CN106433137A - Flame-retarding and high-temperature-resisting nano silicone rubber and preparation method thereof - Google Patents
Flame-retarding and high-temperature-resisting nano silicone rubber and preparation method thereof Download PDFInfo
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
- C08K13/02—Organic and inorganic ingredients
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
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- C—CHEMISTRY; METALLURGY
- 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
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- C08K3/2279—Oxides; Hydroxides of metals of antimony
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- C—CHEMISTRY; METALLURGY
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- C08K5/00—Use of organic ingredients
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/56—Organo-metallic compounds, i.e. organic compounds containing a metal-to-carbon bond
- C08K5/57—Organo-tin compounds
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2237—Oxides; Hydroxides of metals of titanium
- C08K2003/2241—Titanium dioxide
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
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- C—CHEMISTRY; METALLURGY
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Abstract
The invention discloses flame-retarding and high-temperature-resisting nano silicone rubber and a preparation method thereof. The flame-retarding and high-temperature-resisting nano silicone rubber is prepared from the following raw materials: silicone rubber, nano titanium dioxide, dicumyl peroxide, dibutyl tin dialurate, p-toluenesulfonic acid triethylamine, tetrabromobisphenol, antimony trioxide, decabromodiphenyl ether, cyclohexanone peroxide and benzoyl peroxide. The flame-retarding and high-temperature-resisting nano silicone rubber has good oil resistance, corrosion resistance and low cost; the bending strength is 80MPa-100MPa and the oxygen index is 40%-50%; the tensile strength is 50MPa-70MPa and the Vicat softening temperature is 150 DEG C-170 DEG C; the wearing resistance and the elasticity are good and the elastic modulus is 13MPa-15MPa; the Shore hardness is 110-120, raw materials have abundant resources and the impact strength is 70J/m-80J/m; and the elongation at break is 220%-260% and the flame-retarding and high-temperature-resisting nano silicone rubber can be widely used under various extreme conditions and is not easy to age when being used under a high-temperature environment for a long period.
Description
Technical field
The present invention relates to technical field of rubber material, more particularly, to a kind of flame-resistant high-temperature-resistant nanometer silicon rubber and its preparation side
Method.
Background technology
The manufacturer of silicon rubber typically has dozens of or even the up to a hundred kind trades mark, is according to product characteristics and use mostly
Way is numbered, and also has and is classified according to vulcanization and chemical constitution.According to curing temperature, silicon rubber can be divided into high temperature vulcanized
Silicon rubber and room temperature vulcanized silicone rubber.One pack system, two-component room-temperature-vulcanized silicone rubber then can be divided into from packaged form.According to
The degree of polymerization, silicon rubber is further divided into mixed milling type silicon rubber and liquid silastic.
2005, Hainan met with 50 years rare arids and typhoon disaster not seen once in a hundred years, and silicon rubber produces and inflicted heavy losses on.
For excavating the development potentiality of domestic silicon rubber plantation, processing, increase self-supporting, Chinese rubber industry is made that unremitting effort, recognizes
Really implement national security, energy-saving and environmental protection and clean manufacturing policy, and be attended by the most momentous results.Especially Rubber Chemicals Industries are positive
Adjust the product mix, environmental type auxiliary agent increases substantially, age resistor improved seeds production ratio has reached 80%, and accelerator reaches
50%, poisonous, harmful, high carcinogenic NOBS output is effectively controlled；Scrap rubber comprehensive utilization ratio reaches more than 65%, reclaimed rubber
And processing and utilization field expands after rubber powder.
2006, six three councils of Chinese rubber TIA passed through discussion and issue《Chinese rubber industry " 11
Five " scientific development planning》And rubber industry Eleventh Five-Year Plan enforcement famous brand strategy planning.This is first by association and organization
The sector planning worked out.Planning shows, rubber industry the Eleventh Five-Year Plan period Independent Innovation to be walked, and the whole industry will proceed to conscientiously
The track of scientific development, makes China become the power of world rubber industry.
The development prospect of Chinese rubber industry is wide.By 2010, Chinese silicon rubber total flow was up to 2,300,000 tons,
The product structure of rubber industry will have large change, and novel product, renewal product increase, new material, new craft liquor expand
Greatly, production technology has made marked progress.
2011, jumbo fluctuation in the prices of raw materials such as rubber, and the natural rubber first quarter creates 43500 yuan/ton go through
History highest record, have an effect synthetic rubber two, the third quater on attack, amount of increase reaches 10000 yuan/ton, all occurs afterwards plummeting.It is subject to
Rubber price big ups and downs affect, and the main rubber enterprise such as tire stands in the breach, and costs of production and operation is difficult to control to, stock
Increased risk, profit margin is compressed to 2%-5%, and industry faces a severe challenge.
Silicon rubber forms main chain by silicon, oxygen atom, and side chain is carbon-containing group, and consumption maximum is the silicon rubber that side chain is ethene
Glue.Both heat-resisting, resist cold, using temperature between 100-300 DEG C, it has excellent against weather and ozone resistance with good again
Good insulating properties.Shortcoming is low intensity, and tear resistance is poor, and anti-wear performance is also poor.Silicon rubber is mainly used in aircraft industry, electrically
The aspects such as industry, food industry and health care industry.
Silicon rubber divides heat vulcanization type（High temperature vulcanized silica gel HTV）, room temperature vulcanized（RTV）, wherein room temperature vulcanized divides again
Polycondensation reaction type and addition reaction-type.High temperature silicone rubber is mainly for the manufacture of various silastic products, and room temperature silicon rubber is then led
If using as bonding agent, Embedding Material or mould.Heat vulcanization type consumption is maximum, and heat vulcanization type divides methyl silicone rubber again
（MQ）, methyl vinyl silicone rubber（VMQ, consumption and product grade are most）, methyl vinyl phenyl silicon rubber PVMQ（Resistance to low
Temperature, radiation hardness）, other also have eyeball silicon rubber, fluorosioloxane rubber etc..
That is just more for big and small rubber required for industrial department, and wide in variety, purposes is wide, and have also has spy
Different requirement.Main product has adhesive tape, sebific duct, seal washer, rubber roll, offset plate, rubber lining and articles for labour protection.In ore deposit
The industrial aspect application adhesive tape such as mountain, coal, metallurgy transporting finished product, various places all continuously emerging, in order to large-scale production clouds will,
Also produce Steel cord conveyer belt and synthetic fibers conveyer belt.Mining grinding mill rubber lining, replaces manganese steel to forge glue, using the longevity
Life improves two to four times, also reduces noise, this product is worldwide promoted.
Content of the invention
The present invention provides the flame-resistant high-temperature-resistant that a kind of heat distortion temperature is high, tensile strength is high, oxygen index (OI) is high and percentage elongation is high
Nanometer silicon rubber and preparation method thereof, solves that existing elastomeric material heat distortion temperature is low and the low technical problem of oxygen index (OI).
The present invention employs the following technical solutions：A kind of flame-resistant high-temperature-resistant nanometer silicon rubber, mass fraction proportioning pressed by its raw material
As follows：100 parts of silicon rubber, nanometer titanium dioxide 5-15 part, cumyl peroxide 0.6-1 part, dibutyl tin laurate 0.5-
0.45 part, p-methyl benzenesulfonic acid triethylamine 0.2-0.6 part, tetrabromobisphenol is 6-10 part, antimony oxide 5-25 part, deca-BDE
20-40 part, cyclohexanone peroxide 0.5-2.5 part, benzoyl peroxide 1-5 part.
As a preferred technical solution of the present invention：Mass fraction pressed by the raw material of described flame-resistant high-temperature-resistant nanometer silicon rubber
Proportioning is as follows：100 parts of silicon rubber, 5 parts of nanometer titanium dioxide, 0.6 part of cumyl peroxide, 0.5 part of dibutyl tin laurate, right
0.2 part of toluenesulfonic acid triethylamine, tetrabromobisphenol is 6 parts, 5 parts of antimony oxide, 20 parts of deca-BDE, cyclohexanone peroxide
0.5 part, 1 part of benzoyl peroxide.
As a preferred technical solution of the present invention：Mass fraction pressed by the raw material of described flame-resistant high-temperature-resistant nanometer silicon rubber
Proportioning is as follows：100 parts of silicon rubber, 15 parts of nanometer titanium dioxide, 1 part of cumyl peroxide, 0.45 part of dibutyl tin laurate, right
0.6 part of toluenesulfonic acid triethylamine, tetrabromobisphenol is 10 parts, 25 parts of antimony oxide, 40 parts of deca-BDE, cyclohexanone peroxide
2.5 parts, 5 parts of benzoyl peroxide.
As a preferred technical solution of the present invention：Mass fraction pressed by the raw material of described flame-resistant high-temperature-resistant nanometer silicon rubber
Proportioning is as follows：100 parts of silicon rubber, 10 parts of nanometer titanium dioxide, 0.8 part of cumyl peroxide, 0.48 part of dibutyl tin laurate,
0.4 part of p-methyl benzenesulfonic acid triethylamine, tetrabromobisphenol is 8 parts, 15 parts of antimony oxide, 30 parts of deca-BDE, peroxidating hexamethylene
1.5 parts of ketone, 3 parts of benzoyl peroxide.
A kind of method preparing described flame-resistant high-temperature-resistant nanometer silicon rubber, step is：
The first step：Weigh silicon rubber, nanometer titanium dioxide, cumyl peroxide, laurate dibutyl according to mass fraction proportioning
Tin, p-methyl benzenesulfonic acid triethylamine, tetrabromobisphenol, antimony oxide, deca-BDE, cyclohexanone peroxide and benzoyl peroxide first
Acyl；
Second step：Silicon rubber is put in high-speed mixer, is warming up to 100-120 DEG C, add surplus stock, be warming up to 140-
150 DEG C, mixing velocity 800-1000r/min, mix 40-50min；
3rd step：Mixed raw material adds fusion plastification granulation in double screw extruder, 200 DEG C of temperature, 210 DEG C, 220 DEG C,
230 DEG C, 220 DEG C, 210 DEG C, screw speed 120-140r/min.
Beneficial effect
A kind of flame-resistant high-temperature-resistant nanometer silicon rubber of the present invention and preparation method thereof adopts above technical scheme and prior art
Compare, there is following technique effect：1st, oil resistance is good, corrosion-resistant, low cost, bending strength 80-100MPa, oxygen index (OI) 40-
50%；2nd, tensile strength 50-70MPa, 150-170 DEG C of Vicat softening point, wearability and excellent spring, elastic modelling quantity 13-15MPa；
3rd, shore hardness 110-120, raw material resources are enriched, impact strength 70-80J/m；4th, elongation at break 220-260%, can be each
Plant extreme environment to widely use, long-term work is non-aging in high temperature environments, meets environmental requirement, can extensively produce simultaneously
Constantly replace current material.
Specific embodiment
Below in conjunction with example, the invention will be further described, and embodiment is only used for that the present invention will be described, not
Constitute restriction to right, it may occur to persons skilled in the art that other alternative means, all in right of the present invention
In claimed range.
Embodiment 1：
The first step：Weigh 100 parts of silicon rubber according to mass fraction proportioning, 5 parts of nanometer titanium dioxide, 0.6 part of cumyl peroxide,
0.5 part of dibutyl tin laurate, 0.2 part of p-methyl benzenesulfonic acid triethylamine, tetrabromobisphenol is 6 parts, 5 parts of antimony oxide, ten bromines two
20 parts of phenylate, 0.5 part of cyclohexanone peroxide, 1 part of benzoyl peroxide.
Second step：Silicon rubber is put in high-speed mixer, is warming up to 100 DEG C, add surplus stock, be warming up to 140 DEG C,
Mixing velocity 800r/min, mixes 40min.
3rd step：Mixed raw material adds fusion plastification granulation in double screw extruder, 200 DEG C of temperature, 210 DEG C, 220
DEG C, 230 DEG C, 220 DEG C, 210 DEG C, screw speed 120r/min.
Oil resistance is good, corrosion-resistant, low cost, bending strength 80MPa, oxygen index (OI) 40%；Tensile strength 50MPa, dimension card is soft
Change 150 DEG C of point, wearability and excellent spring, elastic modelling quantity 13MPa；Shore hardness 110, raw material resources are enriched, impact strength
70J/m；Elongation at break 220%, can widely use in various extreme environments, long-term work in high temperature environments is difficult always
Change.
Embodiment 2：
The first step：Weigh 100 parts of silicon rubber according to mass fraction proportioning, 15 parts of nanometer titanium dioxide, 1 part of cumyl peroxide,
0.45 part of dibutyl tin laurate, 0.6 part of p-methyl benzenesulfonic acid triethylamine, tetrabromobisphenol is 10 parts, 25 parts of antimony oxide, ten bromines
40 parts of diphenyl ether, 2.5 parts of cyclohexanone peroxide, 5 parts of benzoyl peroxide.
Second step：Silicon rubber is put in high-speed mixer, is warming up to 120 DEG C, add surplus stock, be warming up to 150 DEG C,
Mixing velocity 1000r/min, mixes 50min.
3rd step：Mixed raw material adds fusion plastification granulation in double screw extruder, 200 DEG C of temperature, 210 DEG C, 220
DEG C, 230 DEG C, 220 DEG C, 210 DEG C, screw speed 140r/min.
Oil resistance is good, corrosion-resistant, low cost, bending strength 90MPa, oxygen index (OI) 45%；Tensile strength 60MPa, dimension card is soft
Change 160 DEG C of point, wearability and excellent spring, elastic modelling quantity 14MPa；Shore hardness 115, raw material resources are enriched, impact strength
75J/m；Elongation at break 240%, can widely use in various extreme environments, long-term work in high temperature environments is difficult always
Change.
Embodiment 3：
The first step：Weigh 100 parts of silicon rubber, 10 parts of nanometer titanium dioxide, cumyl peroxide 0.8 according to mass fraction proportioning
Part, 0.48 part of dibutyl tin laurate, 0.4 part of p-methyl benzenesulfonic acid triethylamine, tetrabromobisphenol is 8 parts, 15 parts of antimony oxide, ten
30 parts of dibromodiphenyl ether, 1.5 parts of cyclohexanone peroxide, 3 parts of benzoyl peroxide.
Second step：Silicon rubber is put in high-speed mixer, is warming up to 110 DEG C, add surplus stock, be warming up to 145 DEG C,
Mixing velocity 900r/min, mixes 45min.
3rd step：Mixed raw material adds fusion plastification granulation in double screw extruder, 200 DEG C of temperature, 210 DEG C, 220
DEG C, 230 DEG C, 220 DEG C, 210 DEG C, screw speed 130r/min.
Oil resistance is good, corrosion-resistant, low cost, bending strength 100MPa, oxygen index (OI) 50%；Tensile strength 70MPa, dimension card
170 DEG C of softening point, wearability and excellent spring, elastic modelling quantity 15MPa；Shore hardness 120, raw material resources are enriched, impact strength
80J/m；Elongation at break 260%, can widely use in various extreme environments, long-term work in high temperature environments is difficult always
Change.
Claims (5)
1. a kind of flame-resistant high-temperature-resistant nanometer silicon rubber is it is characterised in that matter pressed by the raw material of described flame-resistant high-temperature-resistant nanometer silicon rubber
Amount number proportioning is as follows：100 parts of silicon rubber, nanometer titanium dioxide 5-15 part, cumyl peroxide 0.6-1 part, laurate two fourth
Base tin 0.45-0.5 part, p-methyl benzenesulfonic acid triethylamine 0.2-0.6 part, tetrabromobisphenol is 6-10 part, antimony oxide 5-25 part, ten
Dibromodiphenyl ether 20-40 part, cyclohexanone peroxide 0.5-2.5 part, benzoyl peroxide 1-5 part.
2. a kind of flame-resistant high-temperature-resistant nanometer silicon rubber according to claim 1 is it is characterised in that described flame-resistant high-temperature-resistant is received
It is as follows that mass fraction proportioning pressed by the raw material of rice silicon rubber：100 parts of silicon rubber, 5 parts of nanometer titanium dioxide, cumyl peroxide 0.6
Part, 0.5 part of dibutyl tin laurate, 0.2 part of p-methyl benzenesulfonic acid triethylamine, tetrabromobisphenol is 6 parts, 5 parts of antimony oxide, ten bromines
20 parts of diphenyl ether, 0.5 part of cyclohexanone peroxide, 1 part of benzoyl peroxide.
3. a kind of flame-resistant high-temperature-resistant nanometer silicon rubber according to claim 1 is it is characterised in that described flame-resistant high-temperature-resistant is received
It is as follows that mass fraction proportioning pressed by the raw material of rice silicon rubber：100 parts of silicon rubber, 15 parts of nanometer titanium dioxide, cumyl peroxide 1
Part, 0.45 part of dibutyl tin laurate, 0.6 part of p-methyl benzenesulfonic acid triethylamine, tetrabromobisphenol is 10 parts, 25 parts of antimony oxide,
40 parts of deca-BDE, 2.5 parts of cyclohexanone peroxide, 5 parts of benzoyl peroxide.
4. a kind of flame-resistant high-temperature-resistant nanometer silicon rubber according to claim 1 is it is characterised in that described flame-resistant high-temperature-resistant is received
It is as follows that mass fraction proportioning pressed by the raw material of rice silicon rubber：100 parts of silicon rubber, 10 parts of nanometer titanium dioxide, cumyl peroxide 0.8
Part, 0.48 part of dibutyl tin laurate, 0.4 part of p-methyl benzenesulfonic acid triethylamine, tetrabromobisphenol is 8 parts, 15 parts of antimony oxide, ten
30 parts of dibromodiphenyl ether, 1.5 parts of cyclohexanone peroxide, 3 parts of benzoyl peroxide.
5. a kind of method of the flame-resistant high-temperature-resistant nanometer silicon rubber prepared described in claim 1 is it is characterised in that include following walking
Suddenly：
The first step：Weigh silicon rubber, nanometer titanium dioxide, cumyl peroxide, laurate dibutyl according to mass fraction proportioning
Tin, p-methyl benzenesulfonic acid triethylamine, tetrabromobisphenol, antimony oxide, deca-BDE, cyclohexanone peroxide and benzoyl peroxide first
Acyl；
Second step：Silicon rubber is put in high-speed mixer, is warming up to 100-120 DEG C, add surplus stock, be warming up to 140-
150 DEG C, mixing velocity 800-1000r/min, mix 40-50min；
3rd step：Mixed raw material adds fusion plastification granulation in double screw extruder, 200 DEG C of temperature, 210 DEG C, 220 DEG C,
230 DEG C, 220 DEG C, 210 DEG C, screw speed 120-140r/min.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112538266A (en) * | 2020-11-28 | 2021-03-23 | 无锡禾杰机械有限公司 | Rubber fan part and preparation method thereof |
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| CN104610750A (en) * | 2015-02-09 | 2015-05-13 | 河北润志电气设备有限公司 | Formula of hard silicone rubber for electrical insulating materials and preparation method of formula |
-
2016
- 2016-09-20 CN CN201610834078.2A patent/CN106433137A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104610750A (en) * | 2015-02-09 | 2015-05-13 | 河北润志电气设备有限公司 | Formula of hard silicone rubber for electrical insulating materials and preparation method of formula |
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| 幸松民等: "《有机硅合成工艺及产品应用》", 30 September 2000, 化学工业出版社 * |
| 王善勤: "《塑料配方设计问答》", 31 January 2003, 中国轻工业出版社 * |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112538266A (en) * | 2020-11-28 | 2021-03-23 | 无锡禾杰机械有限公司 | Rubber fan part and preparation method thereof |
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Application publication date: 20170222 |