CN108530805A - High-strength anti-flaming compounded rubber and preparation method thereof - Google Patents
High-strength anti-flaming compounded rubber and preparation method thereof Download PDFInfo
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- CN108530805A CN108530805A CN201810499289.4A CN201810499289A CN108530805A CN 108530805 A CN108530805 A CN 108530805A CN 201810499289 A CN201810499289 A CN 201810499289A CN 108530805 A CN108530805 A CN 108530805A
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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
- C08L27/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers
- C08L27/02—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L27/12—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
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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
- C08K2003/222—Magnesia, i.e. magnesium oxide
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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
- 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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/32—Phosphorus-containing compounds
- C08K2003/321—Phosphates
- C08K2003/322—Ammonium phosphate
- C08K2003/323—Ammonium polyphosphate
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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
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
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Abstract
A kind of high-strength anti-flaming compounded rubber, fire-retardant combination used in the high-strength anti-flaming compounded rubber is using modified montmorillonite as major ingredient, coordinate the flame retardants such as nanoparticle active agent, antimony oxide and ammonium polyphosphate, has the advantages that low cigarette in high fire-retardance, inexpensive, combustion process, fluorubber, fire-retardant combination, molybdenum series catalyst, anti-aging agent, polyvinyl acetate, ethyl phosphonic acid diethylester and vulcanizing agent are subjected to mixing, obtained can not only have good low-smoke and flame retardant performance rubber, rubber obtained that also there is good mechanical performance.And the high-strength anti-flaming compounded rubber preparation method is simple, raw material is easy to get, and has higher application value.
Description
Technical field
The present invention relates to cable production arts, and in particular, to a kind of high-strength anti-flaming compounded rubber and preparation method thereof.
Background technology
It is exactly to be made of the conductor and external insulating protective layer of one or more mutually insulated for cable is popular, by electric power
Or information is transferred to the conducting wire at another place from one.With the rapid development of economy, more and more places need cable to transmit
Electric power or other information, therefore also have tightened up requirement to the manufacture of cable.The sheath of cable is the indispensable knot of cable
Structure part plays a part of protecting cable, ensures the energization safety of cable, and cable core and water, the isolation of the media such as air is allowed to keep away
Exempt from leaky occur.Resin is material of main part prepared by cable cover(ing), so the property of resin directly determines obtained cable
The property of sheath.
The classification of fire retardant can be divided into halogen system, organic phosphorus and halogen phosphorus system, silicon systems, high purity alumina-magnesia, molybdenum according to element species
System, boron system, nitrogen system etc..Halogenated flame retardant is for a long time with its flame retarding efficiency is high, dosage is few, price is low and well-known.From
The polybrominated diphenyl ethers contained in the product that brominated system burning generates, the double benzdioxans of tetrabromo were found first from Europe in 1986
And double benzofurans of tetrabromo etc. belong to carcinogen, the situation that halogen flame-retardant system rules all the land has received severe choose
The fact that war using bittern-free flame-proof material and product has been trend of the times.Existing inorganic combustion inhibitor (boron system, silicon systems etc.) although
With low toxicity, anti-rotten candle property is inexpensive, in combustion process the advantages that low cigarette, but has the shortcomings that some are very serious, such as low
Flame retarding efficiency and thermal stability cause largely to deteriorate to the physical mechanical property of material.Ammonium polyphosphate is non-toxic and tasteless, no
Etchant gas is generated, hygroscopicity is small, and thermal stability is high, is a kind of non-halogen fire retardant of function admirable.But it is lacked there is also corresponding
Point, since current process polymerisation degree is smaller so having larger hygroscopicity, and very to the Effect on Mechanical Properties of engineering plastics
Greatly.
Therefore, how low cigarette in a kind of less toxic, inexpensive, combustion process, and the fire-retardant rubber with good mechanical properties are provided
Glue, for being a technical problem to be solved urgently in the preparation of CA cable assembly.
Invention content
The object of the present invention is to provide a kind of high-strength anti-flaming compounded rubber, the resistance used in the high-strength anti-flaming compounded rubber
Composition is fired using modified montmorillonite as major ingredient, and the flame retardants such as cooperation nanoparticle active agent, antimony oxide and ammonium polyphosphate have
There is the advantages of low cigarette in high fire-retardance, inexpensive, combustion process, by fluorubber, fire-retardant combination, molybdenum series catalyst, anti-aging agent, poly-vinegar
Vinyl acetate, ethyl phosphonic acid diethylester and vulcanizing agent carry out mixing, obtained can not only have good low-smoke and flame retardant performance
Rubber, rubber obtained also have good mechanical performance.And the high-strength anti-flaming compounded rubber preparation method is simple, raw material is easy
, there is higher application value.
To achieve the goals above, the present invention provides a kind of preparation method of high-strength anti-flaming compounded rubber, this method
Include the following steps：(1) mixing is heated into dibastic sodium phosphate and montmorillonite in water, magnesium chloride is then added, be heated to reflux, obtain
Gelatinous mixture, then pH is adjusted to 8-13；(2) gelatinous mixture is calcined, crushes, obtains phosphate-magnesium-and mix
The montmorillonite of miscellaneous modification；(3) modified montmorillonite, nanoparticle active agent, antimony oxide and ammonium polyphosphate are proportionally mixed,
Obtain fire-retardant combination；(4) by fluorubber, fire-retardant combination, molybdenum series catalyst, anti-aging agent, polyvinyl acetate, ethyl phosphonic acid
Diethylester and vulcanizing agent carry out mixing；(5) mixing object is subjected to stone roller page, cutting, film is made, by film extrusion molding, microwave
Vulcanization.
The present invention also provides a kind of high-strength anti-flaming compounded rubbers being prepared according to previously described preparation method.
Through the above technical solutions, the present invention provides a kind of high-strength anti-flaming compounded rubber, the compound rubber of the high-strength anti-flaming
Fire-retardant combination used in glue is using modified montmorillonite as major ingredient, cooperation nanoparticle active agent, antimony oxide and ammonium polyphosphate etc.
Flame retardant has the advantages that low cigarette in high fire-retardance, inexpensive, combustion process, by fluorubber, fire-retardant combination, molybdenum series catalyst,
Anti-aging agent, polyvinyl acetate, ethyl phosphonic acid diethylester and vulcanizing agent carry out mixing, obtained can not only have good low
Cigarette flame retardant property rubber, rubber obtained also have good mechanical performance.And the high-strength anti-flaming compounded rubber preparation method
Simply, raw material is easy to get, and has higher application value.
Other features and advantages of the present invention will be described in detail in subsequent specific embodiment part.
Specific implementation mode
The specific implementation mode of the present invention is described in detail below.It should be understood that described herein specific
Embodiment is merely to illustrate and explain the present invention, and is not intended to restrict the invention.
The endpoint of disclosed range and any value are not limited to the accurate range or value herein, these ranges or
Value should be understood as comprising the value close to these ranges or value.For numberical range, between the endpoint value of each range, respectively
It can be combined with each other between the endpoint value of a range and individual point value, and individually between point value and obtain one or more
New numberical range, these numberical ranges should be considered as specific open herein.
To achieve the goals above, the present invention provides a kind of preparation method of fire-retardant combination, the preparation method packets
Include following steps：(1) mixing is heated into dibastic sodium phosphate and montmorillonite in water, magnesium chloride is then added, be heated to reflux, coagulated
Colloidal mixture, then pH is adjusted to 8-13；(2) gelatinous mixture is calcined, crushes, obtains phosphate-magnesium-doping
Modified montmorillonite；(3) modified montmorillonite, nanoparticle active agent, antimony oxide and ammonium polyphosphate are proportionally mixed.
Through the above technical solutions, cable fire-retardant combination provided by the invention is matched using modified montmorillonite as major ingredient
The flame retardants such as nanoparticle active agent, antimony oxide and ammonium polyphosphate are closed, there is high fire-retardance, inexpensive, low cigarette in combustion process
Advantage, and applied to when preparing rubber, can not only make rubber obtained that there is good low-smoke and flame retardant performance, additionally it is possible to give rubber
Adhesive tape carrys out good mechanical performance.And the fire retardant preparation method is simple, raw material is easy to get, and has higher application value.
In a kind of preferred embodiment of the present invention, there is high fire-retardance in order to obtain and prepared applied to rubber, plastics
In, the fire-retardant combination of good mechanical properties can be carried out for material strips, it is preferable that modified montmorillonite, nanoparticle active agent, three oxygen
The mass ratio for changing two antimony and ammonium polyphosphate is 10:1-2:1.5-3:2-3.
In a kind of preferred embodiment of the present invention, there is high fire-retardance in order to obtain and prepared applied to rubber, plastics
In, the fire-retardant combination of good mechanical properties can be carried out for material strips, it is preferable that dibastic sodium phosphate, montmorillonite and chlorine in step (1)
The mass ratio for changing magnesium is 3-5:20:2-4.
In a kind of preferred embodiment of the present invention, there is high fire-retardance in order to obtain and prepared applied to rubber, plastics
In, the fire-retardant combination of good mechanical properties can be carried out for material strips, it is preferable that the mass ratio of water and montmorillonite in step (1)
For 15-50:1.
In a kind of preferred embodiment of the present invention, there is high fire-retardance in order to obtain and prepared applied to rubber, plastics
In, the fire-retardant combination of good mechanical properties can be carried out for material strips, it is preferable that dibastic sodium phosphate, montmorillonite are in water in step (1)
The mixed condition of middle heating includes：Temperature is 60-80 DEG C, time 20-40min.
In a kind of preferred embodiment of the present invention, there is high fire-retardance in order to obtain and prepared applied to rubber, plastics
In, the fire-retardant combination of good mechanical properties can be carried out for material strips, it is preferable that it is 90-120 DEG C to be heated to reflux temperature.
In a kind of preferred embodiment of the present invention, there is high fire-retardance in order to obtain and prepared applied to rubber, plastics
In, the fire-retardant combination of good mechanical properties can be carried out for material strips, it is preferable that calcination condition includes in step (2)：Temperature is
200-280 DEG C, time 1.5h-3h.
In a kind of preferred embodiment of the present invention, there is high fire-retardance in order to obtain and prepared applied to rubber, plastics
In, the fire-retardant combination of good mechanical properties can be carried out for material strips, it is preferable that the substance that pH is adjusted in step (1) is hydrogen-oxygen
Change sodium and/or potassium hydroxide.
In a kind of preferred embodiment of the present invention, there is high fire-retardance in order to obtain and prepared applied to rubber, plastics
In, the fire-retardant combination of good mechanical properties can be carried out for material strips, it is preferable that nanoparticle active agent is nano magnesia, nanometer
It is one or more in aluminium oxide, nm-class boron nitride and nano granular of zinc oxide.
Montmorillonite common saying is also compared with bentonite, and in the above-mentioned technical solutions, montmorillonite can be selected in wider range
It selects, such as sodium-based montmorillonite, calcium-base montmorillonite etc., can meet the requirement of the present invention.For the grain size of montmorillonite, also can compared with
Selection, conventional material filler montmorillonite, such as 200 mesh, 325 mesh, the plurality of specifications such as 1250 mesh in wide scope, can meet this
The requirement of invention in embodiment later, is illustrated with the sodium-based montmorillonite of 325 mesh.
In the above-mentioned technical solutions, for the grinding mode of the substance obtained after calcining in step (2) can there are many choosings
It selects, such as grinds, rolls, ball milling etc., as long as substance after calcining can be made to crush, the present invention can be achieved, in this regard, the present invention is not
Be required, in embodiment later, in order to improve production efficiency, also for obtain can be material strips come more preferable mechanical performance
Fire-retardant combination, in embodiment later, the mode of crushing is carried out with ball milling, it is preferable that the condition of ball milling is：In planet
With the rotating speed ball milling of 220~250r/min 3~6 hours on ball mill, dispersant therein is ethyl alcohol.
The present invention also provides a kind of fire-retardant combinations being prepared according to previously described preparation method.
The present invention also provides a kind of preparation methods of high-strength anti-flaming compounded rubber, and this approach includes the following steps：(1) will
Mixing is heated in dibastic sodium phosphate and montmorillonite in water, and magnesium chloride is then added, is heated to reflux, and obtains gelatinous mixture, then will
PH is adjusted to 8-13；(2) gelatinous mixture is calcined, crushes, obtains the montmorillonite of phosphate-magnesium-doping vario-property；
(3) modified montmorillonite, nanoparticle active agent, antimony oxide and ammonium polyphosphate are proportionally mixed, obtains fire-retardant combination；
(4) by fluorubber, fire-retardant combination, molybdenum series catalyst, anti-aging agent, polyvinyl acetate, ethyl phosphonic acid diethylester and vulcanizing agent
Carry out mixing；(5) mixing object is subjected to stone roller page, cutting, film is made, by film extrusion molding, microwave vulcanization.
Through the above technical solutions, the present invention provides a kind of high-strength anti-flaming compounded rubber, the compound rubber of the high-strength anti-flaming
Fire-retardant combination used in glue is using modified montmorillonite as major ingredient, cooperation nanoparticle active agent, antimony oxide and ammonium polyphosphate etc.
Flame retardant has the advantages that low cigarette in high fire-retardance, inexpensive, combustion process, by fluorubber, fire-retardant combination, molybdenum series catalyst,
Anti-aging agent, polyvinyl acetate, ethyl phosphonic acid diethylester and vulcanizing agent carry out mixing, obtained can not only have good low
Cigarette flame retardant property rubber, rubber obtained also have good mechanical performance.And the high-strength anti-flaming compounded rubber preparation method
Simply, raw material is easy to get, and has higher application value.
In a kind of preferred embodiment of the present invention, in order to obtain low cigarette, flame retardant property be good and good mechanical property
Rubber, it is preferable that in parts by weight, relative to 100 parts of fluorubber, the dosage of fire-retardant combination is 10-15 parts, molybdenum series catalysis
The dosage of agent is 0.3-0.8 parts, and the dosage of anti-aging agent is 0.3-0.8 parts, and the dosage of polyvinyl acetate is 6-12 parts, ethyl phosphorus
The dosage of diethyl phthalate is 5-8 parts, and the dosage of vulcanizing agent is 3-8 parts.
In a kind of preferred embodiment of the present invention, in order to obtain low cigarette, flame retardant property be good and good mechanical property
Rubber, it is preferable that the condition of mixing includes：The mixing 20-30min under conditions of 160-190 DEG C of rotating speed is 200-300r/min.
In a kind of preferred embodiment of the present invention, in order to obtain low cigarette, flame retardant property be good and good mechanical property
Rubber, it is preferable that extrusion condition includes：Extrusion temperature is 175-185 DEG C, and steam pressure control is in 0.6- in extrusion
0.8MPa。
In a kind of preferred embodiment of the present invention, in order to obtain low cigarette, flame retardant property be good and good mechanical property
Rubber, it is preferable that microwave vulcanization includes successively：One section of microwave vulcanization, two sections of hot-air cures.
In a kind of preferred embodiment of the present invention, in order to obtain low cigarette, flame retardant property be good and good mechanical property
Rubber, it is further preferred that one section of microwave vulcanization section temperature is 160-180 DEG C, one section of temperature of two sections of hot-air cures is
150-160 DEG C, two sections of temperature of two sections of hot-air cures are 135-145 DEG C.
In a kind of preferred embodiment of the present invention, in order to obtain low cigarette, flame retardant property be good and good mechanical property
Rubber, it is preferable that nanoparticle active agent is in nano magnesia, nano aluminium oxide, nm-class boron nitride and nano granular of zinc oxide
It is one or more.
In a kind of preferred embodiment of the present invention, in order to obtain low cigarette, flame retardant property be good and good mechanical property
Rubber, it is preferable that molybdenum series catalyst is one or more in molybdenum tetrachloride, molybdenum pentachloride and dibromo molybdenum dioxide.
In a kind of preferred embodiment of the present invention, in order to obtain low cigarette, flame retardant property be good and good mechanical property
Rubber, it is preferable that anti-aging agent is 6- ethyoxyls -2,2,4- trimethyls -1,2 dihyaroquinoline, 2,2,4- trimethyls 1,2- dihydros
Change at least one of quinoline condensate, diaryl secondary amine antioxidant and p phenylenediamine type antioxidant.
In a kind of preferred embodiment of the present invention, in order to obtain low cigarette, flame retardant property be good and good mechanical property
Rubber, it is preferable that vulcanizing agent is selected as sulphur.
In the above-mentioned technical solutions, the plurality of specifications of polyvinyl acetate, such as number-average molecular weight are 55000-420000
It can realize the present invention, in specific embodiment later, select the number of Jiangsu silver dollar gum base materials Co., Ltd production equal
Molecular weight is 80000-110000, and grade is that the polyvinyl acetate of PVAC3 illustrates.
Fluorubber can such as select model fluororubber 23, fluororubber 26, fluororubber 246, fluorubber TP there are many selection
Deng, it is achievable of the invention, in embodiment later, fluororubber 26 is selected to illustrate.
The present invention also provides a kind of high-strength anti-flaming compounded rubbers being prepared according to previously described preparation method.
Through the above technical solutions, the present invention provides a kind of high-strength anti-flaming compounded rubber, the compound rubber of the high-strength anti-flaming
Fire-retardant combination used in glue is using modified montmorillonite as major ingredient, cooperation nanoparticle active agent, antimony oxide and ammonium polyphosphate etc.
Flame retardant has the advantages that low cigarette in high fire-retardance, inexpensive, combustion process, by fluorubber, fire-retardant combination, molybdenum series catalyst,
Anti-aging agent, polyvinyl acetate, ethyl phosphonic acid diethylester and vulcanizing agent carry out mixing, obtained can not only have good low
Cigarette flame retardant property rubber, rubber obtained also have good mechanical performance.And the high-strength anti-flaming compounded rubber preparation method
Simply, raw material is easy to get, and has higher application value.
The present invention will be described in detail by way of examples below.
Preparation example 1
The preparation method of fire-retardant combination, includes the following steps：
(1) then in water in 60 DEG C of heating mixing 40min magnesium chloride is added, in 90 DEG C in dibastic sodium phosphate and montmorillonite
It is heated to reflux, obtains gelatinous mixture, then adjusted pH to 13 with sodium hydroxide；Wherein, dibastic sodium phosphate, montmorillonite and chlorination
The mass ratio of magnesium is 3:20:2；Water and the mass ratio of montmorillonite are 15:1；
(2) gelatinous mixture is calcined into 3h, ball mill grinding in 200 DEG C, the illiteracy for obtaining phosphate-magnesium-doping vario-property takes off
Soil；
(3) by modified montmorillonite, nanoparticle active agent, antimony oxide and ammonium polyphosphate according to mass ratio be 10:1:
1.5:2 are mixed；
Wherein, nanoparticle active agent is nano aluminium oxide.
Preparation example 2
The preparation method of fire-retardant combination, includes the following steps：
(1) then in water in 80 DEG C of heating mixing 20min magnesium chloride is added, in 120 DEG C in dibastic sodium phosphate and montmorillonite
It is heated to reflux, obtains gelatinous mixture, then adjusted pH to 8 with sodium hydroxide；Wherein, dibastic sodium phosphate, montmorillonite and chlorination
The mass ratio of magnesium is 5:20:4；Water and the mass ratio of montmorillonite are 50:1；
(2) gelatinous mixture is calcined into 1.5h in 280 DEG C, ball mill grinding obtains the illiteracy of phosphate-magnesium-doping vario-property
De- soil；
(3) by modified montmorillonite, nanoparticle active agent, antimony oxide and ammonium polyphosphate according to mass ratio be 10:2:
3:3 are mixed；
Wherein, nanoparticle active agent is nano granular of zinc oxide.
Preparation example 3
The preparation method of fire-retardant combination, includes the following steps：
(1) then in water in 70 DEG C of heating mixing 30min magnesium chloride is added, in 105 DEG C in dibastic sodium phosphate and montmorillonite
It is heated to reflux, obtains gelatinous mixture, then adjusted pH to 11 with sodium hydroxide；Wherein, dibastic sodium phosphate, montmorillonite and chlorination
The mass ratio of magnesium is 4:20:3；Water and the mass ratio of montmorillonite are 30:1
(2) gelatinous mixture is calcined into 2h, ball mill grinding in 240 DEG C, the illiteracy for obtaining phosphate-magnesium-doping vario-property takes off
Soil；
(3) by modified montmorillonite, nanoparticle active agent, antimony oxide and ammonium polyphosphate according to mass ratio be 10:
1.5:2:2.5 are mixed；
Wherein, nanoparticle active agent is nano magnesia.
Embodiment 1
By fluorubber, fire-retardant combination, molybdenum tetrachloride, -1,2 dihyaroquinoline of 6- ethyoxyl -2,2,4- trimethyls, poly-vinegar
Vinyl acetate, ethyl phosphonic acid diethylester and sulphur the mixing 30min under conditions of 160 DEG C of rotating speeds are 200r/min；Wherein, with weight
Part meter is measured, relative to 100 parts of fluorubber, the dosage of fire-retardant combination is 10 parts, and the dosage of molybdenum tetrachloride is 0.3 part, 6- second
The dosage of oxygroup -2,2,4- trimethyl -1,2 dihyaroquinolines is 0.3 part, and the dosage of polyvinyl acetate is 6 parts, ethyl phosphonic acid
The dosage of diethylester is 5 parts, and the dosage of sulphur is 3 parts；Wherein, fire-retardant combination is the fire-retardant combination in preparation example 1；
Mixing object is subjected to stone roller page, cutting, film is made, by film in 175 DEG C of extrusion moldings, the steam in extrusion
Pressure is controlled in 0.6MPa, then microwave vulcanization, obtains compounded rubber；Wherein microwave vulcanization includes successively：One section of microwave vulcanization, two
Section hot-air cure；One section of microwave vulcanization section temperature is 160 DEG C, and one section of temperature of two sections of hot-air cures is 150 DEG C, two sections of heat
Two sections of temperature of air cure are 135 DEG C.
Flame retardant property test is carried out with reference to national standard GB/T2408-1996：
Horizontal flame retardant property is burnt 20 minutes using 87.9KW coal gas Bunsen burners, and flame is extended to away from coal gas Bunsen burner fire
76 centimetres of flame front end, non smoke generate；Vertical Flame performance is burnt 30 minutes using 154.5KW coal gas Bunsen burners, vertical combustion
Distance is self-extinguish after 1.51 meters, 1.51 meters.Without black smoke and penetrating odor in combustion process.
According to the method tested for tensile strength and elongation at break in national standard GB/T1040-2006, puller system model island
The AG-20KNG of Tianjin company production；Rate of extension is 500mm/min, and test temperature is 23 DEG C, is found after testing, the compounded rubber
Tensile strength be 21.4N/mm2, elongation at break 296.1%.
Embodiment 2
By fluorubber, fire-retardant combination, molybdenum pentachloride, 2,2,4- trimethyl 1,2- dihydro quinolines condensate, poly-vinegar acid second
Enester, ethyl phosphonic acid diethylester and sulphur the mixing 20min under conditions of 190 DEG C of rotating speeds are 300r/min；Wherein, with parts by weight
Meter, relative to 100 parts of fluorubber, the dosage of fire-retardant combination is 15 parts, and the dosage of molybdenum pentachloride is 0.8 part, 2,2,4- tri-
Methyl 1, the polymeric dosage of 2- dihydro quinolines are 0.8 part, and the dosage of polyvinyl acetate is 12 parts, ethyl phosphonic acid diethylester
Dosage is 8 parts, and the dosage of sulphur is 8 parts；Wherein, fire-retardant combination is the fire-retardant combination in preparation example 2；
Mixing object is subjected to stone roller page, cutting, film is made, by film in 185 DEG C of extrusion moldings, the steam in extrusion
Pressure is controlled in 0.8MPa, then microwave vulcanization, obtains compounded rubber；Wherein microwave vulcanization includes successively：One section of microwave vulcanization, two
Section hot-air cure；One section of microwave vulcanization section temperature is 180 DEG C, and one section of temperature of two sections of hot-air cures is 160 DEG C, two sections of heat
Two sections of temperature of air cure are 145 DEG C.
Flame retardant property test is carried out with reference to national standard GB/T2408-1996：
Horizontal flame retardant property is burnt 20 minutes using 87.9KW coal gas Bunsen burners, and flame is extended to away from coal gas Bunsen burner fire
65 centimetres of flame front end, non smoke generate；Vertical Flame performance is burnt 30 minutes using 154.5KW coal gas Bunsen burners, vertical combustion
Distance is self-extinguish after 1.36 meters, 1.36 meters.Without black smoke and penetrating odor in combustion process.
According to the method tested for tensile strength and elongation at break in national standard GB/T1040-2006, puller system model island
The AG-20KNG of Tianjin company production；Rate of extension is 500mm/min, and test temperature is 23 DEG C, is found after testing, the compounded rubber
Tensile strength be 22.4N/mm2, elongation at break 286.1%.
Embodiment 3
By fluorubber, fire-retardant combination, dibromo molybdenum dioxide, -1,2 dihyaroquinoline of 6- ethyoxyl -2,2,4- trimethyls,
Polyvinyl acetate, ethyl phosphonic acid diethylester and sulphur the mixing 25min under conditions of 175 DEG C of rotating speeds are 250r/min；Wherein,
In parts by weight, relative to 100 parts of fluorubber, the dosage of fire-retardant combination is 12 parts, and the dosage of dibromo molybdenum dioxide is 0.6
Part, the dosage of 6- ethyoxyls -2,2,4- trimethyl -1,2 dihyaroquinolines is 0.6 part, and the dosage of polyvinyl acetate is 9 parts,
The dosage of ethyl phosphonic acid diethylester is 7 parts, and the dosage of sulphur is 6 parts；Wherein, fire-retardant combination is fire-retardant group in preparation example 3
Close object；
Mixing object is subjected to stone roller page, cutting, film is made, by film in 180 DEG C of extrusion moldings, the steam in extrusion
Pressure is controlled in 0.7MPa, then microwave vulcanization, obtains compounded rubber；Wherein microwave vulcanization includes successively：One section of microwave vulcanization, two
Section hot-air cure；One section of microwave vulcanization section temperature is 170 DEG C, and one section of temperature of two sections of hot-air cures is 155 DEG C, two sections of heat
Two sections of temperature of air cure are 140 DEG C.
Flame retardant property test is carried out with reference to national standard GB/T2408-1996：
Horizontal flame retardant property is burnt 20 minutes using 87.9KW coal gas Bunsen burners, and flame is extended to away from coal gas Bunsen burner fire
71 centimetres of flame front end, non smoke generate；Vertical Flame performance is burnt 30 minutes using 154.5KW coal gas Bunsen burners, vertical combustion
Distance is self-extinguish after 1.41 meters, 1.41 meters.Without black smoke and penetrating odor in combustion process.
According to the method tested for tensile strength and elongation at break in national standard GB/T1040-2006, puller system model island
The AG-20KNG of Tianjin company production；Rate of extension is 500mm/min, and test temperature is 23 DEG C, is found after testing, the compounded rubber
Tensile strength be 23.4N/mm2, elongation at break 298.1%.
The preferred embodiment of the present invention has been described above in detail, still, during present invention is not limited to the embodiments described above
Detail can carry out a variety of simple variants to technical scheme of the present invention within the scope of the technical concept of the present invention, this
A little simple variants all belong to the scope of protection of the present invention.
It is further to note that specific technical features described in the above specific embodiments, in not lance
In the case of shield, can be combined by any suitable means, in order to avoid unnecessary repetition, the present invention to it is various can
The combination of energy no longer separately illustrates.
In addition, various embodiments of the present invention can be combined randomly, as long as it is without prejudice to originally
The thought of invention, it should also be regarded as the disclosure of the present invention.
Claims (10)
1. a kind of preparation method of high-strength anti-flaming compounded rubber, which is characterized in that the described method comprises the following steps：
(1) mixing is heated into dibastic sodium phosphate and montmorillonite in water, magnesium chloride is then added, be heated to reflux, it is mixed to obtain gel
Object is closed, then pH is adjusted to 8-13；
(2) gelatinous mixture is calcined, crushes, obtains the montmorillonite of phosphate-magnesium-doping vario-property；
(3) modified montmorillonite, nanoparticle active agent, antimony oxide and ammonium polyphosphate are proportionally mixed, obtains fire-retardant group
Close object；
(4) by fluorubber, fire-retardant combination, molybdenum series catalyst, anti-aging agent, polyvinyl acetate, ethyl phosphonic acid diethylester and sulphur
Agent carries out mixing；
(5) mixing object is subjected to stone roller page, cutting, film is made, by film extrusion molding, microwave vulcanization.
2. preparation method according to claim 1, wherein in parts by weight, relative to 100 parts of fluorubber, fire-retardant group
The dosage for closing object is 10-15 parts, and the dosage of molybdenum series catalyst is 0.3-0.8 parts, and the dosage of anti-aging agent is 0.3-0.8 parts, poly-vinegar
The dosage of vinyl acetate is 6-12 parts, and the dosage of ethyl phosphonic acid diethylester is 5-8 parts, and the dosage of vulcanizing agent is 3-8 parts.
3. preparation method according to claim 2, wherein the condition of mixing includes：In 160-190 DEG C of rotating speed be 200-
Mixing 20-30min under conditions of 300r/min.
4. preparation method according to claim 2, wherein extrusion condition includes：Extrusion temperature is 175-185 DEG C, is being squeezed
Steam pressure control is in 0.6-0.8MPa during going out.
5. preparation method according to claim 2, wherein microwave vulcanization includes successively：One section of microwave vulcanization, two sections of heat are empty
Gas vulcanizes；Preferably,
One section of microwave vulcanization section temperature is 160-180 DEG C, and one section of temperature of two sections of hot-air cures is 150-160 DEG C, two sections of heat
Two sections of temperature of air cure are 135-145 DEG C.
6. according to claim 1-5 any one of them preparation methods, wherein modified montmorillonite, nano active in step (3)
The mass ratio of agent, antimony oxide and ammonium polyphosphate is 10:1-2:1.5-3:2-3.
7. preparation method according to claim 6, wherein dibastic sodium phosphate in step (1), montmorillonite and magnesium chloride quality
Than for 3-5:20:2-4；
Preferably, water and the mass ratio of montmorillonite are 15-50 in step (1):1；
It is further preferred that the condition that mixing is heated in dibastic sodium phosphate, montmorillonite in water in step (1) includes：Temperature is 60-80
DEG C, time 20-40min；
And/or, wherein it is 90-120 DEG C to be heated to reflux temperature.
8. preparation method according to claim 6, wherein calcination condition includes in step (2)：Temperature is 200-280 DEG C,
Time is 1.5h-3h.
9. preparation method according to claim 6, wherein nanoparticle active agent is nano magnesia, nano aluminium oxide, nanometer
It is one or more in boron nitride and nano granular of zinc oxide；
And/or molybdenum series catalyst is one or more in molybdenum tetrachloride, molybdenum pentachloride and dibromo molybdenum dioxide；And/or
Anti-aging agent is -1,2 dihyaroquinoline of 6- ethyoxyl -2,2,4- trimethyls, the polymerization of 2,2,4- trimethyl 1,2- dihydro quinolines
At least one of body, diaryl secondary amine antioxidant and p phenylenediamine type antioxidant；
And/or vulcanizing agent is selected as sulphur.
10. the high-strength anti-flaming compounded rubber being prepared according to claim 1-9 any one of them preparation methods.
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