CN104231336B - A kind of antimonous oxide fire retardant glue - Google Patents
A kind of antimonous oxide fire retardant glue Download PDFInfo
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- CN104231336B CN104231336B CN201410380174.5A CN201410380174A CN104231336B CN 104231336 B CN104231336 B CN 104231336B CN 201410380174 A CN201410380174 A CN 201410380174A CN 104231336 B CN104231336 B CN 104231336B
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Abstract
The invention discloses a kind of antimonous oxide fire retardant glue and preparation method thereof, belong to fire retardant glue field.Antimonous oxide fire retardant glue of the present invention, its component and mass fraction as follows: neoprene latex, 30 parts; Natural gum, 50 parts; High saturation Ethylene Propylene Terpolymer rubber, 10 parts; Anti-aging agent RD, 2 ~ 5 parts; 12687 resol, 7 ~ 15 parts; Stearic acid, 1 ~ 6 part; 4 ~ 10 parts, magnesium oxide; 10 ~ 15 parts, potter's clay; Carbon black 10 ~ 16 parts; Antimonous oxide, 10 ~ 12 parts; Paraffin oil, 5 ~ 7 parts; Captax, 1 ~ 3 part; Altax? 1 ~ 3 part; Accelerant N-oxygen diethylene-2-benzene spells thiazolesulfenamide 1 ~ 2 part; 2 ~ 4 parts, sulphur.This fire retardant glue has good flame retardant properties, and tensile strength is high, and extensibility is large.
Description
Technical field
The invention belongs to fire retardant glue field, more particularly, relate to a kind of antimonous oxide fire retardant glue and preparation method thereof.
Background technology
Flame retardant rubber refers to, can delay to catch fire, reduce flame propagation velocity, and after leaving flame, the rubber of the rapid self-extinguish of himself combustion flame energy.Flame retardant rubber can resolve into not so property gas when burning, and to cover thermal source and oxygen, thus plays fire retardation.The auxiliary agent of the every easy degree and flame propagation speed that can reduce plastics ignition is all called fire retardant glue.Fire retardant glue is the compound of V in periodictable, VII and III race's element mostly.As nitrogen, phosphorus, antimony, the secret compound of V race, the chlorine of the VIIth race, the compound of bromine and the boron of the IIIth race, the compound of aluminium.In addition the compound of silicon and molybdenum also can be used as fire retardant glue use.But it is wherein the most frequently used and the most important thing is the compound of phosphorus, bromine, chlorine, antimony and aluminium.
The material of main part of flame retardant rubber is that the rubber of halogen atom-containing is as CR, rubber etc. containing phenyl ring or conjugated double bond.
Add certain fire retardant glue in rubber and make flame retardant rubber, the requirement of fire retardant glue is as follows:
1, fire retardant glue can not damage the physical and mechanical property of plastics.
2, the decomposition temperature of fire retardant glue need adapt to the needs carrying out fire-retardant processing plastic.Fire retardant glue must decompose when plastic hot is decomposed to play its flame retardant effect rapidly, but fire retardant glue thermolysis can not occur again when plastics processing.
Chinese Patent Application No. 200910067605.1, authorized announcement date is on January 5th, 2009, invention and created name is: the formula of environment protection type flame-retardant rubber pipe, this application case relates to a kind of formula of flame-retardant rubber pipe, the present invention relates to the formula of environment protection type flame-retardant rubber pipe, component and mass fraction are: terpolymer EP rubber 100 parts, fast extrusion carbon black 20 ~ 40 parts, calcinated argil 40 ~ 60 parts, 120 ~ 160 parts, aluminium hydroxide, zinc borate 5 ~ 10 parts, antimonous oxide 10 ~ 20 parts, tetra-sulfurized pair thiuram 0.5 ~ 0.8 part, zinc dibutyl dithiocarbamate 1.5 ~ 2.0 parts, tetramethyl-thiuram disulfide 0.5 ~ 0.8 part, 3 ~ 5 parts, zinc oxide, stearic acid 1 ~ 3 part, polyoxyethylene glycol 1 ~ 3 part, curing morphine woods 1.5 ~ 2.0 parts, 0.3 ~ 0.6 part, sulphur, paraffin oil 20 ~ 40 parts.The weak point of this fire retardant glue is, the flame retardant properties of this flame-retardant rubber pipe is poor, and tensile strength and elongation all do not reach service requirements.
Summary of the invention
1. invent the technical problem that will solve
Poor for the fire retardant glue flame retardant properties existed in prior art, and tensile strength and elongation all do not reach the problem of service requirements, the invention provides a kind of antimonous oxide fire retardant glue and preparation method thereof.This fire retardant glue has good flame retardant properties, and tensile strength is high, and extensibility is large.
2. technical scheme
For achieving the above object, technical scheme provided by the invention is:
A kind of antimonous oxide fire retardant glue, its component and mass fraction as follows:
Accelerant N-oxygen diethylene-2-benzene spells thiazolesulfenamide 1 ~ 2 part
2 ~ 4 parts, sulphur.
Further, component and the mass fraction of described fire retardant glue are as follows:
Preferably, described carbon black is N330.
Preferably, described carbon black component and mass fraction as follows:
Preferably, described stearic acid is take animal grease as the stearic acid 1840,1837 or 1842 of main raw material.Stearic acid 1840,1837 or 1842 pairs of activation degrees improve a lot, and the vulcanization rate prepared rubber greatly and degree improve, and reaction is faster, saves time.
Preferably, described paraffin oil is 6 parts.
The effect of paraffin oil is fire-retardant, containing chlorine element.If paraffin oil content is too many, then the tensile strength of glue can be caused to decline, if paraffin oil content very little, the flame retardant effect of glue can be caused again to be deteriorated.The applicant obtains by experiment (as following table), when chlorinated paraffinic oil consumption is 6 parts, the intensity that draws high of glue is 14.3MPa, and flame retardant properties (flaming combustion time) is 8.6s, can obtain higher drawing high intensity and good flame retardant resistance.
| Chlorinated paraffinic oil consumption (mass fraction) | Draw high intensity | Flame retardant properties (flaming combustion time) | |
| Experiment one | 4 | 15.4MPa | 14.4s |
| Experiment two | 5 | 14.6MPa | 12.1s |
| Experiment three | 6 | 14.3MPa | 8.6s |
| Experiment four | 7 | 13.5MPa | 7.8s |
| Experiment five | 8 | 13.1MPa | 7.1s |
Preferably, described magnesium oxide is light magnesium oxide.
Preferably, the oxygen index 30 ~ 50% of described neoprene latex.
A preparation technology for described antimonous oxide fire retardant glue, the steps include:
1) by said components and mass fraction, cut neoprene latex and natural gum, take antimonous oxide;
2) sizing material one section refining glue: mill roll spacing is adjusted to 3mm, plasticates to neoprene latex, antimonous oxide, bottom sheet parks 12 hours, then is plasticated by natural gum, and bottom sheet parks 12 hours;
3) sizing material two sections is plasticated: by step 2) in plasticated one section neoprene latex, antimonous oxide and natural gum, to mix on a mill until, and by mill roll spacing furnishing 1mm, thin-pass rule 5 times, and beat triangle Bao Sanci.Thin-pass rule refers to two rollers allowing all glue by mill, and sizing material is all fallen in the pallet below mill.
4) following auxiliary material is weighed: take high saturation Ethylene Propylene Terpolymer rubber, anti-aging agent RD, resol 12687, stearic acid, magnesium oxide, potter's clay, carbon black according to described mass fraction, be placed in same container;
Take paraffin oil according to described number, be placed in same container;
Take captax, altax, the accelerant N-spelling of oxygen diethylene-2-benzene thiazolesulfenamide, sulphur according to described number, be placed in another container;
5) sizing material is mixing, by step 4) in auxiliary material high saturation Ethylene Propylene Terpolymer rubber, anti-aging agent RD, resol 12687, stearic acid, magnesium oxide, potter's clay, carbon black, paraffin oil, with step 3) in the sizing material of plasticating together put into Banbury mixer, mixing 6 ~ 8 minutes, binder removal, bottom sheet, waits to be cooled;
6) promotor and vulcanizing agent is added: on a mill until, by step 4) in captax, altax, accelerant N-oxygen diethylene-2-benzene spell thiazolesulfenamide, sulphur adds step 5) sizing material in, and when roll spacing 2mm, beat triangle Bao Sanci, then bottom sheet is stand-by.Beating triangle Bao Sanci is to allow promotor and vulcanizing agent mix in sizing material, improves the dispersion effect of promotor and vulcanizing agent.
7) get step 6) in sizing material, put in mould, then put in vulcanizing press by mould, arranging pressure is 0.8MPa, sulfuration 10 minutes at 160 DEG C of temperature.
3. beneficial effect
Adopt technical scheme provided by the invention, compared with prior art, there is following unusual effect:
(1) the nuisanceless fire retardant glue of one of the present invention's use, antimonous oxide belongs to additive flame retardant glue, with other fire retardant glue, smoke suppressor using, produce synergistic effect, antimonous oxide, at the burning initial stage, is first melting, fusing point is 655 DEG C, form protective membrane at material surface and completely cut off air, by inner thermo-negative reaction, combustionvelocity slowed down or stop, there is very excellent flame retardant properties;
(2) the present invention is material of main part with natural rubber, has higher wear resistance and tensile strength, and because natural gum is from reinforced rubber, it has higher Green strength, and suitable Green strength is very necessary for the machine-shaping of rubber;
(3) a kind of important component is additionally used in composition of the present invention, i.e. the Ethylene Propylene Terpolymer rubber of high saturation.Ethylene Propylene Terpolymer rubber saturation ratio depends on the content of Third monomer, along with the content of Third monomer increases, double bond on rubber side chain increases, then degree of unsaturation becomes large, just unstable easily decomposition under the high temperature conditions, therefore high temperature resistant to cross-linked rubber, heat-resisting compression set performance impact is very large, the Third monomer content of current normally used ethylene-propylene diene copolymer is about 8%, and the Third monomer content of the Ethylene Propylene Terpolymer rubber that the present invention adopts is about 2.7%, therefore saturation ratio is higher than the former, on EPT rubber packing part material rubber is selected, tradition is in order to ensure corresponding vulcanization rate, the ethylidene norbornene ethylene-propylene diene copolymer of normal employing content about 8%, but containing double bond in ethylidene norbornene structure, unstable easily decomposition under the high temperature conditions.Terpolymer EP rubber of the present invention is the Ethylene Propylene Terpolymer rubber of high saturation, overcomes this defect.In addition, the Ethylene Propylene Terpolymer rubber of high saturation is on rubber is selected, the less reason of current application is, the difficulty of the Ethylene Propylene Terpolymer rubber application of high saturation is larger, especially its calendering process poor performance, general being difficult to is applied, can say, the Ethylene Propylene Terpolymer rubber how applying high saturation in prior art is a difficult problem in technique always, and the present invention is successfully employed the Ethylene Propylene Terpolymer rubber of high saturation, adopt antimonous oxide and accelerant N-oxygen diethylene-2-benzene to spell thiazolesulfenamide simultaneously, although it is known to those of skill in the art that N-oxygen diethylene-2-benzene spells thiazolesulfenamide as promotor use, but the Ethylene Propylene Terpolymer rubber of high saturation is in conjunction with antimonous oxide and specific promotor, such combination is disclosed in prior art does not have, alternative document is also do not provide the enlightenment of corresponding technology, crucial feature is that such combination can produce synergistic effect, make finally to reach the high temperature resistant of excellence, the resistance to object crossing liquid cooled heat immersion and compression set performance, make the resistance to elevated temperatures that sizing material of the present invention is particluarly suitable for rubber, resistance to liquid cooled heat excessively soaks and elastic performance requires that high occasion uses,
(4) the present invention is preferably using carbon black N330 as reinforced filling, regulates hardness of rubber roll, improves wear resistance; In prior art, that conventional is N220, and technologically, the reinforcing property of carbon black N330 is worse than carbon black N220, but the operation heat generation of carbon black N220, dispersiveness are all poor than N330;
(5) another preferred carbon black material of the present invention is that carbon black N220, carbon black N330, carbon black N550, carbon black N990 combination are as carbon black material.In the various components of rubber, the effect adding carbon black is reinforcement, improves tensile strength.Carbon black N220, carbon black N330, rubbery intensity can be increased substantially, but a large amount of use can reduce and draws high elongation, N550, N990 reinforcing property is slightly poor, but that can improve rubber draws high elongation, found through experiments, these four kinds of carbon black blend rubber can obtain reasonable tensile strength, but tensile elongation also can be guaranteed; The stretcher intensity of general fire retardant glue of the prior art can only reach 12MPa ~ 14MPa, technical scheme of the present invention is adopted to reach 30MPa, this tensile strength reaches the requirement as special rubber products such as tires, improves elongation during rubber tensile, and elongation can reach 25%; In addition, the antimonous oxide in this carbon black assembled scheme and gum base ingredients with the use of, the flame retardant resistance of sizing material is improved greatly;
(6) product that method of the present invention is obtained is compared with traditional product, physical and mechanical properties tensile strength 14MPA, higher than conventional formulation 1.5 times, flame retardant resistance national standard vertical combustion FV ~ 0 grade can be obtained, the i.e. requirement of nonflammable material, reach more excellent flame retardant effect with traditional method, and meet the requirement of current automotive hose environmental protection and safety;
(7) in the inventive solutions, be placed on by antimonous oxide in mill step and plasticate, instead of be placed in Banbury mixer, such step design, improves the degree of scatter of antimonous oxide, decreases the consumption of antimonous oxide.Prior art is all be placed in Banbury mixer, because the component of adding in Banbury mixer is many, is difficult to stirring and comes;
(8) the present invention contains neoprene latex, and between the oxygen index 30 ~ 50% of neoprene latex, and oxygen index is self-extinguishing more than 27%, and it can improve flame retardant properties; The present invention uses the neoprene latex of antimonous oxide and Halogen and the halogen containing flame-retardant of chlorinated paraffinic oil and used time obvious synergistic effect is limited.When HCI or HBr decomposed with halogen containing flame-retardant contacts, the SbCL higher than great boiling point can be produced into
3.This antimony halides, can also-OH free radical in capture system apart from outside good coverage effect, suppresses to decompose further;
(9) basis is bright greatly shares with magnesium oxide and stearic acid, and as activator, anti-aging agent RD, prevents sizing material aging, and potter's clay, as weighting agent, increases volume, reduces costs, and paraffin oil, as process oil use, plays plastification;
(10) resol 12687, increases substantially hardness of rubber roll, wear resistance and lancinating, can reduce the consumption of carbon black, abandon and fill high wear-resistant carbon black in a large number, optimize processing performance, and increases hardness, and consumption is little, and efficiency is high, cost-saving.
Embodiment
For understanding content of the present invention further, the present invention is described in detail.
Embodiment 1
The preparation technology of the antimonous oxide fire retardant glue of the present embodiment, the steps include:
1) press the component as following table 1 and quality, cut neoprene latex and natural gum, take antimonous oxide; Wherein, neoprene latex is chloroprene rubber CR322, company of Changshou, Chongqing Chemical Co., Ltd. is used to produce CR322 model, the oxygen index 50% of neoprene latex, generally oxygen index is self-extinguishing more than 27%, it can improve flame retardant properties, and the oxygen index of this model chloroprene rubber CR322, higher than general material, has very strong self-extinguishment.Wherein, antimonous oxide is superfine antimony trioxide.The neoprene latex of superfine antimony trioxide and Halogen and the halogen containing flame-retardant of chlorinated paraffinic oil used time obvious synergistic effect, superfine antimony trioxide is nano level, the physicals of a large amount of filling on rubber does not affect substantially, reaches outstanding flame retardant effect and smoke suppressing effect at this moment.
2) sizing material one section refining glue: mill roll spacing is adjusted to 3mm, plasticates to neoprene latex, antimonous oxide, bottom sheet parks 12 hours, then is plasticated by natural gum, and bottom sheet parks 12 hours;
3) sizing material two sections is plasticated: by step 2) in plasticated one section neoprene latex, antimonous oxide and natural gum, to mix on a mill until, and by mill roll spacing furnishing 1mm, thin-pass rule 5 times, and beat triangle Bao Sanci.
4) following auxiliary material is weighed: take high saturation Ethylene Propylene Terpolymer rubber, anti-aging agent RD, resol 12687, stearic acid, magnesium oxide, potter's clay, carbon black according to the quality of such as following table 1, be placed in same container; Wherein, carbon black is composed as follows: carbon black N220,2kg; Carbon black N330,3kg; Carbon black N550,3kg; Carbon black N990,2kg.What stearic acid adopted is stearic acid 1840.
Take paraffin oil according to table 1, be placed in same container;
Take captax, altax, the accelerant N-spelling of oxygen diethylene-2-benzene thiazolesulfenamide, sulphur according to table 1, be placed in another container;
Table 1
| Name of material | Quality |
| Neoprene latex | 30kg |
| Natural gum | 50kg |
| High saturation Ethylene Propylene Terpolymer rubber | 10kg |
| Anti-aging agent RD | 2kg |
| 12687 resol | 7kg |
| Stearic acid 1840 | 6kg |
| Light magnesium oxide | 4kg |
| Potter's clay | 10kg |
| Carbon black | 10kg |
| Antimonous oxide | 10kg |
| Paraffin oil | 6kg |
| Captax | 3kg |
| Altax | 1kg |
| Accelerant N-oxygen diethylene-2-benzene spells thiazolesulfenamide | 2kg |
| Sulphur | 3kg |
5) sizing material is mixing, by step 4) in auxiliary material high saturation Ethylene Propylene Terpolymer rubber, anti-aging agent RD, resol 12687, stearic acid, magnesium oxide, potter's clay, carbon black, paraffin oil, with step 3) in the sizing material of plasticating together put into Banbury mixer, mixing 6 ~ 8 minutes, binder removal, bottom sheet, waits to be cooled;
6) promotor and vulcanizing agent is added: on a mill until, by step 4) in captax, altax, accelerant N-oxygen diethylene-2-benzene spell thiazolesulfenamide, sulphur adds step 5) sizing material in, and when roll spacing 2mm, beat triangle Bao Sanci, then bottom sheet is stand-by.
7) get step 6) in sizing material, put in mould, then put in vulcanizing press by mould, arranging pressure is 0.8MPa, sulfuration 10 minutes at 160 DEG C of temperature.
Above-mentioned obtained film alcohol blast burner is used to do combustion test, test according to MT_113-1995 polymer product flame-retardant and anti-static method rule, meet required flame retardant effect, the requirement of nonflammable material can be reached, reach identical flame retardant effect with traditional method.The rubber that the present embodiment 1 is obtained, draw high intensity 30MPa, draw high elongation 420%, flaming combustion time average is lower than 3s, and glowing time is on average lower than 4s.
Embodiment 2
The preparation method of the present embodiment is with embodiment 1, and its difference is, the quality of each material is as following table 2.
Table 2
| Name of material | Quality |
| Neoprene latex | 30kg |
| Natural gum | 50kg |
| Antimonous oxide | 10kg |
| High saturation Ethylene Propylene Terpolymer rubber | 10kg |
| Anti-aging agent RD | 5kg |
| 12687 resol | 15kg |
| Stearic acid 1837 | 1kg |
| Light magnesium oxide | 10kg |
| Potter's clay | 15kg |
| Carbon black N330 | 16kg |
| Antimonous oxide | 12kg |
| Paraffin oil | 7kg |
| Captax | 1kg |
| Altax | 3kg |
| Accelerant N-oxygen diethylene-2-benzene spells thiazolesulfenamide | 1kg |
| Sulphur | 4kg |
Above-mentioned obtained film alcohol blast burner is used to do combustion test, test according to MT_113-1995 polymer product flame-retardant and anti-static method rule, meet required flame retardant effect, the requirement of nonflammable material can be reached, reach identical flame retardant effect with traditional method.The rubber that the present embodiment 2 is obtained, draws high intensity 21MPa, draws high elongation 390%.Flaming combustion time average is lower than 5s, and glowing time is on average lower than 6s.
Claims (7)
1. an antimonous oxide fire retardant glue, is characterized in that: component and the mass fraction of described fire retardant glue are as follows:
The preparation technology of described antimonous oxide fire retardant glue, the steps include:
1) by described component and mass fraction, cut neoprene latex and natural gum, take antimonous oxide;
2) sizing material one section refining glue: mill roll spacing is adjusted to 3mm, plasticates to neoprene latex, antimonous oxide, bottom sheet parks 12 hours, then is plasticated by natural gum, and bottom sheet parks 12 hours;
3) sizing material two sections is plasticated: by step 2) in plasticated one section neoprene latex, antimonous oxide and natural gum, to mix on a mill until, and by mill roll spacing furnishing 1mm, thin-pass rule 5 times, and beat triangle Bao Sanci;
4) following auxiliary material is weighed: take high saturation Ethylene Propylene Terpolymer rubber, anti-aging agent RD, resol 12687, stearic acid, magnesium oxide, potter's clay, carbon black according to described mass fraction, be placed in same container;
Take paraffin oil according to described number, be placed in same container;
Take captax, altax, the accelerant N-spelling of oxygen diethylene-2-benzene thiazolesulfenamide, sulphur according to described number, be placed in another container;
5) sizing material is mixing, by step 4) in auxiliary material high saturation Ethylene Propylene Terpolymer rubber, anti-aging agent RD, resol 12687, stearic acid, magnesium oxide, potter's clay, carbon black, paraffin oil, with step 3) in the sizing material of plasticating together put into Banbury mixer, mixing 6 ~ 8 minutes, binder removal, bottom sheet, waits to be cooled;
6) promotor and vulcanizing agent is added: on a mill until, by step 4) in captax, altax, accelerant N-oxygen diethylene-2-benzene spell thiazolesulfenamide, sulphur adds step 5) sizing material in, and when roll spacing 2mm, beat triangle Bao Sanci, then bottom sheet is stand-by;
7) get step 6) in sizing material, put in mould, then put in vulcanizing press by mould, arranging pressure is 0.8Mpa, sulfuration 10 minutes at 160 DEG C of temperature.
2. a kind of antimonous oxide fire retardant glue according to claim 1, is characterized in that, described carbon black is N330.
3. a kind of antimonous oxide fire retardant glue according to claim 2, is characterized in that, described carbon black component and mass fraction as follows:
4. a kind of antimonous oxide fire retardant glue according to claim 2, is characterized in that, described stearic acid is take animal grease as the stearic acid 1840,1837 or 1842 of main raw material.
5. a kind of antimonous oxide fire retardant glue according to claim 4, is characterized in that, described paraffin oil is 6 parts.
6. a kind of antimonous oxide fire retardant glue according to claim 5, is characterized in that, described magnesium oxide is light magnesium oxide.
7. a kind of antimonous oxide fire retardant glue according to claim 5, is characterized in that, the oxygen index 30 ~ 50% of described neoprene latex.
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