixed；
The fire retardant is mixed by aluminium hydroxide, magnesium hydroxide and melamine cyanurate；The inorganic filler
For the mixture of precipitated silica, the mixture of superfine silicon dioxide or Nano carbon white, superfine silicon dioxide.
2. the preparation method of novel fire resistant flame-proof silicon rubber according to claim 1, it is characterised in that: described anti-oxidant
Agent is at least one of antioxidant 1010, irgasfos 168, antioxidant 1076, anti-oxidant DLTP.
3. the preparation method of novel fire resistant flame-proof silicon rubber according to claim 1, it is characterised in that: the crosslinking
Promotor is cumyl peroxide (DCP), -2,5 di-tert-butyl peroxide of benzoyl peroxide (BPO) or 2,5- dimethyl
At least one of hexane kind.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201811451919.7A CN109401328A (en) | 2018-11-30 | 2018-11-30 | The preparation method of novel fire resistant flame-proof silicon rubber |
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| CN201811451919.7A CN109401328A (en) | 2018-11-30 | 2018-11-30 | The preparation method of novel fire resistant flame-proof silicon rubber |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113072811A (en) * | 2021-03-30 | 2021-07-06 | 陕西省石油化工研究设计院 | Xenon lamp ultraviolet aging resistant flame-retardant silicone rubber material and preparation method thereof |
| CN113717534A (en) * | 2021-09-14 | 2021-11-30 | 深圳市浩宇泰科技有限公司 | Heat conduction material and preparation process |
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| EP1574523A1 (en) * | 2004-03-09 | 2005-09-14 | Tokai Rubber Industries, Ltd. | Rubber product and method for manufacturing the same |
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|---|---|---|---|---|
| EP1574523A1 (en) * | 2004-03-09 | 2005-09-14 | Tokai Rubber Industries, Ltd. | Rubber product and method for manufacturing the same |
| CN104327511A (en) * | 2014-10-30 | 2015-02-04 | 济南泰星精细化工有限公司 | Low-smoke halogen-free flame retardant composition for silicone rubber and application thereof |
| CN105171625A (en) * | 2015-10-31 | 2015-12-23 | 赵雪雅 | Silica gel base material, silica gel tile abrading block and preparation method of silica gel tile abrading block |
| CN108440966A (en) * | 2018-03-13 | 2018-08-24 | 天长市荣盛有机硅科技有限公司 | A kind of environment protection heat-proof flame-proof silicon rubber and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113072811A (en) * | 2021-03-30 | 2021-07-06 | 陕西省石油化工研究设计院 | Xenon lamp ultraviolet aging resistant flame-retardant silicone rubber material and preparation method thereof |
| CN113717534A (en) * | 2021-09-14 | 2021-11-30 | 深圳市浩宇泰科技有限公司 | Heat conduction material and preparation process |
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