CN101585934B - Low-smoke and halogen-free fire-retardant rubber material for covering layer of conveyor belt and preparation method thereof - Google Patents
Low-smoke and halogen-free fire-retardant rubber material for covering layer of conveyor belt and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a low-smoke and halogen-free fire-retardant rubber material for a covering layer of a conveyor belt and a preparation method thereof. The preparation method comprises the following steps: filling a rubber system by adopting nano hydroxid, carrying out surface modification on nano hydroxid, matching proper fire-retardant synergist and antistatic plasticizer, and obtaining the low-smoke and halogen-free fire-retardant rubber material. The fire retardant property, the mechanical property and the antistatic property of the low-smoke and halogen-free fire-retardant rubber material all meet the requirement of a low-smoke and halogen-free fire-retardant conveyor belt covering rubber material used for underground coal mines.
Description
Technical field
The present invention relates to a kind of low-smoke and halogen-free fire-retardant rubber material for covering layer of conveyor belt and preparation method thereof.
Background technology
The colliery mass transport mainly adopts under the fire retarding conveying band, particularly coal mine, because a large amount of flammable methane gas and the finite space of air circulation difference are very high to the safety performance requirement of fire retarding conveying band.At present the conveying belt that uses under the coal mine is many based on halogen-containing matrix such as PVC or PVG (PVC/NBR and with) or by adding halogenous flame-retardant system, though obtained good flame-retardant effect and can realize flame retardant properties substantially and the balance of mechanical property, processing characteristics.But it is low still to exist intensity, and work-ing life is short, the shortcoming that transport efficiency is low, and use halogen-containing conveyor belt material can produce more hydrogen halide in the combustion processes of catching fire, because its amount of being fuming is big, the gas of generation is poisonous, thereby brings bigger danger to personnel.Hydrogen halide easily absorbs water and forms the haloid acid of severe corrosive simultaneously, and equipment is caused corrosion, brings the secondary public hazards.Whole simultaneously core dipping PVC rubber cement relates to a large amount of organic solvents and Pb stabilizer, and formulating of recipe uses a large amount of halogen-antimony fire retardant, produces and uses and all will cause severe contamination to environment.
The requirement of fire retarding conveying band of new generation is high flame retardant, environmental protection and long lifetime (8-10) in the world.The structure design and the common layered fabric core rubber conveyer belt of a new generation's low-smoke low-halogen environmental protection flame retardant conveying belt are similar, the chemical ﹠ blended fabric that working strength is higher substitutes the cotton duck of the whole core band of PVC, significantly improve the intensity of conveying belt in conjunction with the design of belt body layered structure, adopt the vulcanization gelatinization joint joint simultaneously, strength of joint can reach more than 90% of belt body intensity, improved 1 times or more than integral core PVG inhibiting tape work-ing life, improve transmission capacity greatly.The gordian technique difficult point be tectum rubber excellent flame retardancy can with the structure design of fire-retardant and the adhesive coatings technology and the belt of the balance of mechanical property, processing characteristics, fabric core.Although have many domestic well-known conveying belt manufacturer develop 10 surplus year, still do not break through above-mentioned gordian technique bottleneck, do not have product to come out so far.Be directed to tectum rubber and realize that under the low smoke and zero halogen condition excellent flame retardancy can be the main points that the present invention pays close attention to the balance of mechanical property, processing characteristics.
Since resemble inorganic hydroxide materials such as magnesium hydroxide, aluminium hydroxide press down cigarette and fire-retardant aspect all have good performance with and the characteristic of Halogen, become the focus that the preparation bittern-free flame-proof material is paid close attention to gradually.With present research, want to reach fire-retardant preferably service requirements, the addition that uses the inorganic hydroxide material is at least more than 60%, and especially mechanical property, the processing characteristics of elastomeric material significantly descend to have caused material after a large amount of interpolations.Great majority use the inorganic hydroxide flame-retardant system all to be to use in the plastics system at present, from before result of study, await further to study with the characteristic that reaches the fire-retardant requirement of Halogen or low halogen and also will guarantee elastomeric material itself simultaneously preferably by adding inorganic hydroxide.
By inorganic hydroxide being carried out surface modification or in matrix, introducing elasticity or functionalized polymkeric substance can effectively improve the mechanical property of fire retardant material, people such as Yin Dehui disclose a kind of use methacrylic acid (MMA) as properties-correcting agent in " production method of halogen-free fireproof rubber " in (ZL01113261.2), can effectively keep its mechanical property to the butylbenzene and the ethylene-propylene rubber(EPR) system of a large amount of filling magnesium hydroxides and aluminium hydroxide.But adopt this method fundamentally not solve the very poor problem that is difficult to arrive the service requirements of conveying belt of the very big caused mechanical property of inorganic hydroxide addition, and heavy addition has caused the very high problem of the hardness of material not to be improved by this method, thereby has limited its use range to a great extent.Though so can effectively keep the mechanical property of material by the method for surface modification, the mechanical property loss is still very big, still is difficult to satisfy the many requirements in the real production process.
Xiao of Qingdao University of Science and Technology builds the refined people of grade at " application in rubber of microencapsulation technology and fire retardant thereof " [specialty elastomer goods, 2005,26 (6): 17-20] introduced with micro encapsulation red phosphorus bigger as the inorganic hydroxide synergist, and smaller in to the influence of mechanical property to the flame retardant properties effect.Thereby so can reduce its influence by the consumption of selecting suitable synergist to reduce inorganic hydroxide to mechanical property.At present realize the further research that awaits of optimized fire-retardant and mechanical property effect for the reasonable proportioning by synergist in the concrete rubbery system, and use the addition of the minimizing inorganic hydroxide that synergist can not be a large amount of for general elastomeric material, problems such as the intensity that so still can't fundamentally solve system is lower, hardness is higher, and exist fire retarding synergist and when realizing flame retardant properties, caused can producing more flue gas in the combustion processes.
All these adopt methods such as surface modification, interpolation synergist can improve the flame retardant properties of material, thereby the addition that can suitably reduce inorganic hydroxide is to improve the mechanical property of material effectively, but fundamentally do not solve rubbery intensity problem on the low side, still need other interpolation to have fine fine particle carbon black of strengthening the property in a large number, as N330, N110 etc.
Simultaneously, because the complicacy of colliery subsurface environment, thereby require conveying belt can prevent effectively that static from avoiding a large amount of static to cause the down-hole inflammable gas initiation fire that catches fire, so the antistatic property of conveyor belt material is required than higher.An amount of graphitized carbon black that adds just can effectively reduce surface resistivity in traditional carbon black reinforced rubber system, thereby but adding too much carbon black in the system of a large amount of interpolation inorganic hydroxides again can cause the too high transport efficiency that influences conveying belt of hardness.Another effective ways that reduce surface resistivity is to add static inhibitor, because most static inhibitor is again a softening agent simultaneously, reduce surface resistivity and hardness double effects so can play, but in filling a large amount of oxyhydroxide systems, only can reduce surface resistivity by adding static inhibitor, be difficult to resistance is reduced to a more satisfactory scope, if and the static inhibitor addition will cause too greatly material when burning smoke density obviously rise, do not meet the requirement of low cigarette.So it also is to need a difficult point problem paying close attention in the preparation process that conveyor belt material is selected suitable antistatic system.
In sum, realize a kind of flame retardant rubber conveyor belt material of low smoke and zero halogen, at first rubber matrix and fire retardant can not contain halogen element, therefore must take all factors into consideration the kind, consumption, use-pattern of fire retardant and reach fire-retardant requirement, also will consider the selection and the collocation of desired mechanical property of conveyor belt material itself and the desired system of antistatic property simultaneously with the use of the fire retarding synergist of fire retardant collocation.
Summary of the invention
The purpose of this invention is to provide a kind of low-smoke and halogen-free fire-retardant rubber material for covering layer of conveyor belt and preparation method thereof.Adopt nanometer oxyhydroxide filled rubber system and by nanometer oxyhydroxide is carried out surface modification, cooperate suitable fire retarding synergist and antistatic elasticizer to obtain low-smoke and halogen-free fire-retardant rubber material, the requirement of the low-smoke non-halogen flame-retardant conveyer belt coating rubber material that flame retardant properties, mechanical property and antistatic property all can be satisfied use under the coal mine.
The composition of a kind of low-smoke and halogen-free fire-retardant rubber material for covering layer of conveyor belt of the present invention and mass fraction are:
100 parts of rubber matrixes
Modified Nano oxyhydroxide 50-250 part (being preferably 50-150 part)
Fire retarding synergist 3-20 part
Graphitized carbon black 1-10 part
Antistatic plasticising 5-40 part
Vulcanizing agent 0.5-5 part
Vulcanization accelerator 1-5 part
Anti-aging agent 0.5-3 part
Above-mentioned rubber matrix is the mixture of any one or they of natural rubber (NR), styrene-butadiene rubber(SBR) (SBR), paracril (NBR) or terpolymer EP rubber (EPDM).
Above-mentioned modified Nano oxyhydroxide is nano-sized magnesium hydroxide, nano-aluminum hydroxide or the nano hydrotalcite of handling through traditional dry method modification.Concrete method of modifying be with silane coupling agent with acetone diluted after and the inorganic hydroxide mixing, after drying stirs.Silane coupling agent is selected from γ-sulfenyl propyl group three oxygen methyl-monosilanes (A-189), two-[g-(triethoxysilicane) propyl group]-tetrasulfide (silicon 69), [two (the silica-based propyl group of triethoxy) tetrasulfide] (silane KH-845-4) or γ-amidino groups sulfuration propyl group ortho-siliformic acid (QZ-8-5456).
Because inorganic hydroxide flame-retardant system in the past mostly is to adopt micron-sized fire retardant to add form, uses micron-sized fire retardant can only guarantee the fire-retardant and smoke suppressing effect of material, a large amount of interpolations can cause the decline of mechanical property.The present invention considers from the over-all properties of conveyor belt material, adopted nano level magnesium hydroxide filled rubber material, utilize " nanometer enhanced principle " to reach fire-retardant and double effects reinforcement, do not use simultaneously micron filler can improve the wear hardness of material, the work-ing life that helps improving conveyor belt material effectively.
It is vulcanizing agent that the present invention adopts Sulfur, singularity according to Rubber processing, thereby the present invention is directed to silane coupling agent that sulfur sulfide system selected to be complementary with it makes surface-modifying agent be directed to elastomeric material to possess more excellent surface modification effect, can improve the dispersiveness of nano level oxyhydroxide in rubber; The silane coupling agent that contains polysulfidic bond or sulfydryl simultaneously participates in crosslinking reaction in (sulfur sulfide system) sulfidation of rubber, strengthen the interface interaction of nanometer oxyhydroxide and rubber, thereby ensure that material has good mechanical performance and flame retardant properties concurrently, do not need to add in addition the carbon black that has enhancement in a large number.
The fire retarding synergist that the present invention adopts is red phosphorus or swellability graphite.In order to make flame retardant properties more excellent, reduce the decline that inorganic hydroxide adds the back mechanical property simultaneously, fire retarding synergist of the present invention can improve the flame retardant properties of system, can guarantee that the flue gas that material produced in combustion processes is minimum simultaneously again.
The present invention adopts graphitized carbon black and antistatic elasticizer TP-90B (dioxy base ethoxyethyl formaldehyde) to realize antistatic property.Be directed to the singularity of conveyor belt material underground work, the present invention has also taken all factors into consideration antistatic property when guaranteeing mechanical property and flame retardant properties.Because the present invention adopts nano level oxyhydroxide filler, when realizing fire-retardant purpose, play good enhancing and pretended usefulness, can not add carbon black fully.Thereby reduce production and application that the sooty use can make the hardness of material descend to some extent and help conveying belt.But do not use carbon black to cause the surface resistivity of system and volume resistance to be difficult to be reduced to proper value, be unfavorable for the production security of underground conveying belt like this.The present invention adopts and adds a spot of graphitized carbon black, also uses antistatic elasticizer TP-90B simultaneously, to realize not increasing the effect that reduces surface resistivity and volume resistance under the stiffness conditions.
Vulcanization accelerator is CZ (N cyclohexyl 2 benzothiazole sulfenamide), DM (dibenzothiazyl disulfide) or TT (tetramethyl-thiuram disulfide).
Anti-aging agent is antioxidant 4010 (N-phenyl-N '-cyclohexyl Ursol D), anti-aging agent RD (2,2,4-trimethylammonium-1,2-dihyaroquinoline polymer) or anti-aging agent MC (N-(4-anilino phenyl) maleimide).
The preparation method of low-smoke and halogen-free fire-retardant rubber material for covering layer of conveyor belt of the present invention is: join rubber matrix, vulcanizing agent, modified Nano oxyhydroxide, fire retarding synergist, graphitized carbon black, antistatic elasticizer, anti-aging agent, vulcanization accelerator in the opening rubber mixing machine in proportion, the roller temperature control is at 40-50 ℃, mixing evenly after, moulding on vulcanizing press.
The present invention takes all factors into consideration from mechanical property, flame retardant properties and antistatic property aspect, finally determines the optimum formula system of low-smoke non-halogen flame-retardant conveyor belt material.The material that obtains had not only satisfied the desired low cigarette of delivered downhole carrying material, Halogen, fire-retardant, antistatic property simultaneously but also guaranteed to possess mechanical property than higher after over cure fits to conveying belt, can satisfy the requirement of delivered downhole carrying material well.
The present invention will be further described below in conjunction with embodiment:
Embodiment
Embodiment 1
Formula system is as follows:
Rubber matrix: paracril (230S) 100
Nanometer inorganic filler: nano-sized magnesium hydroxide (particle diameter 150～200 nanometers) 90
Properties-correcting agent: silane KH-845-4 5
Fire retarding synergist: red phosphorus 6
Swellability graphite (commercially available) 3.5
Antistatic elasticizer: graphitized carbon black (commercially available) 5
TP-90B 20
Vulcanizing agent: Sulfur 1.5
Activator: zinc oxide 5
Stearic acid 2
Vulcanization accelerator: CZ 1.2
DM 1
Anti-aging agent: RD 1
4010NA 2
Above-mentioned nano-sized magnesium hydroxide method of modifying be with silane KH-845-4 with the acetone diluted of 3 times of quality after and nano-sized magnesium hydroxide mix, after drying stirs.
To be adjusted to roll spacing on 6 cun opening rubber mixing machines is the following thin-pass of 0.2mm 3 times, afterwards the bag roller is reinforced to about 3mm to strengthen roll spacing then, add Sulfur, anti-aging agent, fire retardant, carbon black and vulcanization accelerator etc. successively, the roller temperature control is at 40-50 ℃, and the refining glue time is controlled at about 30min.After mixing was parked, thin slice that moulding 2mm is thick on vulcanizing press and fire-retardant batten were used for performance test.
Embodiment 2
Formula system is as follows:
Rubber matrix: terpolymer EP rubber (EP-35) 100
Nanometer inorganic filler: nano-sized magnesium hydroxide (particle diameter 150～200 nanometers) 130
Properties-correcting agent: Si69 10
Fire retarding synergist: red phosphorus 7
Swellability graphite 3
Antistatic elasticizer: graphitized carbon black 5
TP-90B 40
Vulcanizing agent: Sulfur 1.5
Activator: zinc oxide 5
Stearic acid 2
Vulcanization accelerator: CZ 2
DM 1.5
Anti-aging agent: RD 1
MC 2.5
Above-mentioned nano-sized magnesium hydroxide method of modifying be with Si69 with the acetone diluted of 3 times of quality after and nano-sized magnesium hydroxide mix, after drying stirs.
To be adjusted to roll spacing on 6 cun opening rubber mixing machines is the following thin-pass of 0.2mm 3 times, afterwards the bag roller is reinforced to about 3mm to strengthen roll spacing then, add Sulfur, anti-aging agent, fire retardant, carbon black and vulcanization accelerator etc. successively, the roller temperature control is at 40-50 ℃, and the refining glue time is controlled at about 30min.After mixing was parked, thin slice that moulding 2mm is thick on vulcanizing press and fire-retardant batten were used for performance test.
Embodiment 3
Formula system is as follows:
Rubber matrix: paracril (220S) 100
Nanometer inorganic filler: nano-aluminum hydroxide (particle diameter 150～200 nanometers) 60
Properties-correcting agent: Si69 10
Fire retarding synergist: red phosphorus 10
Swellability graphite 2
Antistatic elasticizer: graphitized carbon black 15
TP-90B 20
Vulcanizing agent: Sulfur 1.5
Activator: zinc oxide 5
Stearic acid 2
Vulcanization accelerator: CZ 2
DM 1
Anti-aging agent RD 1.5
4010 2
Above-mentioned nano-aluminum hydroxide method of modifying be with Si69 with the acetone diluted of 3 times of quality after and nano-aluminum hydroxide mix, after drying stirs.
To be adjusted to roll spacing on 6 cun opening rubber mixing machines is the following thin-pass of 0.2mm 3 times, afterwards the bag roller is reinforced to about 3mm to strengthen roll spacing then, add Sulfur, anti-aging agent, fire retardant, carbon black and vulcanization accelerator etc. successively, the roller temperature control is at 40-50 ℃, and the refining glue time is controlled at about 30min.After mixing was parked, thin slice that moulding 2mm is thick on vulcanizing press and fire-retardant batten were used for performance test.
Comparative Examples 1
Quote people such as Cheng Yanhua and the fire-retardant prescription of halogen is arranged in (" coal engineering " fourth phase in 2005) in " design of PVC unitary-core flame-resistant conveying belt rubber cover optimization of formulation ", the mass parts of each component is: 100 parts of PVC, 60 parts in softening agent, 15 parts of liquid flame retardants, 4 parts of solid flame retardants, 2 parts in static inhibitor, 5 parts of conductive filler materials, 4 parts of stablizers, 1.5 parts of lubricants, 30 parts of fillers.
Comparative Examples 2
The data of referenced patents " production method of halogen-free fireproof rubber " in (ZL01113261.2), in 100 mass parts butadiene-styrene rubbers, in Banbury mixer, mix with 150 mass parts aluminium hydroxides, the DCP that adds 40 mass parts methacrylic acids and 0.9 mass parts then successively, with the vulcanizing press sulfuration, cure conditions is 170 ℃ * 10min again.
The performance comparison of embodiment and Comparative Examples such as following table:
Annotate: the above-mentioned article of data referencing of Comparative Examples 1, Comparative Examples 2 and the data in the patent in the table.
Material performance test method: the mechanical property of measuring material according to GB/T528-1998; Measure its level and vertical combustion experiment according to GB/T2408-1996; Measure the DIN wear hardness of material according to GB9867-88; Measure the oxygen index of this material according to GB/T 2406-93; Measure the surface resistivity and the volume resistance of this material according to GB1410-78; Adopt NBS method test smoke density.
From last table data as can be seen, tectum elastomeric material of the present invention has excellent mechanical property (higher intensity and good wear resistance), flame retardant properties, antistatic property and low smoke density.The hardness of elastomeric material＜80, tensile strength＞16MPa, tensile yield＞400%, tear strength＞55Mpa, DIN abrasion loss＜200, the horizontal firing grade is FH-1, the vertical combustion grade is FV-0, oxygen index＞30%, surface resistivity＜2 * 10
8Ohm, volume resistance is＜1.0 * 10
6Ohm.
The halogen-free flameproof conveying belt prescription that the present invention adopts has for the halogen flame-retardant formulations with respect to traditional, does not discharge toxic gas during the conveying belt burning, and smoke density significantly reduces, and has increased the security that conveying belt uses.Intensity and all relative improving a lot such as flame retardant properties for other halogen-free flameproof prescriptions.And covering glue layer material of the present invention can reach the performance requriements of standard, is a kind of high performance covering glue layer of environment-friendly type.
Claims (3)
1. low-smoke and halogen-free fire-retardant rubber material for covering layer of conveyor belt, it is formed and mass fraction is:
100 parts of rubber matrixes
Modified Nano oxyhydroxide 50-150 part
Fire retarding synergist 3-20 part
Graphitized carbon black 1-10 part
Antistatic elasticizer 5-40 part
Vulcanizing agent 0.5-5 part
Vulcanization accelerator 1-5 part
Anti-aging agent 0.5-3 part
Above-mentioned rubber matrix is a kind of of natural rubber, styrene-butadiene rubber(SBR), paracril or terpolymer EP rubber or their mixture;
Modified Nano oxyhydroxide is nano-sized magnesium hydroxide, nano-aluminum hydroxide or the nano hydrotalcite of handling through dry method modification, concrete method of modifying be with silane coupling agent with acetone diluted after and the mixing of nanometer oxyhydroxide, after drying stirs;
Fire retarding synergist is red phosphorus or swellability graphite;
Sulfur is a vulcanizing agent.
2. low-smoke and halogen-free fire-retardant rubber material for covering layer of conveyor belt according to claim 1 is characterized in that: silane coupling agent is selected from γ-sulfenyl propyl group three oxygen methyl-monosilanes, [two (the silica-based propyl group of triethoxy) tetrasulfide] or γ-amidino groups sulfuration propyl group ortho-siliformic acid.
3. the preparation method of the described low-smoke and halogen-free fire-retardant rubber material for covering layer of conveyor belt of claim 1, join in the rubber mixing machine successively rubber matrix, vulcanizing agent, modified Nano oxyhydroxide, fire retarding synergist, graphitized carbon black, antistatic elasticizer, anti-aging agent, vulcanization accelerator in proportion, the roller temperature control is at 40-50 ℃, mixing evenly after, moulding on vulcanizing press.
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